In a survival situation, primitive tools will get you by but for maximum survivability, you need mechanical weapons and explosives – and nothing beats the time-tested combustive mixture – gunpowder. Gunpowder is the earliest known chemical explosive. It burns fast (flash fast) and if placed inside a sealed container or shell, will create a quick burst of explosive energy. The uses for gunpowder vary widely. Gunpowder can be used to create bullets (or reload used bullets), explosive devices, rescue signals (e.g. fireworks), ignition trails, and more.

What is gunpowder?

Gunpowder consists of charcoal, sulfur, and potassium nitrate (commonly known as saltpeter). Charcoal and sulfur act as the fuels while saltpeter is the oxidizer (more on oxidation below).

Charcoal and its purpose in gunpowder

Of the three components, charcoal is the easiest to obtain in the wild. For the purpose of gunpowder, it provides a weak form of carbon (more accurately, carbon plus cellulose or unburnt wood) and other fuel for the reaction. Its purpose in gunpowder is to burn, pure and simple, and burn fast.

To create charcoal, any soft wood will suffice but willow is the wood of choice (hard wood contains too much ash). Other woods that convert easily to quality charcoal include grapevine, Hazelwood, elder, laurel, chinaberry, cottonwood, redwood, western cedar, and pine cones.

In a pinch however, any substance that burns can be used instead of charcoal including sugar or powdered metals such as aluminum or zinc.

Sulfur and its purpose in gunpowder

Sulfur serves to lower the temperature needed to ignite the gunpowder and thus, increases the rate of combustion. It serves a dual purpose acting somewhat as a cross between an ignition source and a fuel for the burn.

Sulfur is fairly common in nature and can be dug from volcanic ground or obtained from your local garden store (sulfur, which degrades to sulfuric acid, is commonly used by gardeners to correct alkaline soil). Sulfur was regularly mined in caves during the Civil War and today is mined extensively in Chile (called Chile Saltpeter). It is also found and mined in Texas and Louisiana.

Potassium nitrate (saltpeter or niter) and its purpose in gunpowder

Unlike charcoal and sulfur, potassium nitrate is typically manufactured (although it can be found naturally in bat guano) and thus, is the more difficult of the three substances to come by.

In gunpowder, saltpeter supplies oxygen for the reaction. Charcoal typically burns slow because of the limited amount of oxygen reaching the surface area of the wood. Grinding charcoal to a powder increases the surface area while saltpeter acts as the oxidizer, supplying a massive quantity of oxygen needed to rapidly burn the mixture.

Ammonium nitrate can also be used in place of potassium nitrate but it tends to produce a concussive-type explosion that shatters bullets, gun barrels, rocks, and anything else near the explosion. Of course, in some instances this may be the type of reaction you desire. The explosives that brought down the World Trade Centers in New York City and the Federal Building in Oklahoma City both used ammonium nitrate as the oxidant.

Potassium nitrate (saltpeter or “niter”) can be found in nature. A saltpeter expert explained how it was mined in the 1800’s:

“Before the 187Os, caves were the primary source of nitrate used in the manufacture of gunpowder. Saltpeter mining was one of the first major industries of the new frontier, and one of the principle objectives of exploring new territory was to find saltpeter caves. Caves were mined by individuals and also commercially for national defense purposes during the Revolutionary War, the War of 1812, and the Civil War. Cave dirt was tested for its nitrate potential by the following procedure: A footprint or mark was made in the dirt and left for twenty-four hours. If the print was scarcely visible by the next day, then the dirt was deemed high in niter.”

Mix charcoal, sulfur, and potassium nitrate together and you get – gunpowder

Commercially manufactured gunpowder granules are often coated with graphite which prevents any buildup of electrostatic charge and reduces the likelihood of an accidental ignition by static electricity. Other than that, gunpowder is nothing more than powdered charcoal, sulfur, and potassium nitrate mixed in the correct ratio.

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By weight, the ideal ratio of substances would be 75% potassium nitrate (saltpeter), 15% softwood charcoal, and 10% sulfur. This ratio can differ depending upon what the gunpowder will be used for. For instance, blasting powder (used to pulverize rock) is typically a 70/14/16 ratio (nitrate/charcoal/sulfur). Similarly, other substances may be substituted for any of the three primary components to produce a similar reaction. In these cases, the ratio may again differ from the norm. As an example, sodium nitrate may be substituted for potassium nitrate and used in a 40/30/30 mixture.

CAUTION: The dangers of gunpowder

It’s important to understand that the individual components of gunpowder can be dangerous on their own and become especially volatile when mixed together. In fact, gunpowder can be triggered by something as seemingly insignificant as static electricity. You must work slowly and carefully (and be willing to accept the risk that you could be blown to pieces in the blink of an eye).

Also, as it has been warned on hobby sites like TacPack.com that, dangerous chemicals can be released when mixing the substances together. For instance, the cold pack gunpowder recipe discussed below may release toxic ammonia gas during the mixing process. Thus, it is practical to use some sort of fume hood or perform the reaction outdoors (with proper protection).

Finally, without the manufacturing controls found in modern-day gunpowder factories, the resulting gunpowder can vary widely in its properties and burn time. Homemade gunpowder can easily turn your muzzle loader gun into a grenade depending on the ratio of the mix and quality (or lack thereof) of materials used.

How to make gunpowder in the wild

You gotta have saltpeter

There are various ways to make gunpowder in the wild including the original, old-fashioned method which takes advantage of manure and urine chemical reactions. There are also new “hacks” that use easily-available materials to create a gunpowder mixture. In most cases, when making gunpowder, the key is to find a method to produce potassium nitrate, the component that is the most difficult to find in the wild. Both charcoal and sulfur are typically easier to come by.

How to mix components to make gunpowder

Once the potassium nitrate (saltpeter) is obtained using one of the methods below, grind each component (saltpeter, charcoal, sulfur) with a stone or pestle to a fine powder. Do not grind all the ingredients together or they will likely explode, but rather, grind each individual component separately and carefully mix each together once each individual component has been ground separately to a powder. Once the materials are thoroughly combined, the resulting mixture is “gunpowder”.

Making gunpowder with pee (urine) and poop (feces)

Once charcoal and sulfur are obtained, potassium nitrate can be created via a reaction between manure and urine. In the methods discussed below, the resulting saltpeter will appear as a crusty, white substance. You may notice this material on the ground near stables or cattle holding pens where it formed naturally as cattle manure and urine mixed to trigger the chemical reaction.

The French method of creating potassium nitrate

The French method of creating gunpowder is simple but time consuming. Manure is mixed with ashes, straw, and urine. The mixture is tended (stirred periodically) for several months. Once the saltpeter crystals form in the mixture, the solution is filtered through more ashes using water (i.e. mix the solution with water and poor through ashes to collect the saltpeter on the surface of the ashes). Then the saltpeter is mixed with charcoal and sulfur in the traditional 75/15/10 ratio (see above).

The Swiss method of making potassium nitrate

The Swiss method of manufacturing saltpeter begins with the construction of a stable – a stable built upon a bed of sand. Manure is cleaned from the stable while urine naturally filters through the sand bed. As saltpeter begins to accumulate in the sand, it can be removed and isolated by filtering through ash and water (i.e. wet the saltpeter and pour through ash to isolate the saltpeter).

As noted above, this method of making the hard-to-find saltpeter occurs naturally in many stables. The potassium nitrate (saltpeter) is the white, crusty material often seen around trodden parts of a stable or cattle pen.

Backwoods method of creating potassium nitrate

The backwoods method is more of a manual process than the French and Swiss methods. Begin with a large metal drum with a valve located near the bottom of the drum (most drums are constructed like this). Place a screen on the bottom of the barrel. The screen will act as a filter for larger particles.

Place manure in the drum and add urine. Add water to the mixture and mix thoroughly. Continue adding water and pee as the solution reacts. After several months of reaction time, drain the solution from the valve and spread the mixture onto shallow trays and allow to dry. Saltpeter crystals will appear on the surface which can be mixed with charcoal and sulfur in the traditional 75/15/10 ratio.

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Making gunpowder with tree stump remover

Common tree stump remover is almost always pure saltpeter. Begin by grinding charcoal (grilling charcoal works fine) and sulfur to a fine powder. Then grind the tree stump remover into a fine powder. Finally, gently mix the saltpeter, charcoal, and sulfur together in a 75/15/10 ratio (nitrate/charcoal/sulfur).

Making gunpowder with salt, sugar, and a cold pack

With this method, we can obtain saltpeter from a cold pack and substitute sugar and lite salt (sodium-free salt) for the traditional combustible charcoal and sulfur components. First, make sure the cold pack lists ammonium nitrate as the crystal substance (some cold packs use urea). Cut the top off the cold pack and drain the water from the pack. What remains are the ammonium nitrate crystals which are used to activate the cold pack.

Mix about 40 grams of ammonium nitrate crystals with 100 ml water and stir until the ammonium nitrate crystals are completely dissolved (the solution will appear cloudy). Place 40 grams of sodium free salt (aka salt substitute) into a container. Pour the ammonium nitrate solution into the container using a coffee filter to filter our any remaining solids. Heat the solution, but not to the point of boiling, and stir until it becomes clear with no noticeable particles remaining. Place the mixture in a freezer for 1 ½ hours.

Crystals will form in the bottom of the mixture. The crystals are our potassium nitrate (saltpeter) component.

Drain off the liquid leaving the saltpeter crystals and allow the crystals to dry completely. In a non-metal container (yes, it is possible for saltpeter to ignite on its own), grind the saltpeter crystals into a fine powder. Mix one-part saltpeter with one-part powdered sugar (or normal sugar ground to a powder) to create the final gunpowder product.

Additional information

More details on the creation of gunpowders hardest-to-come-by component, potassium nitrate (niter or saltpeter) can be gleaned from the two patents below.

Gunpowder infographic

Patent CN 103771461B Double decomposition method for preparing potassium nitrate

ABSTRACT translated from Chinese

Preparation of the metathesis process of the present invention is based on potassium nitrate and potassium nitrate as raw materials, involving the technical field of inorganic chemical. The process liquor recycling, because the raw material potassium chloride into the impurities, the presence of the mother liquor impurities accumulate and deal with the problem solved in no long cycle, the present invention is to set up a production plant near Split purify production line, which set off In addition to the sodium magnesium unit, 1 to 30% by the total circulation amount of the mother liquor is introduced into the production line for removal of impurities processing, impurity mainly composed of a water-soluble sodium, magnesium, magnesium chloride as a salting-out agent to salt removal to bicarbonate removal of magnesium ammonium precipitating agent, the solution temperature 10 ℃ ~ 90 ℃, liquor return after dedoping treatment liquor circulation system.

[0001] The present invention relates to the technical field of inorganic chemicals, it is a preparation of potassium nitrate decomposition method complex.

Background technique

[0002] potassium nitrate with a wide range of uses in industry and agriculture. In industry, for the manufacture of fireworks, gunpowder, matches, drugs, used as a catalyst, ceramic glaze medicine, glass clarifying agent, in recent years with the development of regenerative solar energy utilization, potassium nitrate as a raw material for high-temperature molten salt, demand the amount of the increase. In agriculture, it is efficient nitrogen and potassium fertilizer, high chlorine-free potash, potassium chloride, potassium sulfate, potassium nitrate in three, high grade potassium nitrate, fertilizer fast, no residue, fertilizer for all crops; With the development of drip irrigation in arid regions of water-soluble fertilizer, potassium nitrate as the main raw material for water-soluble fertilizer, the demand is increasing.

[0003] (I) Chinese patents Publication No. CN100398443C (authorized announcement July 2, 2008), discloses a potassium chloride and ammonium nitrate as raw materials prepared by metathesis potassium nitrate and ammonium chloride invention. The method uses liquor circulating process. Potassium chloride starting material used in this process typically contain I~5% of soluble sodium, magnesium and other impurities, using continuous production apparatus as potassium chloride, sodium, magnesium and other impurities into the continuous system means a solution in which a portion of product into the zone a solution system, part of the accumulation in the solution. With the increase of the cumulative amount of impurities in the mother liquor, impurities out of sync from the product increases, and finally reach equilibrium. The equilibrium concentration of impurities in the mother liquor and the number of products with the raw materials into the impurity band varies, the cumulative amount of impurities in the production unit can reach 15% or higher. With the gradual increase of the cumulative amount of impurities in the mother liquor, the product of impurities gradually increase, which affects the quality of products, which leads to the gradual decline in product yield and energy consumption gradually increased. Deficiencies over patented technology that, for the presence of impurities in the mother liquor in the long-term accumulation cycle issues, as disclosed herein, no potassium nitrate plant circulating liquor impurity removal technology.

[0004] (2) “liquor treatment of potassium nitrate production process one solvent extraction separation of nitric acid and hydrochloric acid” (Dufang Lin, Gong Yu Zhen Shandong Chemical Industry, 1997 Stage I), discloses a method for producing potassium nitrate, using tributyl phosphate as the extractant, kerosene as a diluent, can be effectively extracted from the mother liquor of nitric acid, nitric acid and hydrochloric acid to achieve the purpose of complete separation of nitric acid can be completely recycled materials, the downside is seen as potassium nitrate present invention disclosed production means for circulating liquor impurity removal technology.

[0005] (3) “direct method to optimize the production of potassium nitrate liquor using a Subsidiary” (Wang Yan language, Van Xiushan etc. nationwide network of classified papers compound fertilizer [study based development] 2010 Section 2 (2010.4.29)), discloses a method for producing potassium nitrate, potassium nitrate and potassium nitrate from the reaction process will produce a lot of mother liquor, the mother liquor present a series of problems approach. In order to further optimize the use of the mother liquor, we conducted experiments to research liquor extracted rare earth phosphate, and then take a higher economic value of the rare earth phosphate and magnesium-containing compound with a slow-release NPK and ammonium bicarbonate and made stepwise traitor, the downside is seen as disclosed herein potassium nitrate plant circulating liquor impurity removal technology.

[0006] (4) “Preparation of potassium nitrate conversion of new technology” (Zhang Gang. Chemical Engineering Design, 2009,19 (5)), discloses a method for producing potassium nitrate, sodium nitrate and potassium chloride production metathesis potassium nitrate process, noting that the mother liquor impurity accumulation and processing, presented to the mother liquor should be regularly treated to remove impurities, to ensure product quality standards and production of normal operation, proposed liquor major impurity is sodium nitrite, sodium and magnesium chloride, the solution Ammonium nitrate solution is added to remove the sodium nitrite, sodium sulfate was added to remove barium chloride, magnesium chloride, potassium carbonate was removed, the downside is seen as potassium nitrate plant circulating liquor impurity removal of the disclosed technology.

[0007] (5) Chinese Patent Publication No. CN1113886A (Publication date December 27, 1995), discloses a method for producing potassium nitrate liquor recycling process, circulating liquor containing sodium nitrate and potassium chloride to give a solid role chlorination sodium and potassium nitrate liquor, cooling potassium nitrate product was separated mother liquor into sodium chloride, ammonium nitrate, ammonium chloride by-product and recycling of mother liquor obtained containing sodium nitrate, the downside is seen as disclosed herein potassium nitrate production means for circulating liquor impurity removal technology.

[0008] (6) Chinese Patent Publication No. CN1371864A (Publication date October 2, 2002), discloses a method for producing potassium nitrate liquor recycling process, the potassium salt lake resources, mining and natural sodium saltpeter and potassium nitrate mixed liquor, adjusting potassium, nitrate and water mass ratio, the mixed material converted heat to dissolve to form a slurry of solid-liquid mixing, hot melt saturated supernatant was isolated, cooled to room temperature and precipitation of potassium nitrate, potassium nitrate liquor then return Rerong phase ingredients , the downside is seen as disclosed herein potassium nitrate plant circulating liquor impurity removal technology.

[0009] (7) Lightweight magnesium carbonate and magnesium carbonate medicinal (Salt Industry Manual 2nd edition next book, 1054~1061 pages), discloses the magnesium salt (magnesium chloride, magnesium sulfate) and ammonium carbonate preparing a lightweight magnesium carbonate and medicinal technology, it relates to a magnesium removal technique, the downside is seen as potassium nitrate plant circulating liquor impurity removal of the disclosed technology.

SUMMARY OF THE INVENTION

[0010] The present invention: (I) object of the present invention is to overcome the shortcomings of the prior art and to provide a ammonium nitrate and potassium chloride as raw materials prepared by the metathesis process of removing nitrate liquor impurities, Avoid liquor impurity accumulation approach.

[0011] (2) The object of the present invention is in the process of removing impurities mother liquor, and will not affect the entire solution system production facilities, or that do not, a second removal of impurities operational errors affect the entire solution system composition and performance, thus removing impurities liquor production line and production apparatus of the present invention to provide an entire solution system should be independent, even if a particular operator error that does not mean the removal of impurities affect the entire solution system production facilities, thereby increasing the security of the present invention, , reliability and practicality.

[0012] (3) The object of the present invention is, in large-scale production entities, usually multiple sets of production equipment to run simultaneously, thus requiring the present invention to meet the needs of several sets of production equipment, production facilities are set up do not have condoms , which can reduce the investment, operating costs and land.

[0013] (4) The object of the present invention is to require continuous operation of the present invention can be intermittent operation, when the plant is running can run, when the plant shutdown can also be run, which can increase the effective of the present invention and flexibility.

[0014] (5) The purpose of the present invention is, for the mother liquor impurities, soluble sodium, magnesium is the primary, while the raw material with the grade change, the requirements of the present invention is to adapt to this change, both the simultaneous removal of sodium, magnesium, also the removal of sodium or magnesium salt can be used alone.

[0015] (6) The purpose of the present invention is widely source of salting-out agent and precipitant employed, low prices, which can improve the economics and feasibility of the present invention.

[0016] The present invention can be achieved through the following measures:

[0017] (I) set up a production plant near Split purify production line, production line set up in addition to sodium and magnesium units other units, two units can be run at the same time can also be run separately, will I~30% of the total circulation amount of liquor introduced into the production line removal of impurities were processed, the main component of the water-soluble impurities sodium, magnesium, magnesium chloride as a salting-out agent to remove part of a sodium salt, ammonium bicarbonate as the precipitating agent to remove part of the magnesium salt, the mother liquor after the treatment dedoping return liquor circulation system.

[0018] The object of the present invention can also be achieved through the following measures:

[0019] (2) the set of shunt impurity production lines and production equipment liquor circulation system is run independently and can run continuously can also intermittent operation, usually intermittent operation, ie when the plant outage when liquor circulation system outage, shunt impurity production line can run as usual: The mother liquor from the mother liquor circulation system to the shunt slot mother liquor impurity extraction section production line for processing, returning the processed liquor mother liquor system.

[0020] (3) set shunt purify production line, in a number of sets of potassium nitrate production plant running simultaneously, a shunt purify production line can simultaneously produce multiple sets of potassium nitrate liquor apparatus will be removal of impurities, handling post The mother liquor returned to their production capacity by means of mother liquor system.

[0021] (4) production plant liquor circulation system in a different cycle segments are separated from the pulp obtained liquid crystal potassium nitrate liquor and separating said crystal slurry obtained ammonium chloride liquid called liquor, except shunt miscellaneous liquor is usually ammonium chloride liquor.

[0022] (5) shunt purify production line set, which in addition to sodium and demagging units each unit consists of salting tank, sedimentation tank, hydrocyclones, filter and other equipment.

[0023] (6) the salting-out agent magnesium chloride was added salting tank, part mother liquor impurity sedimentation separation of sodium chloride, the solution temperature 40 ° C~70 ° C.

[0024] (7) in the sedimentation tank precipitant ammonium bicarbonate was added and the precipitate was separated from the impurity of magnesium chloride to generate magnesium carbonate, solution temperature 30 ° C~90 ° C.

Brief Description

[0025] (I) Figure 1 illustrates potassium nitrate plant liquor circulation system and split off relations miscellaneous liquor production line, split off miscellaneous liquor production line is set up near the plant, both of which are run independently.

[0026] (2) Figure 2 illustrates the shunt liquor dedoping process and the main production line equipment configuration, the shunt mother liquor flow meter (not shown) are metered into the salting groove, the groove configuration stirrer, salting-out agent ammonium chloride by the screw feeder (not shown) was added to the mother liquor tank with mixing shunt, salting out effect is completed within a certain residence time, sodium chloride impurities in the mother liquor partially crystallized, crystal pump (Fig. not shown) into the hydrocyclone I implemented initial liquid-solid separation, the upper clear liquid into the sedimentation tank, bottom thick crystal slurry into the filter I implemented a secondary liquid-solid separation, and the resulting residue is sodium chloride impurities, send precinct external processing, filtrate pump (not shown) into the sedimentation tank, ammonium bicarbonate precipitating agent by a screw feeder (not shown) vessel sufficiently mixed with the mother liquor was added to complete the precipitation effect within a certain residence time, mother liquor impurity magnesium chloride to form part crystallized, crystal pump (not shown) into the hydrocyclone 2 liquid-solid implementation of preliminary separation, the upper clear liquid filtrate confluence with filter 2, a pump (not Draw) back to the production equipment liquor circulation system, the bottom of the thick crystal slurry into the filter 2 to implement liquid-solid secondary separation, and the resulting residue is magnesium impurities, outgoing precinct process.

DETAILED DESCRIPTION

[0027] Example 1: In the shunt liquor production line in Figure 2, the shunt liquor temperature of 40 ° C, is pumped into the tank salting, salting-out agent added magnesium chloride hexahydrate crystals were added in an amount according to the magnesium ion meter lOkmol, stir solution temperature 70 ° C, the residence time of 30 minutes, sodium chloride crystal slurry formation of impurities via hydrocyclones 1, filter 1, to obtain a sodium salt of impurities precipitate residues, residues amount by sodium ions from about lOkmol, sodium salt precipitation purity of about 98%.

[0028] Example 2: 1, salting tank solution temperature 60 ° C, according to the amount of sodium ion residues from about lOkmol, salt precipitation purity about 95% Example.

[0029] Example 3: 1, salting tank solution temperature of 50 ° C, according to the amount of sodium ion residues from about lOkmol, salt precipitation purity of about 90%. Example.

[0030] Example 4: 1, salting tank solution temperature 40 ° C, according to the amount of sodium ion residues from about lOkmol, salt precipitation purity about 85% Example.

[0031] Example 5: In the salting tank solution temperature 30 ° C, according to the amount of sodium ion residues from about lOkmol, salt precipitation purity of about 80% in Example 1.

[0032] Example 6: Example 4 in the mother liquor, removal of the precipitated salt, the temperature of 40 ° C, into the sedimentation tank, in the tank by adding ammonium bicarbonate precipitating agent, was added by an amount of ammonium ion meter 30kmol, stir solution temperature 90 ° C, residence time 30 minutes, via hydrocyclone 2, filter 2, to give magnesium precipitate residues, residues of magnesium ions by an amount from about 15kmol, about 98% purity magnesium precipitation.

[0033] Example 7: In Example 6, the solution temperature 80 ° C, according to the amount of magnesium ion residues from about 14kmol, magnesium precipitation purity of about 95%.

[0034] Example 8: In Example 6, the solution temperature 70 ° C, according to the amount of magnesium ion residues from about 13kmol, magnesium precipitation purity of about 90%.

[0035] Example 9: In Example 6, the solution temperature 60 ° C, according to the amount of magnesium ion residues from about 12kmol, magnesium precipitation purity of about 85%.

[0036] Example 10: In Example 6, the solution temperature 50 ° C, according to the amount of magnesium ion residues from about lOkmol, magnesium precipitation purity of about 80%.

[0037] Effect

[0038] The present invention over the prior art has the following advantages:

[0039] (I) for ammonium nitrate and potassium chloride as raw material, prepared by metathesis potassium nitrate production process, the mother liquor recycling, because the raw material potassium chloride into sodium chloride, magnesium and other impurities, the mother liquor in the long cycle The presence of impurities accumulated and handling problems, and no known treatment techniques, the present invention provides a technique to ensure the mother liquor impurities accumulate maintained at an appropriate level, e.g., the use of the present invention, can ensure that the equilibrium concentration of the mother liquor impurities remain below 10%, the best can be maintained at 5% or less, compared with the usual 15%, energy products may decline 10 percent, the fluctuation range of the product impurity chlorine ion content can be reduced from 0.2 percent to 0.1 percentage point.

[0040] (2) the removal of circulating liquor sodium magnesium impurities present invention provides methods of salting-out agent and precipitating agent magnesium chloride hexahydrate ammonium bicarbonate source is easy, inexpensive, low impurity costs.

CLAIMS(6) translated from Chinese

1. Preparation of the metathesis method potassium nitrate, ammonium nitrate and potassium chloride raw materials, products for potassium nitrate and ammonium chloride, recycled mother liquor, wherein the device is provided close to the production of a shunt purify production line, production line set up in addition to sodium unit and the unit except magnesium, which in addition to the sodium magnesium unit and the addition means respectively, by salting tank, sedimentation tank, a hydrocyclone, filter composed of two units can be run at the same time can also be run separately, the total circulation amount of the mother liquor 1% ~ 30% is introduced into the production line for removal of impurities processing, impurity mainly composed of water-soluble sodium, magnesium, magnesium chloride as the salting-out agent to remove part of the sodium, ammonium bicarbonate as the precipitating agent to remove part of the magnesium salt the solution temperature 10 ° C~90 ° C, the mother liquor return after dedoping treatment liquor circulation system.

2. The method according to claim 1, wherein, wherein the set of shunt impurity production lines and production equipment liquor circulation system is run independently, continuous operation or intermittent operation, ie when the plant outage stop liquor circulation system When shipped, the shunt purify production line to run as usual: the mother liquor from the mother liquor withdrawn part of the circulatory system to the shunt impurity liquor tank production line for processing, the mother liquor is returned after treatment liquor circulation system.

3. The method according to claim 1, characterized in that the set of shunt purify production line, in a number of sets of potassium nitrate production plant running simultaneously, a shunt purify production line can simultaneously multiple sets of potassium nitrate production plant mother liquor impurity removal process, the mother liquor after the treatment according to the amount of processing plant returned to their mother liquor system.

4. The method according to claim 1, characterized in that the plant mother liquor circulation system circulating at different segments of potassium nitrate crystals are separated from the liquid phase of said slurry resulting potassium chloride crystals separated from the mother liquor and the resulting slurry was commensurate with ammonium chloride liquor, ammonium chloride shunt purify the mother liquor is liquor.

5. The method according to claim 1, characterized in that the salting-out agent added magnesium chloride salting tank, so that part of the mother liquor impurity sedimentation separation of sodium chloride, a solution temperature of 40 ° C~70 ° C.

6. The method according to claim 1, characterized in that the precipitating agent is added in the sedimentation tank ammonium chloride impurities generated carbonate precipitation separation, a solution temperature of 30 ° C~90 ° C.

Process for the preparation of potassium nitrate

US 2157260 A

y 1939- J. DESSEVRE ET AL 2,157,260

PROCESS FOR THE PREPARATION OF POTASSI UM NITRATE Fi led May 27. 1957 w r l “H4 A 7 A H INVENTORS JEAN DsssvRE Louis DUREPAIRE BERNARD QUANQUIN J W M Wys.

Patented May 9, 1939 IS’FED :EFS ‘T 3’ ENZT OFF IE E “”PROGESS’FOR THE. PREPARATION OF POTASSIUM NITRATE Jean. Dessvre, Louis Durepaire, and Bernard v, .Quanquin, Paris, France “Application May’fl, 1937; Serial No. 145,150

In France June. 8, 1936 3 Claims.

‘ nitrate, possibly containing asmall-proportion of ammonium-nitrate and ammonium chloride; such a mixturemayfor-i-nstancebe collected after a double decomposition betweenammonium nitrate andpotassiumchlorideweither–pure or mixed with sodium-‘ chloride-“- (sylvinite) The present-inventiomhas ion-its object to prepare potassium nitrate in “the practically pure state by the. use of such a mixture of nitrates, this being effected not only by separating the potassium nitrate. from the mixture, but also by convertingythe sodium:nitrate into potassium nitrate.

The surprising observation has been made that in spite of the possible presence of ammoniacal salts (chloride or nitrate), even in considerable proportion, it is possible to convert the sodium nitrate into potassium nitrate, within the mixture itself, by means of potassium chloride, either alone or accompanied by sodium chloride (sylvinite) This makes it possible to obtain in the form of practically pure potassium nitrate, the whole of the nitrogen in nitric form which is contained .in the mixture, in spite of the presence, in the mother-liquor, of more than 10 grams molecule of ammoniacal salts per 1,000 grams of water.

The process in conformity with the invention consists in placing the mixture of nitrates in the mother-liquor resulting from a preceding operation, in adding potassium chloride, or sylvinite, and in heating for a suitable time. After the conversion, the sodium chloride thus formed is removed, then Water is added and the whole is allowed to cool.

The pure crystallized potassium nitrate may be removed, and the proper quantity of mother-liquor is brought to the starting point of the cycle, the remainder being separated for any possible further use, and chiefly in the cycle of double decomposition which affords the mixture of nitrates.

The quantity of water to be added during the process in conformity with the invention should be just sumcient to maintain in solution, during the cooling, the ammoniacal salts contained in the original mixture, and the sodium salts which tend to precipitate.

The quantity of potassium chloride, KCl, or of sylvinite employed for the conversion may vary considerably Without producing any great changes in the manufacture.

This quantity is especially determined by the proportion of salts, sodium chloride and potassium’nitrate, which it is desired to’obtain.

“The drawing illustratesone’embodiment of the process.

, Example 5 To 2,150 litres ofmother-liquorobtained from a preceding double decomposition between ammonium nitrate and sylvinite, with a specific gravity of 41 B. and containing: 10

. Kgs. H2O 1,200 NH4NO3 n “880 KNO: 407 NaNOs 2’71 ll NaCl 225 Percent H2O 1.4 KNO3 45.0 NaNOs 38.0 NH4NO3 6.2 NHiCl 9A This is heated at 80 C. for 30 minutes, and one proceeds, at about this temperature, that is, from to with the separation of the solid product, for instance by a centrifugal treatment.

After washing with litres of water, there 35 are removed 580 kgs. of sodium chloride accompanied by the insoluble impurities of the raw material, but not containing measurable traces of potassium, of nitrogen in the nitric state, nor of ammoniacal nitrogen. 40

The mother liquor which is collected after the centrifugal treatment and to which is added the water from the preceding washing, has also added to it 360 litres of Water, and is then subjected to a cooling to 28 C. in 30 minutes. 5

There are then removed, by centrifugal treatment or otherwise, and after washing with 120 litres of water, 1,090 kgs. of potassium nitrate having the following composition in the dry state:

Per cent 50 KNOs 95.7 NI-I4NO3 3.5 NHlCl 0.81

that is, containing only 4.3% of impurities. 55

A part of the mother-liquor or the washing water, containing 600 litres of water, is removed from the cycle, and the remainder is again utilized for a subsequent operation of conversion.

The portion of the mother-liquor removed from the cycle may be treated by any suitable means, for the recovery of the salts which it contains, but it is particularly advantageous to employ it for the preparation of the mother-liquors required for the process of the double decomposition between the ammonium nitrate and the chlorides of potassium and sodium.

W claim:

1. A process of manufacturing potassium nitrate, comprising treating ammonium nitrate with a mixture of potassium chloride and sodium chloride in a solution saturated with these salts, separating a mixture of potassium nitrate and sodium nitrate, treating the latter mixture with a mixture of potassium chloride and sodium chloride in a solution saturated with these salts, heating the mass, recovering the sodium chloride precipitated, diluting the remaining solution, cooling the diluted solution, and recovering the crystallized potassium nitrate.

2. A process of manufacturing potassium nitrate, comprising treating ammonium nitrate with a mixture of potassium chloride and sodium chloride in a first saturated mother-liquor obtained from a preceding double decomposition between ammonium nitrate, potassium chloride and sodium chloride, separating a mixture containing potassium nitrate and sodium nitrate, treating the latter mixture with a mixture of potassium chloride and sodium chloride in a second saturated mother-liquor obtained from a preceding conversion of sodium nitrate into potassium nitrate by means of a mixture of potassium chloride and sodium chloride, heating said second mother-liquor, recovering the sodium chloride precipitated, diluting the remaining solution with water, cooling the diluted solution, and. recovering the crystallized potassium nitrate.

3. A process of manufacturing potassium nitrate, comprising treating ammonium nitrate with a mixture of potassium chloride and sodium chloride in a first saturated mother-liquor obtained from a preceding double decomposition between ammonium nitrate, potassium chloride and sodium chloride, separating a mixture containing potassium nitrate and sodium nitrate, treating the latter mixture with a mixture of potassium chloride and sodium chloride in a second saturated mother-liquor obtained from a preceding conversion of sodium nitrate into potassium nitrate by means of a mixture of potassium chloride and sodium chloride, heating said sec” ond mother-liquor, recovering the sodium chloride precipitated, diluting the remaining solution with Water, cooling the diluted solution, recovering the crystallized potassium nitrate, saving a part of the remaining mother-liquor for adding to the first mother-liquor, and utilizing the other part as the second mother-liquor.

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