CN87101529A - A kind of method of producing multiple compound manure of uniting - Google Patents
A kind of method of producing multiple compound manure of uniting Download PDFInfo
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- CN87101529A CN87101529A CN 87101529 CN87101529A CN87101529A CN 87101529 A CN87101529 A CN 87101529A CN 87101529 CN87101529 CN 87101529 CN 87101529 A CN87101529 A CN 87101529A CN 87101529 A CN87101529 A CN 87101529A
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- phosphoric acid
- potassium
- reaction
- ammonium
- producing multiple
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Abstract
A kind of method of producing multiple compound manure of uniting, it is to be raw material with phosphoric acid by wet process (or thermal phosphoric acid, phosphorus mud fire dilute phosphoric acid), Repone K, ammonia, bicarbonate of ammonia, under the alkyl tertiary amine effect, produce potassium primary phosphate, potassium hydrogen phosphate ammonium and nitrogen, phosphorus, potassium ternary mixed fertilizer, get the closed circuit Chemical Manufacture technology of a kind of comprehensive utilization of resources of byproduct potassium silicofluoride simultaneously.Its product meets country's agricultural and uses standard, and production technique is simple, and cost is low, is fit to large-scale continuous production.
Description
The present invention relates to a kind of Chemical Manufacture technology of producing potassium primary phosphate, potassium hydrogen phosphate ammonium and nitrogen, phosphorus, potassium ternary mixed fertilizer of uniting.
The present invention is the improvement of application patent of invention " a kind of novel method of producing potassium primary phosphate " (applying date 860221, publication number CK86101186).Former method is to utilize 5～20% phosphoric acid and Repone K under the tertiary amine effect, put through associating, replace, forming, regeneration, finished product makes with extra care and byproduct for treatment six step process processes, make the potassium primary phosphate that meets the foodstuff additive standard, and get byproduct ammonium chloride, vitriolate of tartar etc.
The objective of the invention is to utilize the processing method of having simplified, produce multiple compound manure, reduce cost.
The object of the present invention is achieved like this: utilize phosphoric acid by wet process (or thermal phosphoric acid, phosphorus mud fire dilute phosphoric acid), agricultural Repone K, under the alkyl tertiary amine effect, through preparation, form put, salt is washed, regeneration and five step of finished product process are produced agricultural potassium primary phosphate.Again the potassium primary phosphate and the ammonium bicarbonate for agricultural use solid state reaction that reclaim are produced the potassium hydrogen phosphate ammonium; Mother liquor behind the recovery potassium primary phosphate is fed ammonia, and liquid phosphoric acid hydrogen potassium is produced in ammonification; To form the ammonium chloride that the precipitate phosphoric acid salt put in the reaction and regenerative response generate, produce that isolated vitriolate of tartar is mixed and made into the ternary mixed fertilizer in the liquid phosphoric acid hydrogen potassium process.
Fig. 1 is the process flow sheet of preparation method of the present invention.
Below in conjunction with accompanying drawing the present invention is done and to be described in detail:
1, potassium dihydrogen phosphate produces.
1. preparation: the phosphoric acid by wet process with 30% (or hot method phosphorus, phosphorus mud fire dilute phosphoric acid) pumps in the preparing tank, presses H
2PO
4Add agricultural with HCl with 1: 1 mole ratio and use Repone K, stirred 1～4 hour under 15～60 ℃ of temperature, make its dissolving, most silicofluoric acid of carrying under one's arms in the phosphoric acid are separated out with the form of sylvite at this moment.
After treating that precipitation is fully, filter rough potassium silicofluoride, filtrate is stand-by for preparation liquid.
2. form and put: the association agent is an alkyl tertiary amine, and general formula is R
3N, wherein R is the fatty alkyl with free functional group form, the carbonatoms of alkyl is more than seven.It is insoluble in water, can with phosphoric acid generation association reaction, and the chlorine root of Repone K can be replaced the dihydrogen phosphate of tertiary amine dihydrogen phosphate get off, and generates potassium primary phosphate.To prepare liquid pump and go in the reactor, add alkyl tertiary amine with 1: 1: 1.05～1.20 mole ratio, and under 10～90 ℃ of temperature, stir to form in 5～60 minutes and put reaction: R according to phosphoric acid, Repone K and the alkyl tertiary amine of preparation in the liquid
3N
(organic phase)+ H
3PO
The 4(water)+ KCl
(water)=(R
3NH) Cl
(organic phase)+ KH
2PO
The 4(water)Form the side reaction of putting, the sulfuric acid in the main and phosphoric acid by wet process, the silicofluoric acid that does not eliminate react:
Leaving standstill then and making two phase stratification, lower floor is water, wherein is potassium primary phosphate in the solution, and precipitation is water-fast phosphoric acid salt and a spot of silicofluoride, and the upper strata is an organic phase, i.e. Amine from Tertiary Amine Hydrochloride, organic phase are stayed in the reactor to treat that salt washes.
3. salt is washed: with an amount of concentration is that 5～25% Klorvess Liquid pumps in the reactor, under 15～90 ℃ of temperature, stirs 5～60 minutes, carries out salt and washes.Wash the small amounts of phosphoric acid dihydro root of still carrying under one's arms in the amine salt off, to improve the rate of recovery.Leave standstill two phase stratification after salt is washed, lower floor is a water, and promptly the salt washing lotion turns back in the preparing tank and uses, the upper strata is an organic phase, and the Amine from Tertiary Amine Hydrochloride of promptly having cleaned continues to stay in the reactor waiting and regenerates.
4. regeneration: regenerator is that concentration is 10～25% ammoniacal liquor.According to HCl in the amine salt and NH
3Mole ratio with 1: 1.00～1.20 is added to ammoniacal liquor in the reactor, under 30～80 ℃ of temperature, stirs 10～60 minutes, regenerates:
After leaving standstill two phase stratification, lower floor is a water, i.e. ammonium chloride solution is put and is cooler than below 15 ℃, makes its crystallization, separates obtaining ammonium chloride, as the raw material that is mixed of nitrogen, phosphorus, potassium three element fertilizers.Mother liquor uses as regenerator behind ammonia, and the upper strata is an organic phase, and promptly the alkyl tertiary amine after the regeneration recycles.
5. finished product: will form and put mixed solution to add concentration be 20～40% potassium hydroxide solution, and neutralize, control PH4.2～4.6 are heated to 60～100 ℃, are incubated 1 hour, precipitate complete after-filtration, and wash with less water.Filter cake is precipitate phosphoric acid salt, as the raw material that is mixed of nitrogen, phosphorus, potassium ternary mixed fertilizer.Filtrate reaches more than 47% the biphosphate potassium content through evaporation concentration, puts coldly, and crystallization under agitation is the finished product potassium primary phosphate after separate drying.Mother liquor is for system potassium hydrogen phosphate ammonium.
2, the potassium hydrogen phosphate ammonium produces
1. producing of solid phosphoric acid hydrogen potassium ammonium: will separate the mother liquor behind the potassium primary phosphate, carrying out double evaporation-cooling concentrates, content reach 45% put when above cold, crystallization under agitation, be the potassium primary phosphate of recovery after separate drying, dry under 60 ℃ of temperature, again with chemical fertilizer level bicarbonate of ammonia with 1: 1.0～1.2 mole ratio, thorough mixing under 40～50 ℃ of temperature is cured reaction:
Make solid phosphoric acid hydrogen potassium ammonium, mother liquor is for system liquid phosphoric acid hydrogen potassium ammonium.
2. producing of liquid phosphoric acid hydrogen potassium ammonium: will reclaim the separation mother liquor behind the potassium primary phosphate, according to KH
2PO
4: NH
3Be 1: 1.05～1.20 mole ratio, feed ammonia, carry out aminating reaction:
Evaporation concentration reaches more than 50% its content then, puts coldly, leaches the crystalline vitriolate of tartar, as the raw material of preparation nitrogen, phosphorus, potassium ternary mixed fertilizer.Filtrate is 50% liquid phosphoric acid hydrogen potassium ammonium.
3, producing of nitrogen, phosphorus, potassium three element fertilizers: will form the ammonium chloride, the ammonification that produce in the precipitate phosphoric acid salt put in the reaction and the regenerative response and produce isolated vitriolate of tartar in the liquid phosphoric acid hydrogen potassium ammonium process, according to N-P
2O
5-K
2O is the proportioning of 17-10-7%, and combination drying is nitrogen, phosphorus, potassium ternary mixed fertilizer.
Technology of the present invention is simple, and cost is low, can produce multiple compound manure by utilize resources synthetically, is fit to large-scale continuous production.
Be described further below by embodiment:
Example: with 33.24 kilograms of 30% phosphoric acid by wet processes (rolling over 0 kilogram of 100% phosphatase 11), agriculture with 7.17 kilograms in Repone K (rolling over 6.81 kilograms in 100% Repone K), 0.81 kilogram in 99% liquefied ammonia (rolling over 0.8 kilogram of 100% ammonia), 1.36 kilograms of 95% ammonium bicarbonate for agricultural use (rolling over 1.29 kilograms in 100% bicarbonate of ammonia), be the association agent with the alkyl tertiary amine and recycle, 7.47 kilograms of potassium primary phosphates of output agricultural, 4.57 kilograms of liquid phosphoric acid hydrogen potassium ammoniums, 2.36 kilograms of solid phosphoric acid hydrogen potassium ammoniums, 6.16 kilograms in nitrogen, phosphorus, potassium ternary mixed fertilizer.Wherein the yield of phosphorus is 92.02%, and the yield of potassium is 96.80%, and the yield of ammonia is 93.78%, and the bicarbonate of ammonia utilization ratio is 90%.The processing condition of principal reaction are in the present embodiment:
1. preparation: mole ratio: H
3PO
4: KCl=1: 1
Solvent temperature: 25～50 ℃
Dissolution time: 2～3 hours.
2. form and put: mole ratio: H
3PO
4: KCl: R
3W=1: 1: 1.05～1.20
Temperature of reaction: 50～70 ℃
Churning time: 20～50 minutes
3. salt is washed: washings: 5～20% Klorvess Liquids
Wash temperature: 50～70 ℃
Washing time: 20～50 minutes
4. regeneration: regenerator: the aqueous solution of 10～20% ammonia
Mole ratio: HCl: NH
3=1: 1.0～1.2
Churning time: 20～50 minutes
5. producing of solid phosphoric acid hydrogen potassium ammonium:
Solid state reaction mole ratio: KH
2PO
4: NH
4NCO
3=1: 1.05～1.15
Temperature of reaction: 40～50 ℃
6. producing of liquid phosphoric acid hydrogen potassium ammonium:
Aminating reaction mole ratio: KH
2PO
4: NH
3=1: 1.05～1.10
7. being mixed of nitrogen, phosphorus, potassium ternary mixed fertilizer:
Proportioning: K-P
2O
5-K
2O=17-10-7%
The product index of potassium primary phosphate:
The project quality index
Potassium primary phosphate (KH
2PO
4) content: 97.16%
PH value: 4.5
Moisture＜4%
Liquid phosphoric acid hydrogen potassium ammonium product quality indicator:
Project name: quality index
Potassium hydrogen phosphate ammonium (KNH
4HPO
4) content: 50.05%
Solid phosphoric acid hydrogen potassium ammonium product quality indicator:
The project name quality index
Potassium hydrogen phosphate ammonium (KNH
4HPO
4) content: 97.02%
Nitrogen, phosphorus, potassium ternary mixed fertilizer quality index:
The project name quality index
Potassium oxide (K
2O) content: 7%
Available phosphorus (P
2O
5) content: 10%
Ammonia-state nitrogen (N) content: 17%
Claims (5)
1, a kind of method of producing multiple compound manure of uniting, it is characterized in that earlier Repone K being dissolved in the phosphoric acid, associate with alkyl tertiary amine then, replacement(metathesis)reaction produces potassium primary phosphate, the potassium hydrogen phosphate ammonium is produced in the potassium primary phosphate and the bicarbonate of ammonia reaction of reclaiming, to form the ammonium chloride that the precipitate phosphoric acid salt of putting reaction and regenerative response produce, produce that isolated vitriolate of tartar is mixed and made into the ternary mixed fertilizer in the liquid phosphoric acid hydrogen potassium ammonium process.
2, want the 1 described method of producing multiple compound manure of uniting according to right, it is characterized in that the mole ratio of Repone K by 1: 1 is mixed in the phosphoric acid by wet process, mixing temperature is 15～60 ℃, stirs 1～4 hour.
3, the method for producing multiple compound manure of uniting according to claim 1 and 2, it is characterized in that to be furnished with the phosphoric acid solution of Repone K, with the alkyl tertiary amine effect, associate simultaneously, (mole ratio of Repone K, phosphoric acid, alkyl tertiary amine is 1: 1: 1.05～1.20 to replacement(metathesis)reaction, under 10～90 ℃ of temperature, stirred 5～60 minutes).
4, the method for producing multiple compound manure of uniting according to claim 1, it is characterized in that the potassium primary phosphate that will reclaim and bicarbonate of ammonia are with 1: 1.0～1.2 mole ratio, under 40～50 ℃ of temperature, mix, carry out solid state reaction and produce the potassium hydrogen phosphate ammonium.
5, the method for producing multiple compound manure of uniting according to claim 1 is characterized in that the isolated vitriolate of tartar of ammonium chloride, ammonification that produces in the precipitate phosphoric acid salt put in the reaction, the regenerative response forming, according to N-P
2O
5-K
2O is that nitrogen, phosphorus, potassium ternary mixed fertilizer are produced in the proportioning mixing of 17-10-17%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87101529 CN87101529A (en) | 1987-04-04 | 1987-04-04 | A kind of method of producing multiple compound manure of uniting |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87101529 CN87101529A (en) | 1987-04-04 | 1987-04-04 | A kind of method of producing multiple compound manure of uniting |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN87101529A true CN87101529A (en) | 1988-10-19 |
Family
ID=4813500
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87101529 Pending CN87101529A (en) | 1987-04-04 | 1987-04-04 | A kind of method of producing multiple compound manure of uniting |
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| Country | Link |
|---|---|
| CN (1) | CN87101529A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390050C (en) * | 2006-03-30 | 2008-05-28 | 云南省化工研究院 | Method of continuously preparing potassium dihydrogen phosphate |
| CN102976869A (en) * | 2012-12-06 | 2013-03-20 | 江苏湛蓝科技开发有限公司 | Technique for producing macroelement water-soluble fertilizer and coproducing slow-release fertilizer |
| CN110423144A (en) * | 2019-09-04 | 2019-11-08 | 李东峰 | A kind of N P and K water soluble fertilizer and preparation method thereof |
-
1987
- 1987-04-04 CN CN 87101529 patent/CN87101529A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390050C (en) * | 2006-03-30 | 2008-05-28 | 云南省化工研究院 | Method of continuously preparing potassium dihydrogen phosphate |
| CN102976869A (en) * | 2012-12-06 | 2013-03-20 | 江苏湛蓝科技开发有限公司 | Technique for producing macroelement water-soluble fertilizer and coproducing slow-release fertilizer |
| CN110423144A (en) * | 2019-09-04 | 2019-11-08 | 李东峰 | A kind of N P and K water soluble fertilizer and preparation method thereof |
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