CN103832988A - Preparation method of potassium dihydrogen phosphate - Google Patents
Preparation method of potassium dihydrogen phosphate Download PDFInfo
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- CN103832988A CN103832988A CN201210473990.1A CN201210473990A CN103832988A CN 103832988 A CN103832988 A CN 103832988A CN 201210473990 A CN201210473990 A CN 201210473990A CN 103832988 A CN103832988 A CN 103832988A
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- phosphoric acid
- solution
- potassium hydroxide
- preparation
- potassium
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Abstract
The invention discloses a preparation method of potassium dihydrogen phosphate. According to the preparation method, two-step reaction is adopted. The preparation method comprises following steps: phosphoric acid is reacted with potassium hydroxide so as to obtain dipotassium phosphate with extremely high solubility firstly, and a solution which can be filtered and possesses a pH value close to 7 is prepared with a small amount of water; and an obtained filtrate is neutralized using a phosphoric acid solution so as to obtain pure potassium dihydrogen phosphate. The preparation method is capable of removing insoluble substances and mechanical impurities in raw materials; no special filtration is needed; reaction conditions are mild; equipment is simple; mother liquor amount is less; condensation is avoided; energy consumption and labor intensity are reduced; yield is increased; and cost is reduced greatly.
Description
Technical field
The present invention relates to the field of chemical synthesis, especially a kind of preparation method of potassium primary phosphate.
Background technology
Potassium primary phosphate (KH
2pO
4), colourless tetragonal crystal or white crystalline powder, relative density 2.338,252.6 ℃ of fusing points, soluble in water, 100 ℃ time, solubleness is 83.5g/100ml water, it is acid that the aqueous solution is, mass percent is that the pH value of 1% potassium dihydrogen phosphate is 4.0, is insoluble to alcohol, has deliquescence, while being heated to 400 ℃, fusing forms transparent liquid, and cooling after fixing is dense glass shape potassium metaphosphate.
The production method of potassium primary phosphate is a lot, is roughly summarised as neutralisation, extraction process, ion exchange method, double decomposition, direct method, crystallization process and electrolytic process etc.
Neutralisation, to deliver to neutralizer after Pian Zhuan caustic potash flakes or salt of wormwood are made into the solution of mass percent 30%, under agitation neutralize with 50% phosphoric acid solution, control temperature at 80～100 ℃, pH is 4～5, neutralized reaction product after filtration, concentrated, crystallisation by cooling, centrifugation, get product after dry, crystalline mother solution turns back to concentration section and carries out reuse.
Its chemical equation is:
H
3PO
4+KOH=KH
2PO
4+H
2O
2H
3PO4+K
2CO3=2KH
2PO4+H
2O+CO
2↑
The feature of neutralisation is that technical process is short, technology maturation, and equipment is few, and quality product is high, and energy consumption is low, less investment.This method is take thermal phosphoric acid and potash as raw material, production cost is high, is difficult to apply in agricultural, mainly for the production of the potassium primary phosphate of food, medicine and technical grade, this method output has more decline from now on, can shake the dominant position of its product in foodstuffs industry but there is no at present other method.Current, the throughput of national neutralisation potassium primary phosphate accounts for the more than 90% of overall throughput.
Extraction process divides organic extraction and inorganic extraction process, and current industrialized method is organic extraction.Organic extraction is the characteristic different compounds according to organic solvent with different solubilities, optionally with an organic solvent carries out extracting and separating and come the method for preparing potassium dihydrogen phosphate.It is that by Repone K and phosphatase reaction, the hydrochloric acid of generation is almost extracted in organic solvent under suitable organic solvent (S) exists, after phase-splitting, separating, potassium primary phosphate crystallizes out from water, and after washing, be drying to obtain product potassium primary phosphate, separating, mother liquor recycles; Hydrochloric acid by reverse-extraction agent from organic phase back extraction out, extraction agent recycles during the course.
Ion exchange method, utilizes Klorvess Liquid to pass through styrene type cation exchange resin, adsorbs K from solution
+, then ammonium dihydrogen phosphate is replaced by resin, make potassium dihydrogen phosphate, then feed liquid obtains finished product potassium primary phosphate through concentrated, crystallisation by cooling, centrifugation, after dry, and crystalline mother solution turns back to concentration section and carries out reuse.
Due to generally (partial impurities does not meet specification of quality) of low quality of salt of wormwood, therefore conventionally use potassium hydroxide and phosphoric acid to prepare potassium primary phosphate.
In the production of pharmaceutical excipient, require effectively to remove impurity, comprise the mechanical impurity that starting material are introduced.Therefore, need under solution, filter, to remove insoluble impurities and mechanical impurity.
Potassium hydroxide is strong alkaline substance, multiple filter material is had to strong corrosion, directly by its filtration, operational risk is larger, and itself and phosphoric acid are all mixed with after solution, because potassium primary phosphate solubleness is larger, need to be concentrated to finite concentration and carry out again crystallization, to obtain being satisfied with yield, increase energy consumption.
And directly solid potassium hydroxide is reacted with phosphoric acid, because strong acid and strong base reacts under high density, too violent, danger is larger, and product is separated out in a large number simultaneously, can not effectively remove mechanical impurity, as product added to filtering for crystallizing after pure water, must increase mother liquor amount, both affect yield, increase again production link, caused cost up.
Summary of the invention
The object of the invention is to overcome defect of the prior art, a kind of preparation method of potassium primary phosphate is provided, can effectively remove insolubles and the mechanical impurity in raw material, introduced, not need special filter material, reaction temperature and, equipment is simple, mother liquor amount is few, avoids concentrated, has reduced energy consumption and labour intensity, improved yield, cost reduces greatly.
For addressing the above problem, the preparation method of a kind of potassium primary phosphate of the present invention, desired raw material by mass fraction proportioning is:
1 part, potassium hydroxide
0.545～0.727 part of pure water
1.894～1.909 parts of phosphoric acid solutions (mass percent 85%)
Comprise the following steps:
1) form potassium hydroxide solution by being dissolved in 0.545～0.727 part of pure water under 1 part of solid potassium hydroxide whipped state;
2) get 60% in the phosphoric acid solution that 1.894～1.909 parts of mass percents are 85%, slowly add in potassium hydroxide solution;
3) after adding, stir 10 minutes, filter;
4) 40% part of the residue in phosphoric acid solution is slowly added in step 3) gained filtrate;
5) stir 10～20 minutes, with the micro-adjust pH of dipotassium hydrogen phosphate mother liquor, make solution PH=4.0 in step 4);
6) under whipped state, make solution naturally cool to 50 ℃, the crystallization of having separated out is taken out, filter;
7) pour the crystallization after filtering into whizzer, carry out solid-liquid separation;
8) pour the solid crystal after separating into moisture eliminator, dry under 80 ℃ of conditions, obtain potassium primary phosphate.
Described raw material by massfraction proportion optimization is:
1 part, potassium hydroxide
0.545 part of pure water
1.909 parts of phosphoric acid solutions (mass percent 85%)
The preparation method of potassium primary phosphate of the present invention, reacts by two-step approach, first phosphoric acid is reacted with potassium hydroxide and generates the very large dipotassium hydrogen phosphate of solubleness, and reaction formula is as follows:
H
3PO
4+2KOH=K
2HPO
4+H
2O
Thereby using the less water yield to form can filter, pH approaches neutral solution, and then filtrate, neutralizing with phosphoric acid solution, obtains pure potassium primary phosphate, and reaction formula is as follows:
K
2HPO
4+H
3PO
4=2KH
2PO
4
Embodiment
In order to make those skilled in the art person understand better technical solution of the present invention, below in conjunction with embodiment, the present invention is described in further detail.
Embodiment mono-:
In 5000ml beaker, inject 600ml pure water, stirring and dissolving 1100g solid potassium hydroxide; Potassium hydroxide solution is poured in the there-necked flask of 3000ml, started and stir; The phosphatase 11 250g that is 85% by mass percent pours in separating funnel, and is connected with there-necked flask, opens separating funnel bottom pipe valve after completing, and phosphoric acid is added with the speed of 20g/min; After stir about 10 minutes, mass percent 85% phosphoric acid 850g is poured in separating funnel, open pipe valve phosphoric acid is added with the speed of 15g/min; Stir 10 minutes, with the micro-adjust pH of dipotassium hydrogen phosphate mother liquor, make PH=4.0; Stirring is cooled to 50 ℃, and the crystallization of having separated out is taken out, and puts into Büchner funnel inner filtration; Pour the crystallization after filtering into whizzer, carry out solid-liquid separation, in whizzer, the outlet of material mother liquor, without becoming stream mother liquor to flow out, is considered as having separated; Pour solid crystal into moisture eliminator, dry under 80 ℃ of conditions, obtain potassium primary phosphate.Through check, the biphosphate potassium content making is mass percent 99.8%, pH=4.05.
Embodiment bis-:
In 5000ml beaker, inject 800ml pure water, stirring and dissolving 1100g potassium hydroxide; Potassium hydroxide solution is poured in the there-necked flask of 3000ml, started and stir; The phosphatase 11 250g that is 85% by mass percent pours in separating funnel, and is connected with there-necked flask, opens separating funnel bottom pipe valve after completing, and phosphoric acid is added with the speed of 20g/min; After stir about 10 minutes, be that 85% phosphoric acid 850g pours in separating funnel by mass percent, open pipe valve phosphoric acid is added with the speed of 15g/min; Stir 10 minutes, with the micro-adjust pH of dipotassium hydrogen phosphate mother liquor, make PH=4.0; Stirring is cooled to 50 ℃, and the crystallization of having separated out is taken out, and puts into Büchner funnel inner filtration; Pour the crystallization after filtering into whizzer, carry out solid-liquid separation, in whizzer, the outlet of material mother liquor, without becoming stream mother liquor to flow out, is considered as having separated; Pour solid crystal into moisture eliminator, dry under 80 ℃ of conditions, obtain potassium primary phosphate.Through check, the biphosphate potassium content making is mass percent 99.8%, pH=4.05.
Embodiment tri-:
300kg pure water is evacuated to by vacuum pump in the enamel still of 1000L, starts agitator; 425kg solid potassium hydroxide is put in enamel still with the speed of 4.25kg/min; Stir 10 minutes, solid potassium hydroxide is dissolved completely, form uniform potassium hydroxide solution; Be accompanied by stirring, open phosphoric acid header tank pipe valve, take the speed of kg/min, 455kg mass percent is joined in the solution of potassium hydroxide as 85% phosphoric acid; Stir 20 minutes, make its reaction completely fully, form the dipotassium hydrogen phosphate solution of clarification uniformly; Open baiting valve valve at the bottom of still, will in the settled solution inflow filter of dipotassium hydrogen phosphate, filter; When the dipotassium hydrogen phosphate solution filtering is evacuated to after enamel still with vacuum pump, open and stir; Be accompanied by stirring, open phosphoric acid header tank pipe valve, take the speed of 6kg/min, 350kg mass percent is joined in the solution of dipotassium hydrogen phosphate as 85% phosphoric acid; Continue to stir 5 minutes, make to obtain reacting completely fully between material, form the solid-liquid mixing solutions of potassium primary phosphate; With the micro-adjust pH of dipotassium hydrogen phosphate mother liquor, make PH=4.0, continue to stir 20 minutes; The crystallization of having separated out is taken out and poured whizzer into, carry out solid-liquid separation; Crystalline solid after separating is dry at 80 ℃ of temperature, obtain potassium primary phosphate.Through check, the biphosphate potassium content making is mass percent 99.8%, pH=4.05.
Use phosphoric acid and potassium hydroxide to prepare dipotassium hydrogen phosphate solution (wherein containing a small amount of potassium primary phosphate generating), in the time that temperature is moderate, can effectively filter wherein insolubles and mechanical impurity, filtering solution pH value is 7～8, and filter material and equipment requirements are greatly reduced.
Experimental results show that, the feeding sequence of phosphoric acid and potassium hydroxide has no significant effect the generation of product, but from the angle of actual production, strong phosphoric acid is added in potassium hydroxide solution, can use more economic stainless steel equipment, avoid because local superheating causes glassed steel reaction vessels burst porcelain, cause equipment loss.Should avoid adding too much water, affect yield or have to and concentrate.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (2)
1. a preparation method for potassium primary phosphate, desired raw material by mass fraction proportioning is:
1 part, potassium hydroxide
0.545～0.727 part of pure water
1.894～1.909 parts of phosphoric acid solutions (mass percent 85%)
Comprise the following steps:
1) form potassium hydroxide solution by being dissolved in 0.545～0.727 part of pure water under 1 part of solid potassium hydroxide whipped state;
2) get 60% in the phosphoric acid solution that 1.894～1.909 parts of mass percents are 85%, slowly add in potassium hydroxide solution;
3) after adding, stir 10 minutes, filter;
4) 40% part of the residue in phosphoric acid solution is slowly added in step 3) gained filtrate;
5) stir 10～20 minutes, with the micro-adjust pH of dipotassium hydrogen phosphate mother liquor, make solution PH=4.0 in step 4);
6) under whipped state, make solution naturally cool to 50 ℃, the crystallization of having separated out is taken out, filter;
7) pour the crystallization after filtering into whizzer, carry out solid-liquid separation;
8) pour the solid crystal after separating into moisture eliminator, dry under 80 ℃ of conditions, obtain potassium primary phosphate.
2. the preparation method of potassium primary phosphate as claimed in claim 1, is characterized in that: described raw material by massfraction proportion optimization is:
1 part, potassium hydroxide
0.545 part of pure water
1.909 parts of phosphoric acid solutions (mass percent 85%).
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|---|---|---|---|
| CN201210473990.1A CN103832988A (en) | 2012-11-21 | 2012-11-21 | Preparation method of potassium dihydrogen phosphate |
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|---|---|---|---|
| CN201210473990.1A CN103832988A (en) | 2012-11-21 | 2012-11-21 | Preparation method of potassium dihydrogen phosphate |
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Family
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891465A (en) * | 2015-05-29 | 2015-09-09 | 湖北三宁化工股份有限公司 | Method for preparing potassium dihydrogen phosphate from industrial monoammonium phosphate mother solution |
| CN105948011A (en) * | 2016-05-06 | 2016-09-21 | 四川安达农森科技股份有限公司 | Preparation method of potassium dihydrogen phosphate |
| CN107804832A (en) * | 2017-11-16 | 2018-03-16 | 达州瓮福蓝剑化工有限责任公司 | A kind of neutralized by the heating of dense mother liquor obtains the method for potassium dihydrogen phosphate |
| CN109987594A (en) * | 2019-04-01 | 2019-07-09 | 太仓沪试试剂有限公司 | A kind of preparation method of potassium dihydrogen phosphate |
| CN112321348A (en) * | 2020-11-17 | 2021-02-05 | 李东峰 | Nitrogen-phosphorus-potassium water-soluble fertilizer and preparation method thereof |
| CN114057172A (en) * | 2021-12-29 | 2022-02-18 | 山东省神农生态科技股份有限公司 | Method for producing monopotassium phosphate by recovering potassium ions in corn steep liquor and monopotassium phosphate produced by method |
| CN115253980A (en) * | 2022-08-23 | 2022-11-01 | 太仓沪试试剂有限公司 | Open type enamel reaction kettle of linkage crushing assembly and method for preparing dipotassium hydrogen phosphate by adopting reaction kettle |
| CN115253979A (en) * | 2022-08-23 | 2022-11-01 | 太仓沪试试剂有限公司 | Open type enamel reaction kettle and method for preparing sodium nitrate by adopting same |
-
2012
- 2012-11-21 CN CN201210473990.1A patent/CN103832988A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891465A (en) * | 2015-05-29 | 2015-09-09 | 湖北三宁化工股份有限公司 | Method for preparing potassium dihydrogen phosphate from industrial monoammonium phosphate mother solution |
| CN105948011A (en) * | 2016-05-06 | 2016-09-21 | 四川安达农森科技股份有限公司 | Preparation method of potassium dihydrogen phosphate |
| CN107804832A (en) * | 2017-11-16 | 2018-03-16 | 达州瓮福蓝剑化工有限责任公司 | A kind of neutralized by the heating of dense mother liquor obtains the method for potassium dihydrogen phosphate |
| CN109987594A (en) * | 2019-04-01 | 2019-07-09 | 太仓沪试试剂有限公司 | A kind of preparation method of potassium dihydrogen phosphate |
| CN112321348A (en) * | 2020-11-17 | 2021-02-05 | 李东峰 | Nitrogen-phosphorus-potassium water-soluble fertilizer and preparation method thereof |
| CN114057172A (en) * | 2021-12-29 | 2022-02-18 | 山东省神农生态科技股份有限公司 | Method for producing monopotassium phosphate by recovering potassium ions in corn steep liquor and monopotassium phosphate produced by method |
| CN114057172B (en) * | 2021-12-29 | 2023-01-20 | 山东省神农生态科技股份有限公司 | Method for producing monopotassium phosphate by recovering potassium ions in corn steep liquor and monopotassium phosphate produced by method |
| CN115253980A (en) * | 2022-08-23 | 2022-11-01 | 太仓沪试试剂有限公司 | Open type enamel reaction kettle of linkage crushing assembly and method for preparing dipotassium hydrogen phosphate by adopting reaction kettle |
| CN115253979A (en) * | 2022-08-23 | 2022-11-01 | 太仓沪试试剂有限公司 | Open type enamel reaction kettle and method for preparing sodium nitrate by adopting same |
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Application publication date: 20140604 |