CN1324760A - Production process of potassium dihydrogen phosphate - Google Patents
Production process of potassium dihydrogen phosphate Download PDFInfo
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- CN1324760A CN1324760A CN 01107208 CN01107208A CN1324760A CN 1324760 A CN1324760 A CN 1324760A CN 01107208 CN01107208 CN 01107208 CN 01107208 A CN01107208 A CN 01107208A CN 1324760 A CN1324760 A CN 1324760A
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Abstract
A production method of potassium dihydrogen phosphate includes the following steps: using phosphoric acid and potassium chloride to make them produce double decompositino reaction to produce potassium dihydric pyrophosphate and hydrogen chloride gas; hydrolizing potassium dihydri pyrophosphate to produce potassium dihydrogen phosphate; and the equipment used can solve the problems of mixed hydrochloric and phosphoric acids corrosion and expansion due to heating. Said invention product can reach the quality obtained by using neutralization process of phosphoric acid and potassium hydroxide, so that it can greatly save cost of raw material.
Description
The invention relates to a method for producing potassium dihydrogen phosphate by using potassium chloride and phosphoric acid as raw materials.
At present, the production method of potassium dihydrogen phosphate still adopts the traditional neutralization method of potassium hydroxide and hot phosphoric acid, and the method is simple, because the used potassium raw material is potassium hydroxide secondarily processed by a potash plant, the price is high, and other methods are as follows: although the raw materials are low in price, the processes are complex, the flow is too long, the utilization rate of the raw materials is low, the corrosion of equipment cannot be solved, and the synergistic production of byproducts is considered, so that the ideal effect cannot be achieved.
The invention aims to provide a method for producing potassium dihydrogen phosphate by using potassium chloride and phosphoric acid as raw materials, which solves the problems that the heat transfer and corrosion resistance of equipment and long heat and cold contraction cannot be solved during high-temperature reaction, and reduces the cost.
The purpose of the invention is realized as follows:
the production principle of the invention is as follows: potassium chloride is used for carrying out double decomposition reaction with phosphoric acid to generate hydrochloric acid and potassium dihydrogen pyrophosphate, and then the potassium dihydrogen pyrophosphate is hydrolyzed into potassium dihydrogen phosphate by adding water.
The specific process of the invention is as follows: adding phosphoric acid into a reaction kettle, adding potassium chloride, heating through heat conduction oil, and escaping hydrogen chloride gas; absorbing by-product hydrochloric acid through water, adding water into slurry which generates potassium dihydrogen pyrophosphate in a reaction kettle for hydrolysis, cooling, crystallizing and separating to obtain a potassium dihydrogen phosphate product, and therefore, the method is characterized by comprising the following steps of:
A. feeding phosphoric acid and potassium chloride into a reaction kettle;
B. heating the reaction mass by dividing walls;
C. hydrogen chloride gas generated by the reaction is absorbed by liquid;
D. adding water into the reaction materials for heating and hydrolyzing;
E. cooling and crystallizing the hydrolyzed material, separating out monopotassium phosphate, and drying a monopotassium phosphate semi-finished product;
F. the separated mother liquor is returned to the step A to be used as the ingredient of the raw materials of phosphorus and potassium.
The reaction kettle is sealed by a graphite ring through a tongue-and-groove and is heated by adopting a heat conduction oil dividing wall.
The amount of phosphoric acid and potassium chloride added is according to H3PO4The molar ratio of KCl is 1.1-1.8, and the optimal molecular ratio is 1.2-1.5.
The reaction temperature of the invention is 150-250 ℃, and the optimal reaction temperature is 180-220 ℃.
The reaction time of the invention is 1.5-4 hours, and the optimal reaction time is 2.0-3.0 hours.
The hydrogen chloride gas removed by the reaction of the invention is absorbed by liquid, the liquid is water and alkaline solution thereof, the reaction product of the invention is added with water for heating hydrolysis, and the concentration of the hydrolysis material is P2O5The optimal hydrolyzed material concentration is 30-60 percentDegree is P2O5The content is 35-45%.
The hydrolysis temperature of the invention is 90-130 ℃, and the optimal hydrolysis temperature is 100-120 ℃.
The hydrolyzed material is cooled and crystallized, and the mother liquid after the potassium dihydrogen phosphate is separated is returned to the first reaction procedure and is used as the raw material to be mixed. After a plurality of cycles, the mother liquor and the product are discarded when the magnesium and sodium content is higher, and the mother liquor and the product are used for other purposes.
The invention aims to solve the problem that the materialof a reaction kettle is used under the condition of high-temperature corrosion of mixed acid of phosphoric acid and hydrochloric acid, the contact part of the reaction kettle and a reaction medium is made of graphite material impregnated with tetrafluoro, and the graphite material is easy to fall off under the condition of temperature change due to the difference of expansion coefficients between a steel material and a binder in a common graphite lining and a lining, and has poor heat transfer performance when the steel transfers heat to graphite. The invention adopts an integral graphite ring, is sealed by a tongue-and-groove tetrafluoro pad, directly heats graphite by a heat conducting medium, transfers heat to reaction feed liquid, and is processed by selecting integral graphite from an upper end socket and a lower end socket of a reaction kettle.
The reaction kettle adopts the technology of the application of another utility model of the applicant, which is a special reaction kettle suitable for the production method of the monopotassium phosphate, and the two are mutually matched for use, thereby better realizing the aim of the invention.
The invention adopts the reaction of potassium chloride and phosphoric acid to replace the raw material for producing potassium dihydrogen phosphate by the reaction of potassium hydroxide and phosphoric acid, thereby greatly reducing the production cost, and reducing the cost of each ton of products by 1000 yuan. The adopted reaction equipment solves the problems of high temperature, high corrosion, difficult heating and industrialized reaction equipment failure of the method.
The figures and the description of the figures of the present invention are given below:
FIG. 1 is a process flow diagram of the present invention
Inthe figure: 1-reaction kettle 2-hydrochloric acid absorption tower
3-hydrolysis tank 4-core machine
FIG. 2: reaction kettle structure diagram
The invention is further illustrated by the following figures and examples.
The first embodiment is as follows:
210g of phosphoric acid (containing P) was taken2O558.68%) in 500cm3Into a flask, 101g of potassium chloride (containing K) was added2O:59.6％；Cl-46.73%), i.e., the P/Cl molecular ratio is 1.3. Heating the flask on an electric heating jacket, introducing air when the temperature of the materials is raised to 108 ℃, exhausting gas after water absorption, evacuating, continuously heating to 220 ℃, keeping the temperature for 2.5 hours, and then adding water to P2O5The mixture was heated to 110 ℃ at a concentration of 40% and hydrolyzed for 1 hour. Cooling, crystallizing and separating the materials to obtain 115gThe potassium dihydrogen phosphate product has the following product quality: p2O552.73％、K2O34.18％、Cl-:0.08％、H2O:1.17％。
Example two:
210g of phosphoric acid (containing P) was taken2O558.68%) in 500cm3Into the flask, 86.8g of potassium chloride (containing K) was added2O:59.6％；Cl-46.73%), i.e., the P/Cl molecular ratio is 1.5. Heating the flask on an electric heating jacket, introducing air when the temperature of the materials is raised to 108 ℃, exhausting gas after water absorption, evacuating, continuously heating to 180 ℃, keeping the temperature for 2.5 hours, and then adding water to P2O5The mixturewas heated to 110 ℃ at a concentration of 40% and hydrolyzed for 1 hour. Cooling, crystallizing and separating the materials to obtain 88.25g of monopotassium phosphate product, wherein the product quality is as follows: p2O552.04％、K2O33.38％、Cl-:0.15％、H2O:1.85％。
Example three:
according to the method of the first embodiment, mother liquor after cooling, crystallizing and separating the product is used as raw material, and the amount of the mother liquor is subtracted from the amount of the added phosphoric acid and potassium chloride. The cyclic production is carried out, and the results are shown in the table I. K2The single yield of O is 65 percent, and the return rate of phosphoric acid is 43 percent。
Example four:
a reactor according to the design of FIG. 2 was charged with 840kg of phosphoric acid (P)2O561.5%) and 440kg of potassium chloride (K)2O60.3%), removing gas, absorbing with water, heating the reaction material to 220 deg.C with heat-conducting oil, maintaining for 2.5 hr, placing the reaction material in a hydrolysis tank, adding water to the material P2O5The concentration is 40%, the temperature is raised to 110 ℃, and the hydrolysis is carried out for 1 hour. The materials are cooled, crystallized and centrifugally separated, and the mother liquid is returned to the reaction tank to be used as the ingredients of the reaction materials. Drying the centrifugal semi-finished product to obtain a monopotassium phosphate product, wherein the mass of the monopotassium phosphate product is as follows: p2O552.6％、K2O33.06％、Cl-:0.18％、H20.82 percent of O, absorbing the exhaust gas into hydrochloric acidthrough water, wherein the HCl content is 28 percent
The invention reduces the production cost, and the adopted reaction equipment solves the problems of high temperature, high corrosion, difficult heating and incapability of industrialization of the method.
Claims (14)
1. A method for producing monopotassium phosphate is characterized by comprising the following steps:
A. feeding phosphoric acid and potassium chloride into a reaction kettle;
B. heating the reaction mass by dividing walls;
C. hydrogen chloride gas generated by the reaction is absorbed by liquid;
D. adding water into the reaction materials for heating and hydrolyzing;
E. cooling and crystallizing the hydrolyzed material, separating out monopotassium phosphate, and drying a monopotassium phosphate semi-finished product;
F. the separated mother liquor is returned to the step A to be used as the ingredient of the raw materials of phosphorus and potassium.
2. The method for producing monopotassium phosphate according to claim 1, wherein: the reaction kettle is a graphite ring sealed by a tongue-and-groove and is heated by adopting a heat conducting oil dividing wall.
3. The method for producing monopotassium phosphate according to claim 1, wherein: adding phosphoric acid and potassium chloride in the amount of H3PO4The molar ratio of/KCl is 1.1-1.8.
4. The method for producing monopotassium phosphate according to claim 1, wherein:the reaction temperature is 150-250 ℃.
5. The method for producing monopotassium phosphate according to claim 1, wherein: the reaction time is 1.5-4 hours.
6. The method for producing monopotassium phosphate according to claim 1, wherein: the hydrogen chloride gas removed by the reaction is absorbed by a liquid, which is water and its alkaline solution.
7. The method for producing monopotassium phosphate according to claim 1, wherein: adding water into the reaction product, heating and hydrolyzing, wherein the concentration of the hydrolyzed material is P2O5The content is 30-60%.
8. The method for producing monopotassium phosphate according to claim 1, wherein: the hydrolysis temperature is 90-130 ℃.
9. The method for producing monopotassium phosphate according to claim 1, wherein: cooling and crystallizing the hydrolyzed material, separating mother liquor of potassium dihydrogen phosphate, and returning to the first reaction process as raw material. After a plurality of cycles, the mother liquor and the product are discarded when the magnesium and sodium content is higher, and the mother liquor and the product are used for other purposes.
10. The method for producing monopotassium phosphate according to claim 1 or 3, wherein: adding phosphoric acid and potassium chloride in the amount of H3PO4The molar ratio of/KCl is 12-15.
11. The method for producing monopotassium phosphate according to claim 1 or 4, wherein: the reaction temperature is 180-220 ℃.
12. The method for producing monopotassium phosphate according to claim 1 or 5, wherein: the reaction time is 20-3.0 hours.
13. The method for producing monopotassium phosphate according to claim 1 or 7, wherein: concentration of hydrolyzed material is represented by P2O5The content is 35-45%.
14. The method for producing monopotassium phosphate according to claim 1 or 8, wherein: the hydrolysis temperature is 100-120 ℃.
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| CN 01107208 CN1324760A (en) | 2001-02-28 | 2001-02-28 | Production process of potassium dihydrogen phosphate |
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| CN 01107208 CN1324760A (en) | 2001-02-28 | 2001-02-28 | Production process of potassium dihydrogen phosphate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343053B (en) * | 2008-08-29 | 2010-05-12 | 四川川恒化工股份有限公司 | Method for preparing composite phosphate |
| CN102167298A (en) * | 2010-12-29 | 2011-08-31 | 武汉同源药业有限公司 | Preparation method of high-purity dipotassium phosphate crude drug |
| CN102530902A (en) * | 2011-11-24 | 2012-07-04 | 广西力源肥业科技农化有限公司 | Industrialized continuous potassium dihydrogen phosphate production method |
| CN102862964A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Device and method for producing monopotassium phosphate by using double decomposition |
| CN103569981A (en) * | 2012-08-02 | 2014-02-12 | 浙江新安化工集团股份有限公司 | Method for producing orthophosphate products from polyphosphates through hydrolysis |
| CN103879981A (en) * | 2014-03-19 | 2014-06-25 | 钟林 | Method for preparing potassium dihydrogen phosphate by using extraction residual acid of phosphoric acid |
| CN104477864A (en) * | 2014-12-22 | 2015-04-01 | 什邡圣地亚化工有限公司 | Technology for producing phosphate from pyrophosphate |
| CN109422548A (en) * | 2017-09-01 | 2019-03-05 | 陈运谋 | The method of the agricultural liquid potassium dihydrogen phosphate of mobile process units preparation synergy |
| CN109896893A (en) * | 2019-03-15 | 2019-06-18 | 王新勇 | A kind of high concentration fulvic acid potassium dihydrogen phosphate preparation method |
-
2001
- 2001-02-28 CN CN 01107208 patent/CN1324760A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343053B (en) * | 2008-08-29 | 2010-05-12 | 四川川恒化工股份有限公司 | Method for preparing composite phosphate |
| CN102167298A (en) * | 2010-12-29 | 2011-08-31 | 武汉同源药业有限公司 | Preparation method of high-purity dipotassium phosphate crude drug |
| CN102167298B (en) * | 2010-12-29 | 2012-08-29 | 武汉同源药业有限公司 | Preparation method of high-purity dipotassium phosphate crude drug |
| CN102530902A (en) * | 2011-11-24 | 2012-07-04 | 广西力源肥业科技农化有限公司 | Industrialized continuous potassium dihydrogen phosphate production method |
| CN102530902B (en) * | 2011-11-24 | 2014-08-20 | 广西力源肥业科技农化有限公司 | Industrialized continuous potassium dihydrogen phosphate production method |
| CN103569981B (en) * | 2012-08-02 | 2018-08-31 | 浙江新安化工集团股份有限公司 | A method of hydrolyzing production orthophosphates product with condensed phosphate |
| CN103569981A (en) * | 2012-08-02 | 2014-02-12 | 浙江新安化工集团股份有限公司 | Method for producing orthophosphate products from polyphosphates through hydrolysis |
| CN102862964A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Device and method for producing monopotassium phosphate by using double decomposition |
| CN102862964B (en) * | 2012-09-08 | 2014-07-23 | 湖北三宁化工股份有限公司 | Device and method for producing monopotassium phosphate by using double decomposition |
| CN103879981A (en) * | 2014-03-19 | 2014-06-25 | 钟林 | Method for preparing potassium dihydrogen phosphate by using extraction residual acid of phosphoric acid |
| CN103879981B (en) * | 2014-03-19 | 2016-02-17 | 钟林 | A kind of method utilizing phosphoric acid raffinate to prepare potassium primary phosphate |
| CN104477864A (en) * | 2014-12-22 | 2015-04-01 | 什邡圣地亚化工有限公司 | Technology for producing phosphate from pyrophosphate |
| CN109422548A (en) * | 2017-09-01 | 2019-03-05 | 陈运谋 | The method of the agricultural liquid potassium dihydrogen phosphate of mobile process units preparation synergy |
| CN109896893A (en) * | 2019-03-15 | 2019-06-18 | 王新勇 | A kind of high concentration fulvic acid potassium dihydrogen phosphate preparation method |
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