CN115285953A - Phosphorus trichloride hydrolysis preparation process - Google Patents
Phosphorus trichloride hydrolysis preparation process Download PDFInfo
- Publication number
- CN115285953A CN115285953A CN202210781467.9A CN202210781467A CN115285953A CN 115285953 A CN115285953 A CN 115285953A CN 202210781467 A CN202210781467 A CN 202210781467A CN 115285953 A CN115285953 A CN 115285953A
- Authority
- CN
- China
- Prior art keywords
- reaction
- phosphorus trichloride
- tank
- hydrochloric acid
- hydrolysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000126 substance Substances 0.000 claims abstract description 21
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005507 spraying Methods 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 239000003595 mist Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000008213 purified water Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 2
- 239000000203 mixture Substances 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/163—Phosphorous acid; Salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention discloses a phosphorus trichloride hydrolysis preparation process, which comprises the following preparation steps: s1, carrying out hydrolysis preparation, and connecting equipment; s2, performing hydrolysis reaction, namely reacting water mist with phosphorus trichloride; s3, absorbing substances, namely absorbing the substances generated by the reaction by adopting water dissolving and spraying; s4, separating hydrochloric acid, and preserving heat to evaporate the hydrochloric acid; s5, phosphorous acid crystals are crystallized from phosphorous acid. Through above-mentioned structure, react through atomizing water and phosphorus trichloride, the material after the reaction combines with the fog, and subsequent dissolving of being convenient for, and can make material and temperature after the reaction transmit, make its reation kettle inside temperature be convenient for control, through spraying and inside and water dissolve, can make the reactant fuse comparatively smoothly, make it fuse completely, can not cause the waste.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a phosphorus trichloride hydrolysis preparation process.
Background
Most of the production methods of the internal phosphorous acid use phosphorus trichloride as a raw material to prepare the phosphorous acid through hydrolysis. The production process is that water or phosphorous acid saturated solution in certain amount is added into hydrolysis reactor in certain proportion, phosphorus trichloride solution is dropped slowly into the reactor, the dropping speed and reaction temperature of phosphorus trichloride solution are controlled strictly, and the hydrogen chloride gas produced in the reaction is absorbed in several stages of water bubbling absorber to produce 25-30% by-product hydrochloric acid. After the phosphorus trichloride is dripped in the hydrolysis reaction, reacting for one hour, pumping a phosphorous acid mixture synthesized by the hydrolysis reaction into a distillation deacidification kettle by using a pump, carrying out negative pressure distillation concentration until hydrogen chloride and water in the phosphorous acid mixture are evaporated to dryness, then putting the mixture into a crystallization kettle for cooling crystallization, and separating an uncrystallized mother solution by centrifugal separation to obtain qualified crystal phosphorous acid.
And because phosphorus trichloride can produce a large amount of heat, the temperature of its reaction is higher, and difficult control makes the reactant gasification, thereby leads to that subsequent processing procedure is comparatively complicated.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art, and provides a phosphorus trichloride hydrolysis preparation process, which reduces the reaction temperature and simplifies the subsequent processes.
The invention also provides a phosphorus trichloride hydrolysis preparation process, which comprises the following preparation processes:
s1, carrying out hydrolysis preparation
Connecting a reaction kettle, a dissolving tank, a separation tank and a collecting tank, wherein an atomizer is arranged at the edge of a reaction kettle object;
s2, hydrolysis reaction
Phosphorus trichloride is placed in a reaction kettle, a large amount of atomized purified water is blown into the reaction kettle through an atomizer, hydrolysis reaction is carried out on phosphorus trichloride in the reaction kettle, a soaking effect cannot be generated, the reaction is smooth, heat is released in the reaction, phosphorous acid and hydrochloric acid generated in the reaction are combined with subsequently generated water mist, and the generated water mist is transmitted to a dissolving tank;
s3. Substance absorption
S2, transferring the substances generated by the reaction in the S2 to a dissolving tank through a transmission pipe, and after the substances are dissolved by an internal water source in the dissolving tank, spraying and dissolving the substances through a spraying pipe above the dissolving tank again to enable the substances to fall into the tank body;
s4, separating hydrochloric acid
Preserving the temperature of the mixed solution obtained in the step S3 through a separation box to evaporate the internal hydrochloric acid solution, enabling the internal hydrochloric acid solution to reach a collection tank, and collecting the solution after condensation;
s5. Phosphorous acid crystal
And (3) distilling and deacidifying the solution after hydrochloric acid separation in a deacidification kettle under negative pressure for concentration, and cooling and crystallizing after distillation to obtain phosphorous acid crystals.
According to the phosphorus trichloride hydrolysis preparation process provided by the invention, the bottom of the reaction kettle is provided with the conical hopper, and the phosphorus trichloride is positioned in the conical hopper.
According to the hydrolysis preparation process of phosphorus trichloride provided by the invention, the atomizer in S1 atomizes by ultrasonic waves, and the temperature of atomized water is 10-14 ℃.
According to the hydrolysis preparation process of phosphorus trichloride, provided by the invention, the water sources in the dissolving tanks are all 0-1 ℃, and the two dissolving tanks are communicated with each other.
According to the phosphorus trichloride hydrolysis preparation process provided by the invention, the temperature inside the separation box is 80-90 ℃, and the slow stirring is carried out during heat preservation.
According to the hydrolysis preparation process of phosphorus trichloride, the pressure in the dissolving tank is 30-50 mmHg.
According to the phosphorus trichloride hydrolysis preparation process provided by the invention, water and trace hydrochloric acid in the solution are removed by negative pressure distillation and concentration.
According to the hydrolysis preparation process of phosphorus trichloride provided by the invention, the cooling crystallization temperature is 35-40 ℃.
Advantageous effects
Compared with the prior art, the invention has obvious and prominent substantive characteristics and remarkable advantages:
1. according to the invention, atomized water reacts with phosphorus trichloride, and the reacted substance is combined with mist, so that subsequent dissolution is facilitated, the reacted substance and temperature can be transmitted, and the internal temperature of the reaction kettle can be conveniently controlled.
2. According to the invention, through spraying and dissolving the inner part of the reactor with water, the reactants can be smoothly fused, so that the reactants are completely fused, and waste is avoided.
Detailed Description
This section will describe in detail specific embodiments of the present invention so that one can intuitively and visually understand each technical feature and the whole technical solution of the present invention, but it should not be construed as limiting the scope of the present invention.
The phosphorus trichloride hydrolysis preparation process provided by the embodiment of the invention comprises the following preparation processes:
s1, carrying out hydrolysis preparation
Connecting a reaction kettle, a dissolving box, a separating box and a collecting tank, arranging an atomizer at the edge of a reaction kettle object, wherein the atomizer is communicated with the reaction kettle, the dissolving box, the separating box and the collecting tank are sequentially communicated, a conical hopper is arranged at the bottom of the reaction kettle, and phosphorus trichloride is positioned in the conical hopper;
s2, hydrolysis reaction
Phosphorus trichloride is placed in a conical hopper of a reaction kettle, so that fog is in contact with the phosphorus trichloride, a large amount of atomized purified water is blown into the reaction kettle through an atomizer, the atomizer atomizes water through ultrasonic waves, the temperature of the atomized water is 10-14 ℃, phosphorous acid and hydrochloric acid are generated through hydrolysis reaction with the phosphorus trichloride in the reaction kettle, a soaking effect cannot be generated, the reaction is smooth, in addition, in the reaction heat release, the phosphorous acid generated in the reaction is combined with the hydrochloric acid and subsequent generated water mist, the generated fog is transmitted to a dissolving tank, an air pump can be increased to transmit the fog more quickly, and heat is transmitted;
s3. Substance absorption
S2, transferring the substances generated by the reaction in the dissolving tank into the dissolving tank through a transmission pipe, wherein the pressure in the dissolving tank is 30-50 mmHg, after the substances are dissolved by an internal water source in the dissolving tank, spraying and dissolving the substances by a spraying pipe above the dissolving tank again to enable the substances to fall into the tank body, and performing bidirectional dissolving to facilitate complete dissolving of the generated substances, wherein the water sources in the dissolving tank are all 0-1 ℃, so that the temperature of the water sources is slowly increased, and the two dissolving tanks are communicated with each other and can dissolve the rest undissolved parts of the water sources;
s4, separating hydrochloric acid
Keeping the temperature of the mixed solution obtained in the step (3) through a separation box, wherein the temperature inside the separation box is 80-90 ℃, and slowly stirring the mixed solution during keeping the temperature to evaporate the internal hydrochloric acid solution to reach a collection tank, condensing the internal hydrochloric acid solution and collecting the internal hydrochloric acid solution to obtain a hydrochloric acid solution;
s5. Phosphorous acid crystal
And (3) distilling and deacidifying the solution after hydrochloric acid separation in a deacidification kettle at negative pressure for distillation concentration to remove water and trace hydrochloric acid in the solution, cooling and crystallizing after distillation is finished, wherein the cooling and crystallizing temperature is 35-40 ℃, and thus, a phosphorous acid crystal is obtained.
When the method is used for preparation, the continuous reaction can be carried out for a long time, the internal concentration of the obtained solution is high, and the subsequent treatment is convenient.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (8)
1. A phosphorus trichloride hydrolysis preparation process is characterized by comprising the following preparation processes:
s1, carrying out hydrolysis preparation
Connecting a reaction kettle, a dissolving tank, a separation tank and a collecting tank, and arranging an atomizer at the edge of a reaction kettle object;
s2, hydrolysis reaction
Phosphorus trichloride is placed in a reaction kettle, a large amount of atomized purified water is blown into the reaction kettle through an atomizer, hydrolysis reaction is carried out on phosphorus trichloride in the reaction kettle, a soaking effect cannot be generated, the reaction is smooth, heat is released in the reaction, phosphorous acid and hydrochloric acid generated in the reaction are combined with subsequently generated water mist, and the generated water mist is transmitted to a dissolving tank;
s3. Substance absorption
S2, transferring the substances generated by the reaction in the S2 to a dissolving tank through a transmission pipe, and after the substances are dissolved by an internal water source in the dissolving tank, spraying and dissolving the substances through a spraying pipe above the dissolving tank again to enable the substances to fall into the tank body;
s4, separating hydrochloric acid
Preserving the temperature of the mixed solution obtained in the step S3 through a separation box to evaporate the internal hydrochloric acid solution, enabling the internal hydrochloric acid solution to reach a collection tank, and collecting the solution after condensation;
s5. Phosphorous acid crystal
And (3) distilling and deacidifying the solution after hydrochloric acid separation in a deacidification kettle under negative pressure for concentration, and cooling and crystallizing after distillation to obtain phosphorous acid crystals.
2. The hydrolysis preparation process of phosphorus trichloride according to claim 1, wherein a conical hopper is installed at the bottom of the reaction kettle, and the phosphorus trichloride is located inside the conical hopper.
3. The hydrolysis preparation process of phosphorus trichloride according to claim 1, wherein the atomizer in S1 atomizes by ultrasonic waves, and the temperature of atomized water is 10 ℃ to 14 ℃.
4. The hydrolysis preparation process of phosphorus trichloride according to claim 1, wherein the water source inside the dissolution tank is 0 ℃ to 1 ℃, and the dissolution tank has two parts which are communicated with each other.
5. The hydrolysis preparation process of phosphorus trichloride according to claim 1, wherein the temperature inside the separation tank is 80 ℃ to 90 ℃ and the slow stirring is performed while the temperature is maintained.
6. The process of claim 1, wherein the pressure in the dissolution tank is 30-50 mmHg.
7. The process of claim 1, wherein the negative pressure distillation concentration is used to remove water and trace hydrochloric acid from the solution.
8. The process of claim 1, wherein the cooling crystallization temperature is 35-40 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210781467.9A CN115285953A (en) | 2022-07-04 | 2022-07-04 | Phosphorus trichloride hydrolysis preparation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210781467.9A CN115285953A (en) | 2022-07-04 | 2022-07-04 | Phosphorus trichloride hydrolysis preparation process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115285953A true CN115285953A (en) | 2022-11-04 |
Family
ID=83822068
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210781467.9A Pending CN115285953A (en) | 2022-07-04 | 2022-07-04 | Phosphorus trichloride hydrolysis preparation process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115285953A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201395512Y (en) * | 2009-05-13 | 2010-02-03 | 河南清水源科技股份有限公司 | Reaction vessel used for producing orthophosphorous acid |
| CN102249202A (en) * | 2011-06-16 | 2011-11-23 | 江苏大明科技有限公司 | Preparation process for synthesizing phosphorous acid by hydrolyzing phosphorous trichloride |
| CN204550062U (en) * | 2015-04-13 | 2015-08-12 | 四川贝尔化工集团有限公司 | A kind of for the phosphorous acid reaction unit in pmida98 production technique |
| CN114291799A (en) * | 2021-12-17 | 2022-04-08 | 临沂市春明化工有限公司 | Production process of high-purity phosphorous acid |
-
2022
- 2022-07-04 CN CN202210781467.9A patent/CN115285953A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201395512Y (en) * | 2009-05-13 | 2010-02-03 | 河南清水源科技股份有限公司 | Reaction vessel used for producing orthophosphorous acid |
| CN102249202A (en) * | 2011-06-16 | 2011-11-23 | 江苏大明科技有限公司 | Preparation process for synthesizing phosphorous acid by hydrolyzing phosphorous trichloride |
| CN204550062U (en) * | 2015-04-13 | 2015-08-12 | 四川贝尔化工集团有限公司 | A kind of for the phosphorous acid reaction unit in pmida98 production technique |
| CN114291799A (en) * | 2021-12-17 | 2022-04-08 | 临沂市春明化工有限公司 | Production process of high-purity phosphorous acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104944398B (en) | Glyphosate mother solution recoverying and utilizing method | |
| CN102311100B (en) | Method for preparing potassium hydrogen peroxymonosulfate composite salt | |
| CN103880625A (en) | Method for preparing D, L-mandelic acid and derivative of D, L-mandelic acid | |
| CN103524352A (en) | Method for recovering glycine acid-binding agent triethylamine employing triethylamine method | |
| CN106745099A (en) | A kind of method that utilization lithium phosphate prepares lithium carbonate | |
| CN104910031B (en) | The combine production method and device of glycine and hydantoins | |
| CN109180508A (en) | A kind of method of electrodialytic membranes separation production glycine | |
| CN106629644B (en) | A method of producing industrial level-one and LITHIUM BATTERY monoammonium phosphate with chemical fertilizer grade monoammonium phosphate | |
| CN215756458U (en) | Device for reducing content of mechanical impurities in phosphorus pentafluoride | |
| CN115285953A (en) | Phosphorus trichloride hydrolysis preparation process | |
| CN111606335B (en) | Clean comprehensive utilization method of potassium salt-containing mother liquor | |
| CN101555209A (en) | Clean producing method of aminoacetic acid with chloroactic acid ammonolysis method | |
| CN203048602U (en) | Device for producing industrial-scale monoammonium phosphate by using wet-process phosphoric acid | |
| CN216808418U (en) | Sodium sulfate waste water resourceful treatment system | |
| CN113443768A (en) | Gelatin wastewater recycling method and treatment system | |
| CN210595276U (en) | Production system for co-production of monoammonium phosphate from monopotassium phosphate | |
| CN111517972A (en) | Preparation method of environment-friendly betaine | |
| CN103274921B (en) | Device and method for preparing calcium formate by utilizing yellow phosphorus tail gas | |
| CN113461616A (en) | Synthesis process of 2-methyl-5-nitroimidazole | |
| CN112479960B (en) | Vitamin D 3 Purification method of (2) | |
| CN104355990A (en) | Method for recycling and mechanically using L- (+) -tartaric acid in D-ethyl ester production | |
| CN109455742B (en) | Method for simply producing pharmaceutic adjuvant anhydrous sodium sulfite | |
| CN210710760U (en) | System for producing caprolactam from caprolactam sulfate and feed-grade calcium hydrophosphate | |
| CN107540001A (en) | A kind of ammonium acid fluoride production technology | |
| CN104176718A (en) | Method for preparing calcium hypophosphite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20221104 |