CN104140087A - Orthophosphorous acid production method - Google Patents
Orthophosphorous acid production method Download PDFInfo
- Publication number
- CN104140087A CN104140087A CN201310168814.1A CN201310168814A CN104140087A CN 104140087 A CN104140087 A CN 104140087A CN 201310168814 A CN201310168814 A CN 201310168814A CN 104140087 A CN104140087 A CN 104140087A
- Authority
- CN
- China
- Prior art keywords
- phosphorous acid
- reaction
- phosphorus trichloride
- production method
- orthophosphorous acid
- 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
Abstract
The invention discloses an orthophosphorous acid production method, and belongs to the field of the fine chemical industry. Orthophosphorous acid is prepared through phosphorus trichloride hydrolysis, crude orthophosphorous acid crystallization and centrifugal drying with phosphorus trichloride, an orthophosphorous acid saturated liquid and water as raw materials and a hydrolysis reaction kettle, a crystallization reaction kettle and a centrifugal drier as devices. The orthophosphorous acid production method has the main advantages of use of general devices, short production cycle, no emission of toxic harmful gases or liquids, production of hydrochloric acid by recovering a byproduct hydrogen chloride gas, and obtaining of industrial grade orthophosphorous acid. Orthophosphorous acid can be used as a reducing agent, a pesticide intermediate or a nylon whitening agent, can be a phosphate preparation raw material, can be a raw material for preparing plastic stabilizers and organophosphorus pesticides, can be a polycarbonate stabilizer, can be used as an antioxidant of nylon 1010, and can also be used as a chemical reagent.
Description
Technical field
The invention belongs to field of fine chemical, relate in particular to a kind of production method of phosphorous acid.
Background technology
Phosphorous acid is a kind of oxygen acid of phosphorus, and molecular formula is H3PO3, and molecular weight is 82.00, and fusing point is 74 DEG C, and boiling point is 200 DEG C, and outward appearance is clear crystal; Phosphorous acid is diprotic acid, belongs to mineral compound, and its acidity is slightly stronger than phosphoric acid, and it has strong reducing property, easily silver ion reduction is become to argent, sulfate reduction can be become to sulfurous gas, has strong water absorbability and deliquescence, is corrosive; Soluble in water and alcohol, in air, slow oxidation becomes phosphoric acid, is decomposed into phosphuret-(t)ed hydrogen and phosphoric acid 180 DEG C time.The synthetic route of phosphorous acid generally adopts: 1. hydrolysis method, and by phosphorus trichloride hydrolysis, through steam refining, crystallisation by cooling and obtaining; 2. be dissolved in concentrated hydrochloric acid by phosphorus trichloride, then boil off hydrochloric acid and obtain in low temperature; Also can by phosphorus trioxide slowly and water effect generate; The present invention produces phosphorous acid by hydrolysis method.The purposes of phosphorous acid is: be used as reductive agent and pesticide intermediate, nylon whitening agent; Being the raw material of manufacturing phosphite, is also the raw material of manufacturing stabilizer for plastics and organophosphorus pesticide; As the stablizer of polycarbonate, be also used as the antioxidant of nylon 1010; As chemical reagent, also can be used for producing High-efficient Water treatment agent Amino Trimethylene Phosphonic Acid.The present invention, taking phosphorus trichloride, phosphorous acid saturated solution, water as raw material, taking hydrolytic reaction pot, condensing crystal still, centrifugal drier as equipment, makes phosphorous acid by the hydrolysis of phosphorus trichloride, the operation such as crystallization, centrifugal drying of phosphorous acid crude product.The method is produced the major advantage of phosphorous acid: the equipment of use for general-purpose equipment, with short production cycle, without toxic and harmful and liquid discharge, the recyclable hydrochloric acid of making of byproduct hydrogen chloride gas, the product obtaining is technical grade phosphorous acid.
Summary of the invention
The problem that the present invention mainly solves is to provide a kind of method of producing phosphorous acid in batches, the method is taking phosphorus trichloride, phosphorous acid saturated solution, water as raw material, taking hydrolytic reaction pot, condensing crystal still, centrifugal drier as equipment, make phosphorous acid finished product by the hydrolysis of phosphorus trichloride, the operation such as condensing crystal, centrifugal drying of phosphorous acid crude product, the raw material weight proportioning that the present invention uses is: phosphorus trichloride 23-25%, phosphorous acid saturated solution 4%, water 71-73%.
The present invention can be achieved through the following technical solutions:
A production method for phosphorous acid, is characterized in that being made up of following steps:
(1) water of formula ratio and phosphorous acid saturated solution are sent into hydrolytic reaction pot, starting agitator stirs, the rotating speed of agitator is 35-45 rev/min, the phosphorus trichloride of formula ratio is splashed in hydrolytic reaction pot slowly, exothermic heat of reaction, the speed that drips phosphorus trichloride by control is carried out temperature of reaction in controlled hydrolysis reactor between 82-86 DEG C, after dropwising, phosphorus trichloride stops stirring, insulation reaction 1.2-1.4 hour, the hydrogen chloride gas that reaction obtains reclaims and makes hydrochloric acid, and remaining liquid is phosphorous acid aqueous solution.
(2) by phosphorous acid aqueous solution by pumping condensing crystal still condensing crystal, after phosphorous acid crystallization, remaining moisture is discharged, phosphorous acid after crystallization is sent into centrifugal drier and is carried out high speed drying, and making phosphorous acid water content is to obtain finished product after 0.5-1%, sends into phosphorous acid storage tank stores.
Temperature of reaction in hydrolytic reaction pot described in step (1) is 84 DEG C; The insulation reaction time is 1.3 hours.
The described finished product phosphorous acid water content of step (2) is 0.75%.
The invention has the beneficial effects as follows: a kind of production method of phosphorous acid is provided, and the advantage of the method is: the equipment of use for general-purpose equipment, with short production cycle, product purity is high, without toxic and harmful and liquid discharge, can be mass.
Embodiment
Embodiment 1
Be 71% water and to account for total amount be that 4% phosphorous acid saturated solution is sent into hydrolytic reaction pot by accounting for total amount, starting agitator stirs, the rotating speed of agitator is 35-45 rev/min, be that 25% phosphorus trichloride splashes in hydrolytic reaction pot slowly by accounting for total amount, exothermic heat of reaction, the speed that drips phosphorus trichloride by control is carried out temperature of reaction in controlled hydrolysis reactor at 82 DEG C, after dropwising, phosphorus trichloride stops stirring, insulation reaction 1.4 hours, the hydrogen chloride gas that reaction obtains reclaims and makes hydrochloric acid, and remaining liquid is phosphorous acid aqueous solution.By phosphorous acid aqueous solution by the crystallization of pumping condensing crystal still, after phosphorous acid crystallization, remaining moisture is discharged, phosphorous acid after crystallization is sent into centrifugal drier and is carried out high speed drying, and making phosphorous acid water content is to obtain finished product after 0.5-1%, sends into phosphorous acid storage tank stores.
Embodiment 2
Be 72% water and to account for total amount be that 4% phosphorous acid saturated solution is sent into hydrolytic reaction pot by accounting for total amount, starting agitator stirs, the rotating speed of agitator is 35-45 rev/min, be that 24% phosphorus trichloride splashes in hydrolytic reaction pot slowly by accounting for total amount, exothermic heat of reaction, the speed that drips phosphorus trichloride by control is carried out temperature of reaction in controlled hydrolysis reactor at 84 DEG C, after dropwising, phosphorus trichloride stops stirring, insulation reaction 1.3 hours, the hydrogen chloride gas that reaction obtains reclaims and makes hydrochloric acid, and remaining liquid is phosphorous acid aqueous solution.By phosphorous acid aqueous solution by the crystallization of pumping condensing crystal still, after phosphorous acid crystallization, remaining moisture is discharged, phosphorous acid after crystallization is sent into centrifugal drier and is carried out high speed drying, and making phosphorous acid water content is to obtain finished product after 0.5-1%, sends into phosphorous acid storage tank stores.
Embodiment 3
Be 73% water and to account for total amount be that 4% phosphorous acid saturated solution is sent into hydrolytic reaction pot by accounting for total amount, starting agitator stirs, the rotating speed of agitator is 35-45 rev/min, be that 23% phosphorus trichloride splashes in hydrolytic reaction pot slowly by accounting for total amount, exothermic heat of reaction, the speed that drips phosphorus trichloride by control is carried out temperature of reaction in controlled hydrolysis reactor at 86 DEG C, after dropwising, phosphorus trichloride stops stirring, insulation reaction 1.2 hours, the hydrogen chloride gas that reaction obtains reclaims and makes hydrochloric acid, and remaining liquid is phosphorous acid aqueous solution.By phosphorous acid aqueous solution by the crystallization of pumping condensing crystal still, after phosphorous acid crystallization, remaining moisture is discharged, phosphorous acid after crystallization is sent into centrifugal drier and is carried out high speed drying, and making phosphorous acid water content is to obtain finished product after 0.5-1%, sends into phosphorous acid storage tank stores.
Claims (3)
1. a production method for phosphorous acid, the raw material of use comprises: phosphorus trichloride 23-25%, phosphorous acid saturated solution 4%, water 71-73%; It is characterized in that: step (1) is sent the water of formula ratio and phosphorous acid saturated solution into hydrolytic reaction pot, starting agitator stirs, the rotating speed of agitator is 35-45 rev/min, the phosphorus trichloride of formula ratio is splashed in hydrolytic reaction pot slowly, exothermic heat of reaction, the speed that drips phosphorus trichloride by control is carried out temperature of reaction in controlled hydrolysis reactor between 82-86 DEG C, after dropwising, phosphorus trichloride stops stirring, insulation reaction 1.2-1.4 hour, the hydrogen chloride gas that reaction obtains reclaims and makes hydrochloric acid, and remaining liquid is phosphorous acid aqueous solution; Step (2 by phosphorous acid aqueous solution by pumping condensing crystal still condensing crystal, after phosphorous acid crystallization, remaining moisture is discharged, phosphorous acid after crystallization is sent into centrifugal drier and is carried out high speed drying, and making phosphorous acid water content is to obtain finished product after 0.5-1%, sends into phosphorous acid storage tank stores.
2. the production method of a kind of phosphorous acid as claimed in claim 1, the feature of its step (1) is: the temperature of reaction in described hydrolytic reaction pot is 84 DEG C; The insulation reaction time is 1.3 hours.
3. the production method of a kind of phosphorous acid as claimed in claim 1, the feature of its step (2) is: described finished product phosphorous acid water content is 0.75%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310168814.1A CN104140087A (en) | 2013-05-09 | 2013-05-09 | Orthophosphorous acid production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310168814.1A CN104140087A (en) | 2013-05-09 | 2013-05-09 | Orthophosphorous acid production method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104140087A true CN104140087A (en) | 2014-11-12 |
Family
ID=51849444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310168814.1A Pending CN104140087A (en) | 2013-05-09 | 2013-05-09 | Orthophosphorous acid production method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104140087A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190382541A1 (en) * | 2015-10-23 | 2019-12-19 | Covestro Deutschland Ag | Method for producing polycarbonate molding compositions with improved thermal processing stability |
| CN112724056A (en) * | 2020-12-28 | 2021-04-30 | 安道麦安邦(江苏)有限公司 | Method and device for effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butylthiourea mother liquor to improve yield |
| 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 |
| CN114572947A (en) * | 2021-12-17 | 2022-06-03 | 临沂市春明化工有限公司 | Phosphorous acid crystallization process |
-
2013
- 2013-05-09 CN CN201310168814.1A patent/CN104140087A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190382541A1 (en) * | 2015-10-23 | 2019-12-19 | Covestro Deutschland Ag | Method for producing polycarbonate molding compositions with improved thermal processing stability |
| US10844182B2 (en) * | 2015-10-23 | 2020-11-24 | Covestro Deutschland Ag | Method for producing polycarbonate molding compositions with improved thermal processing stability |
| CN112724056A (en) * | 2020-12-28 | 2021-04-30 | 安道麦安邦(江苏)有限公司 | Method and device for effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butylthiourea mother liquor to improve yield |
| 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 |
| CN114572947A (en) * | 2021-12-17 | 2022-06-03 | 临沂市春明化工有限公司 | Phosphorous acid crystallization process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104140087A (en) | Orthophosphorous acid production method | |
| CN102311100B (en) | Method for preparing potassium hydrogen peroxymonosulfate composite salt | |
| CN104944398B (en) | Glyphosate mother solution recoverying and utilizing method | |
| CN1923700A (en) | Method of producing calcium chloride from industrial waste carbide slag | |
| CN103524352A (en) | Method for recovering glycine acid-binding agent triethylamine employing triethylamine method | |
| CN101823704B (en) | Method for continuously synthesizing phosphorous acid | |
| CN101786744A (en) | Method for directly utilizing waste liquor containing phosphoric acid and phosphorous acid | |
| CN106629644A (en) | Method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage monoammonium phosphate | |
| CN105480959A (en) | Method for producing monopotassium phosphate by fluoride salt purification process | |
| CN109206343A (en) | A kind of preparation method of adiponitrile | |
| CN203284212U (en) | Novel industrial-grade phosphorous acid production device | |
| CN202924739U (en) | Novel device for producing phosphorous acid | |
| CN101734634A (en) | Method for producing monopotassium phosphate | |
| CN1332113A (en) | Prepn of sodium percarbonate | |
| CN103819505B (en) | A kind of method improving PMIDA yield | |
| CN104140086A (en) | Mechanical device for producing industrial grade orthophosphorous acid | |
| CN103303883B (en) | A kind of production technique of phosphorus oxychloride | |
| CN102502570B (en) | Production method of medical sodium metavanadate | |
| CN107540001A (en) | A kind of ammonium acid fluoride production technology | |
| CN205419779U (en) | Novel production of high -purity phosphorous oxychloride device | |
| CN103723696A (en) | Preparation method of calcium phosphite | |
| CN107161971A (en) | A kind of preparation technology of magnesium dihydrogen phosphate | |
| CN107176860A (en) | A kind of ultrahigh concentration P-K fertilizer and preparation method | |
| CN100432082C (en) | Synthesis method of chloro diisopropyl phosphine | |
| CN104555962B (en) | Method for increasing defluorination rate of high-impurity concentrated phosphoric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141112 |