CN101412523A - Preparation of high-purity potassium cyanate - Google Patents
Preparation of high-purity potassium cyanate Download PDFInfo
- Publication number
- CN101412523A CN101412523A CNA2008101568346A CN200810156834A CN101412523A CN 101412523 A CN101412523 A CN 101412523A CN A2008101568346 A CNA2008101568346 A CN A2008101568346A CN 200810156834 A CN200810156834 A CN 200810156834A CN 101412523 A CN101412523 A CN 101412523A
- Authority
- CN
- China
- Prior art keywords
- potassium cyanate
- purity
- urea
- reaction
- solvent
- 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 a method for preparing high-purity potassium cyanate, which belongs to preparation of the potassium cyanate. The method takes industrial urea and potassium carbonate as raw materials and dimethyl sulfoxide or dimethyl formamide as a solvent, and adopts proper technological conditions: the reaction temperature is 130 DEG C, the reaction time is 8 hours, the mol ratio of the urea to the potassium carbonate is 3.5 to 1, and the mass ratio of the solvent to the urea is 7 to 1; the product with 96 percent (mass fraction) of the potassium cyanate can be obtained, and the obtained potassium cyanate is washed by adopting anhydrous alcohol as a detergent, wherein the amount of the detergent is 3 to 4 times of the volume of the potassium cyanate; and the potassium cyanate after washing is dried, and the potassium cyanate with the purity of more than 98 percent (mass fraction) can be obtained. The method has the advantages that the technology is simple and easy and the purity of the prepared potassium cyanate is as high as more than 98 percent (mass fraction).
Description
Technical field
The present invention relates to the preparation method of potassium cyanate, specifically is a kind of preparation method of high-purity potassium cyanate.
Background technology
Potassium cyanate of many uses can be used for producing soporific and anaesthetic, as weedicide, defoliant and organic synthesis, in addition, also is widely used in glass manufacturing, ceramic art, metallic surface hardening treatment, fertilizer, agrochemical field.
The method of synthetic potassium cyanate has solid-state melting method, absorption process, liquid phase absorption process, liquid and solid phase reaction method etc., and wherein the liquid and solid phase reaction method has raw material sources and is easy to get, and is easy and simple to handle, easily and the characteristics of separated from solvent, good economy performance, is suitable for suitability for industrialized production.
In the liquid and solid phase reaction method, the great invention with Gao Muqing of high mountain justice that changes into company with Japan is comparatively advanced, and this invention is the synthetic potassium cyanate of solvent with the dimethyl formamide.The reaction of synthetic potassium cyanate is undertaken by reflux type usually, has the reaction unit that the solvent that can make evaporation flows back to the condenser of reactor so must use.The consumption of solvent is generally by 0.5-10 times (weight) of amount of urea, is preferably in 1-3 times the scope.Temperature of reaction is generally 100 ℃--and 200 ℃, be preferably between the boiling point (DMF's is 150 ℃) of 100 ℃ and solvent and choose.Reaction pressure, adopt normal pressure or pressurization can, but see that from work angle to adopt normal pressure better.Reaction times, generally in 1-10 hours scopes, product purity had 94% (weight).
At present, the demand to the potassium cyanate product on the world market is bigger, and the potassium cyanate that China produces is mainly used in outlet, and manufacturer is few, exists that technology is immature, potassium cyanate content is low in the product, does not reach external producer and requires (〉 96%) problem.
Summary of the invention
The invention provides a kind of preparation method of high-purity potassium cyanate.The potassium cyanate product purity that makes with the present invention〉98%.
The present invention realizes with following technical scheme: a kind of preparation method of high-purity potassium cyanate is characterized in that with industrial urea and salt of wormwood preparing as solvent reaction with dimethyl sulfoxide (DMSO) or dimethyl formamide as raw material; The mol ratio of its urea and salt of wormwood is 3.5:1, and the mass ratio of solvent and urea is 7:1; Concrete preparation process is as follows:
1) solvent is heated to 130 ℃, adds raw material salt of wormwood while stirring, treat that stable back adds the reaction that urea synthesizes potassium cyanate, the temperature of reaction in the reaction process is 130 ℃, the material after reaction times 8h must reflect;
2) reacted material is cooled to room temperature, vacuum filtration then, drying is cooled to room temperature again, purity be 96% (mass fraction) potassium cyanate;
3) be that 96% potassium cyanate adds detergent washing with purity, after left standstill 4 hours, vacuum filtration, drying is cooled to room temperature, the potassium cyanate (KOCN) of Chun Du ≧ 98.2% (mass fraction); Described washing composition is a dehydrated alcohol.
The invention has the beneficial effects as follows: simple for process, the potassium cyanate purity that makes is up to more than 98% (mass fraction).
Embodiment
Further specify preparation method of the present invention below in conjunction with embodiment.
Embodiment
Solvent dimethyl sulfoxide (DMSO) 109.2g is added in the three-necked bottle, start electric mixer, connect the electrically heated cover, regulate powerstat, heated solvent to 130 ℃, regulating electric mixer simultaneously stirs, add salt of wormwood 10g, treat that stable back adds urea 15.6g, will keep desired temperature of reaction in the reaction process.Question response stops heating and stirs after 8 hours.Material in the three-necked bottle is cooled to room temperature, and vacuum filtration was delivered in the thermostatic drying chamber 105 ℃ of down dry half an hour, was cooled to room temperature in moisture eliminator, and the weighing product quality can get 10.5 gram potassium cyanates, and potassium cyanate purity is 96.4%.
10.5 gram potassium cyanates are put into beaker, add 42 gram dehydrated alcohols, stir the back and placed 4 hours, vacuum filtration was delivered in the thermostatic drying chamber 105 ℃ of down dry half an hour, was cooled to room temperature in moisture eliminator, purity is 98.2% potassium cyanate.
Claims (1)
1, a kind of preparation method of high-purity potassium cyanate is characterized in that with industrial urea and salt of wormwood preparing as solvent reaction with dimethyl sulfoxide (DMSO) or dimethyl formamide as raw material; The mol ratio of urea and salt of wormwood is 3.5:1, and the mass ratio of solvent and urea is 7:1; Concrete preparation process is as follows:
1) solvent is heated to 130 ℃, adds raw material salt of wormwood while stirring, treat that stable back adds the reaction that urea synthesizes potassium cyanate, the temperature of reaction in the reaction process is 130 ℃, and reaction times 8h gets reacted material;
2) reacted material is cooled to room temperature, vacuum filtration then, drying is cooled to room temperature again, purity be 96% potassium cyanate;
3) be to leave standstill 4 hours after 96% potassium cyanate adds detergent washing purity, vacuum filtration, drying is cooled to room temperature, the potassium cyanate of Chun Du ≧ 98.2%; Described washing composition is a dehydrated alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101568346A CN101412523A (en) | 2008-09-27 | 2008-09-27 | Preparation of high-purity potassium cyanate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101568346A CN101412523A (en) | 2008-09-27 | 2008-09-27 | Preparation of high-purity potassium cyanate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101412523A true CN101412523A (en) | 2009-04-22 |
Family
ID=40593294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101568346A Pending CN101412523A (en) | 2008-09-27 | 2008-09-27 | Preparation of high-purity potassium cyanate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101412523A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955206A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Metod for preparing sodium carbonate heptahydrate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN101955207A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing sodium carbonate and ammonium sulfate from waste obtained in process of producing sodium cyanate by urea method |
| CN101955208A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing sodium carbonate decahydrate and ammonium sulfate from waste obtained by producing sodium cyanate with urea method |
| CN101955205A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing monohydrate sodium carbonate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN101955204A (en) * | 2010-05-27 | 2011-01-26 | 汪晋强 | Method for preparing potassium carbonate dihydrate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN101962199A (en) * | 2010-05-27 | 2011-02-02 | 汪晋强 | Method for preparing potassium carbonate monohydrate and ammonium sulfate from waste obtained from producing sodium cyanate by urea method |
| CN101962201A (en) * | 2010-05-27 | 2011-02-02 | 汪晋强 | Method for preparing potassium carbonate and ammonium sulfate from wastes obtained in the process of producing sodium cyanate by urea method |
| CN102336416A (en) * | 2011-08-29 | 2012-02-01 | 湖北得力新材料有限公司 | Method for cleanly producing high-purity cyanate at low temperature |
| CN109911915A (en) * | 2019-04-02 | 2019-06-21 | 湖南立德科技新材料有限公司 | The method of continuous processing production photoelectricity grade potassium cyanate |
-
2008
- 2008-09-27 CN CNA2008101568346A patent/CN101412523A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955206A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Metod for preparing sodium carbonate heptahydrate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN101955207A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing sodium carbonate and ammonium sulfate from waste obtained in process of producing sodium cyanate by urea method |
| CN101955208A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing sodium carbonate decahydrate and ammonium sulfate from waste obtained by producing sodium cyanate with urea method |
| CN101955205A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing monohydrate sodium carbonate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN101955204A (en) * | 2010-05-27 | 2011-01-26 | 汪晋强 | Method for preparing potassium carbonate dihydrate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN101962199A (en) * | 2010-05-27 | 2011-02-02 | 汪晋强 | Method for preparing potassium carbonate monohydrate and ammonium sulfate from waste obtained from producing sodium cyanate by urea method |
| CN101962201A (en) * | 2010-05-27 | 2011-02-02 | 汪晋强 | Method for preparing potassium carbonate and ammonium sulfate from wastes obtained in the process of producing sodium cyanate by urea method |
| CN101955205B (en) * | 2010-05-27 | 2012-09-05 | 王嘉兴 | Method for preparing monohydrate sodium carbonate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN101955206B (en) * | 2010-05-27 | 2012-09-05 | 王嘉兴 | Metod for preparing sodium carbonate heptahydrate and ammonium sulfate from wastes produced in process for producing sodium cyanate by urea method |
| CN102336416A (en) * | 2011-08-29 | 2012-02-01 | 湖北得力新材料有限公司 | Method for cleanly producing high-purity cyanate at low temperature |
| CN109911915A (en) * | 2019-04-02 | 2019-06-21 | 湖南立德科技新材料有限公司 | The method of continuous processing production photoelectricity grade potassium cyanate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101412523A (en) | Preparation of high-purity potassium cyanate | |
| CN102070535A (en) | Preparing method for synthesizing sanmate from calcium cyanamide | |
| CN108187719A (en) | A kind of C3N4-Mt-SO3H composite materials and its preparation and application | |
| CN101462980B (en) | Industrial production method of 2,6-difluorobenzamide | |
| CN106008586A (en) | POSS-containing high temperature-resistant solid ionic liquid and preparation method thereof | |
| CN101671283A (en) | Preparation method of columnar crystal taurine | |
| CN108586265A (en) | Pentanediamine sebacate and its crystal | |
| CN106336446B (en) | A kind of preparation method of potassium glycyrrhizana | |
| CN106336341A (en) | Process for synthesizing ethyl chloride | |
| Wang et al. | Co-crystal of Ti 4 Ni 2 and Ti 8 Ni 4 clusters with enhanced photochemical properties | |
| CN107892649A (en) | A kind of preparation method of 9,9 pairs of (4 aminophenyl) fluorenes | |
| CN108160095A (en) | A kind of preparation method and application of the catalyst without mercury of acetylene hydrochlorination reaction | |
| CN101665406B (en) | Method for synthesizing 4,4-bis(chloromethyl) biphenyl | |
| CN108546248B (en) | Preparation method of 1, 2-dihydro-3, 6-pyridazine dione | |
| CN103319326A (en) | Preparation method for vanadyl oxalate | |
| Pan et al. | Solubility and crystallization of BaHPO4 crystals | |
| CN1284725C (en) | Method of producing sodium formate method sodium hydrosulfite using liquid sulfur dioxide and solid sodium carbonate | |
| CN105566283A (en) | Chiral crown ether containing ent-beyeren skeleton, and preparation method and application thereof | |
| CN1199857C (en) | Method for preparing nano mesoporous silicon dioxide from green gram rock | |
| CN101328174B (en) | Method for preparing 3-(2-chloroethyl)-2-methyl-4H- naphthyridine[1,2-a]pyrimidine-4-ketone | |
| CN105523565B (en) | Vapor assisted Solid-state converts the method for preparing W molecular sieves | |
| CN104447290A (en) | Method for preparing 2,4-dichlorophenoxyacetic acid | |
| CN109096222A (en) | A kind of 2,6- accelerine base thiazine chemical synthesis process | |
| CN220386510U (en) | Device for continuously producing sodium tert-butoxide | |
| CN106588623A (en) | Method for preparing magnesium acetate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20090422 |