CN1235876C - Prepn of guanidyl thiocyanate - Google Patents
Prepn of guanidyl thiocyanate Download PDFInfo
- Publication number
- CN1235876C CN1235876C CN 03158319 CN03158319A CN1235876C CN 1235876 C CN1235876 C CN 1235876C CN 03158319 CN03158319 CN 03158319 CN 03158319 A CN03158319 A CN 03158319A CN 1235876 C CN1235876 C CN 1235876C
- Authority
- CN
- China
- Prior art keywords
- guanidine thiocyanate
- thiocyanate
- present
- weight
- guanidine
- 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.)
- Expired - Fee Related
Links
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 title description 3
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 title 1
- ZJYYHGLJYGJLLN-UHFFFAOYSA-N guanidinium thiocyanate Chemical compound SC#N.NC(N)=N ZJYYHGLJYGJLLN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 230000018044 dehydration Effects 0.000 claims abstract description 4
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012043 crude product Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- STIAPHVBRDNOAJ-UHFFFAOYSA-N carbamimidoylazanium;carbonate Chemical compound NC(N)=N.NC(N)=N.OC(O)=O STIAPHVBRDNOAJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- LYOTWQPVTCLBHB-UHFFFAOYSA-N cyanatosulfanyl cyanate;guanidine Chemical compound NC(N)=N.N#COSOC#N LYOTWQPVTCLBHB-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for preparing chemical products, particularly to a method for preparing guanidine thiocyanate. The present invention comprises the following technological processes: a. melting; b. dissolution; c. filtration; d. dehydration; e. crystallization. Thus, high-purity guanidine thiocyanate is obtained. The present invention has the advantages of simple and practical technology and reasonable principle. The guanidine thiocyanate prepared by the method of the present invention has the advantages of good quality and high purity reach more than 99%, and is greatly popular with users.
Description
Affiliated technical field
The present invention relates to a kind of production method of Chemicals, especially the preparation method of guanidine thiocyanate.
Background technology
Guanidine thiocyanate, chemical name: thiocyanic acid imido urea, English name: Guanidine thio cyanate salt, its molecular formula is: (NH
2)
2C:NHHSCN (118.2).Be the white crystals body, 116～121 ℃ of fusing points, in the time of 20 ℃, the pH value of 6mol/L in water is 4.5～6, solubleness is dissolving fully.Can be used as biochemical reagents, medicine intermediate.Be used for the oil prodution industry degreasing, the strong fat degradation agents of conduct in the daily-use chemical industry, the membranolysis agent in the bio-pharmaceuticals.Its structural formula is:
Present production technique, the product purity that obtains are not very high, and in use, some occasion is just very high to the purity requirement of guanidine thiocyanate.
Summary of the invention
In order to overcome existing guanidine thiocyanate preparation method's deficiency, the invention provides a kind of method, this method can obtain highly purified guanidine thiocyanate.
The technical solution adopted for the present invention to solve the technical problems is: a kind of guanidine thiocyanate preparation method has following technical process:
A, be that 2: 1 Guanidinium carbonate and ammonium thiocyanate put into reactor with weight ratio, 50～90 ℃ of reactions 2 hours down, the guanidine thiocyanate crude product;
B, dissolving, at normal temperatures, the guanidine thiocyanate crude product is water-soluble by weight 1: 1 ratio;
C, filtration are removed impurity such as raw material and reaction by-product with filtering method;
D, dehydration are at high temperature dewatered the mother liquor after filtering;
E, crystallization, supersaturated solution cooling, condensing crystal has obtained purity greater than 99% guanidine thiocyanate.
Further: again through b, c, d, e step, is 1: 1 with the part by weight of water in the b step with the guanidine thiocyanate after the e step wherein, for drawing purity greater than 99.9% guanidine thiocyanate, can repeatedly repeat this step.
Its reaction formula is:
Features simple and practical process of the present invention, principle is reasonable, and with the guanidine thiocyanate of the inventive method preparation, quality is good, and the purity height can reach 99.9%, is highly commended by customers deeply.
Embodiment
A kind of guanidine thiocyanate preparation method has following technical process: a, is that 2: 1 Guanidinium carbonate and ammonium thiocyanate put into reactor with weight ratio, 50～90 ℃ of reactions 2 hours down, the guanidine thiocyanate crude product;
B, dissolving, at normal temperatures, the guanidine thiocyanate crude product is water-soluble by weight 1: 1 ratio;
C, filtration are removed impurity such as raw material and reaction by-product with filtering method;
D, dehydration are at high temperature dewatered the mother liquor after filtering;
E, crystallization, supersaturated solution cooling, condensing crystal has obtained purity greater than 99% guanidine thiocyanate.
Further: again through b, c, d, e step, is 1: 1 with the part by weight of water in the b step with the guanidine thiocyanate after the e step wherein, for drawing purity greater than 99.9% guanidine thiocyanate, can repeatedly repeat this step.
Claims (2)
1. guanidine thiocyanate preparation method is characterized in that having following technical process:
A, be that 2: 1 Guanidinium carbonate and ammonium thiocyanate put into reactor with weight ratio, 50～90 ℃ of reactions 2 hours down, the guanidine thiocyanate crude product;
B, dissolving, at normal temperatures, the guanidine thiocyanate crude product is water-soluble by weight 1: 1 ratio;
C, filtration are removed impurity such as raw material and reaction by-product with filtering method;
D, dehydration are at high temperature dewatered the mother liquor after filtering;
E, crystallization, supersaturated solution cooling, condensing crystal has obtained purity greater than 99% guanidine thiocyanate.
2. guanidine thiocyanate preparation method according to claim 1, it is characterized in that: with the guanidine thiocyanate after the e step again through b, c, d, e step, be 1: 1 with the part by weight of water in the b step wherein,, can repeatedly repeat this step for drawing purity greater than 99.9% guanidine thiocyanate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03158319 CN1235876C (en) | 2003-09-19 | 2003-09-19 | Prepn of guanidyl thiocyanate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03158319 CN1235876C (en) | 2003-09-19 | 2003-09-19 | Prepn of guanidyl thiocyanate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1526701A CN1526701A (en) | 2004-09-08 |
| CN1235876C true CN1235876C (en) | 2006-01-11 |
Family
ID=34287248
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03158319 Expired - Fee Related CN1235876C (en) | 2003-09-19 | 2003-09-19 | Prepn of guanidyl thiocyanate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1235876C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209856A (en) * | 2020-10-15 | 2021-01-12 | 苏州亚科科技股份有限公司 | Preparation method of guanidine thiocyanate |
-
2003
- 2003-09-19 CN CN 03158319 patent/CN1235876C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1526701A (en) | 2004-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101489970B (en) | The preparation method of succinic acid | |
| CN105236452A (en) | Technology for producing highly pure potassium nitrate through reaction of sodium nitrate and potassium chloride | |
| CN1173943C (en) | Process for producing 2-hydroxy-4-methylthiobutyric acid | |
| CN1171103A (en) | Milamine purifying process | |
| CN1235876C (en) | Prepn of guanidyl thiocyanate | |
| CN1247536C (en) | Process for preparing guanidine hydrochloride | |
| CN1234596C (en) | Process for preparing fluorine compound and SiO2 from sodium fluosilicate | |
| CN109534369A (en) | A kind of film is integrated to prepare lithium chloride device and method thereof | |
| CN1616434A (en) | Method for producing 1,3-dimethyl -2-imidazolinone | |
| CN1164572C (en) | Process for preparing dimethyl sulfone | |
| CN113845433B (en) | Method for efficiently preparing beta-aminopropionic acid from acrylic acid | |
| CN101066915A (en) | Synthesis of 2,4-D | |
| CN1056368C (en) | Preparation process of albendazole | |
| CN102633701B (en) | Synthesis method of S-methyl isothiourea salt | |
| CN111732133A (en) | Preparation method of tetraamminepalladium sulfate | |
| EP0427435A1 (en) | Process for direct isolation of captopril | |
| CN114369073B (en) | Method for preparing high-purity hydrochlorothiazide | |
| CN118184546B (en) | Preparation method of O-methyl-N-nitroisourea | |
| CN110343046A (en) | A kind of production method improving paranitrochlorobenzene purity | |
| CN1663946A (en) | Method for preparing and purifying cyanate | |
| CN101830831B (en) | Method for preparing ortho-diazanyl benzonitrile | |
| CN116655679B (en) | Hexamethyldisiloxane and preparation method thereof | |
| US7161029B2 (en) | DiL-lysine monosulfate trihydrate crystal and method of making | |
| CN1583718A (en) | Preparation of nickel sulphamate | |
| CN112375084A (en) | Purification and preparation method of ixabepilone with stable crystal form |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |