CN107840811A - A kind of preparation method of dicyandiamide - Google Patents
A kind of preparation method of dicyandiamide Download PDFInfo
- Publication number
- CN107840811A CN107840811A CN201711345594.XA CN201711345594A CN107840811A CN 107840811 A CN107840811 A CN 107840811A CN 201711345594 A CN201711345594 A CN 201711345594A CN 107840811 A CN107840811 A CN 107840811A
- Authority
- CN
- China
- Prior art keywords
- dicyandiamide
- urea
- preparation
- reaction
- pocl3
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of chemical synthesis, specifically provides a kind of preparation method of dicyandiamide, and this method carries out dehydration polymerization reaction with urea and POCl3 in the presence of acid binding agent triethylamine and dicyandiamide is made；Reaction is carried out under 50 DEG C, condition of normal pressure, reaction terminate after through alkali cleaning, filtering, extraction, concentrate and produce；The method of the present invention prepares dicyandiamide by urea dehydration, can effectively solve the problems, such as caused waste residue in traditional handicraft, and this method also has the advantages that energy-conservation, green, high income, simple technique.
Description
Technical field
The invention belongs to the field of chemical synthesis, more particularly to a kind of preparation method of dicyandiamide.
Background technology
Dicyandiamide (dicyanodiamine) chemical formula is as follows：
It is the dimer of cyanamide, and the cyano derivative of guanidine, white crystalline powder, water-soluble, alcohol, DMF etc., it is several
Ether and benzene are not dissolved in, non-combustible, drying is stable.Dicyandiamide is a kind of important fine-chemical intermediate raw material, is used extensively
In medicine, dyestuff, agricultural chemicals, electronics, lubricant etc..Such as：In medicine synthesizes, for preparing sulfa drugs and guanidine nitrate
Deng.
The traditional processing technology of dicyandiamide is hydrolyzed by lime nitrogen, while is passed through carbon dioxide by body into reaction system
Calcium in system precipitates as calcium carbonate, and filtering and concentrating obtains cyanamide solution, then makes single cyanogen in the basic conditions
Dimerization occurs for amine, through supercooling, crystallization, separate, be dried to obtain dicyandiamide.Its reaction equation：
2CaCN2+2H2O→Ca(HCN2)2+Ca(OH)2
Ca(HCN2)2+CO2+H2O→2H2NCN+CaCO3
Above-mentioned lime nitrogen hydrolysis prepares cyanamide, produces substantial amounts of waste residue, and the production pollution environment of lime nitrogen raw material
Very serious, energy consumption is big.Under instantly severe Environmental Protection Situation, it is necessary to and must more new production process.
The content of the invention
The present invention is directed to many weak points existing for prior art, there is provided a kind of preparation method of dicyandiamide, the party
Method carries out dehydration polymerization reaction with urea and POCl3 in the presence of acid binding agent and dicyandiamide is made；Reaction is in 50 DEG C, normal pressure
Under the conditions of carry out, reaction terminate after through alkali cleaning, filtering, extraction, concentrate and produce；The method of the present invention is prepared double by urea dehydration
Cyanamide, can effectively solve the problems, such as caused waste residue in traditional handicraft, and this method also has energy-conservation, green, high income, work
The advantages that skill is simple.
The concrete technical scheme of the present invention is as follows：
A kind of preparation method of dicyandiamide, is comprised the following steps that：
Urea and triethylamine are disposably added in tetrahydrofuran, afterwards at interval of 20 minutes, divides 6 times and averagely adds three
Chlorethoxyfos, at 40~60 DEG C, reacted 5~7 hours under normal pressure, reaction terminate rear product through alkali cleaning, filtering, extract, be concentrated to give
Dicyandiamide；
Wherein the mol ratio of POCl3 and urea is 1:3~6；
The mol ratio of POCl3 and triethylamine is 1:3~10；
The mass ratio of urea and tetrahydrofuran is 1:4~8.
The specific chemical equation of above-mentioned reaction is as follows：
In methods described, alkali cleaning uses the NaHCO of saturation3Solution.
In methods described, extractant is from any one in ethyl acetate, butyl acetate.
Described alkali cleaning, filtering, extraction, concentration are ordinary skill in the art scheme, and inventor will not be repeated here；
The existing technique for preparing dicyandiamide is to first pass through lime nitrogen to prepare cyanamide, then polymerize and prepare dicyandiamide, and this
The above-mentioned technique of invention then realizes the step dehydration acquisition cyanamide of urea by choosing special dehydrating agent and acid binding agent,
Cyanamide still realizes the process that cyanamide polymerization obtains dicyandiamide while generation, realize one kettle way and prepare dicyandiamide,
Such scheme will not produce waste residue compared with prior art, and raw material urea is cheap and easy to get, overcome in traditional handicraft with lime
The shortcomings of nitrogen is highly energy-consuming, high pollution existing for the preparation of raw material.
In summary, dicyandiamide is prepared by urea dehydration using above-mentioned technique, effectively can solved in traditional handicraft
Caused waste residue problem, this method also have the advantages that energy-conservation, green, high income, simple technique.
Embodiment
Embodiment 1：
0.05mol urea, 30mL tetrahydrofurans, 0.045mol triethylamines, afterwards at interval of 20 are added into four-hole boiling flask
Minute, divide 6 times and 0.015mol POCl3s are averagely added portionwise, stirred 5 hours at 45 DEG C, system is in pale yellow transparent liquid
Body.Reaction is evaporated under reduced pressure away solvent after terminating, with the NaCO of saturation3Product of distillation is washed, adds the salt in ethanol removing system,
Filtering.Product is extracted with ethyl acetate again, is analyzed through liquid-matter, liquid phase quantitative analysis, conversion rate of urea 100%, yield is
92.9%.
Embodiment 2：
0.5mol urea, 150mL tetrahydrofurans, 0.45mol triethylamines, afterwards at interval of 20 points are added into four-hole boiling flask
Clock, divide 6 times and 0.15mol POCl3s are averagely added portionwise, stirred 6 hours at 55 DEG C, system is in light yellow transparent liquid.Instead
Solvent is evaporated under reduced pressure away after should terminating, with the NaHCO of saturation3Product of distillation is washed, adds the salt in ethanol removing system, mistake
Filter.Product is extracted with ethyl acetate again, is analyzed through liquid-matter, liquid phase quantitative analysis, conversion rate of urea 100%, yield is
87.3%.
Claims (3)
- A kind of 1. preparation method of dicyandiamide, it is characterised in that：Comprise the following steps that：Urea and triethylamine are disposably added in tetrahydrofuran, afterwards at interval of 20 minutes, divides 6 times and averagely adds trichlorine oxygen Phosphorus, at 40~60 DEG C, reacted 5~7 hours under normal pressure, reaction terminate rear product through alkali cleaning, filtering, extract, be concentrated to give double cyanogen Amine；Wherein the mol ratio of POCl3 and urea is 1:3~6；The mol ratio of POCl3 and triethylamine is 1:3~10；The mass ratio of urea and tetrahydrofuran is 1:4~8.
- 2. the preparation method of dicyandiamide according to claim 1, it is characterised in that：The alkali cleaning uses the NaHCO of saturation3 Solution.
- 3. the preparation method of dicyandiamide according to claim 1, it is characterised in that：The extractant from ethyl acetate, Any one in butyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711345594.XA CN107840811A (en) | 2017-12-15 | 2017-12-15 | A kind of preparation method of dicyandiamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711345594.XA CN107840811A (en) | 2017-12-15 | 2017-12-15 | A kind of preparation method of dicyandiamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107840811A true CN107840811A (en) | 2018-03-27 |
Family
ID=61663960
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711345594.XA Pending CN107840811A (en) | 2017-12-15 | 2017-12-15 | A kind of preparation method of dicyandiamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107840811A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113511988A (en) * | 2021-08-20 | 2021-10-19 | 四川金象赛瑞化工股份有限公司 | System and method for preparing dicyandiamide by using urea |
| CN113527144A (en) * | 2021-08-06 | 2021-10-22 | 四川金象赛瑞化工股份有限公司 | Production method of cyanamide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1028126B (en) * | 1952-01-17 | 1958-04-17 | American Cyanamid Co | Process for the preparation of a mixture containing melamine and cyanamide from urea |
| CN102728400A (en) * | 2011-04-15 | 2012-10-17 | 中国石油化工股份有限公司 | Catalyst for preparing cyanamide by dehydrating urea and its preparation method |
| CN105984888A (en) * | 2015-02-16 | 2016-10-05 | 福建金东阳化工工贸有限公司 | Process for preparing hydrogen cyanamide by utilizing urea |
-
2017
- 2017-12-15 CN CN201711345594.XA patent/CN107840811A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1028126B (en) * | 1952-01-17 | 1958-04-17 | American Cyanamid Co | Process for the preparation of a mixture containing melamine and cyanamide from urea |
| CN102728400A (en) * | 2011-04-15 | 2012-10-17 | 中国石油化工股份有限公司 | Catalyst for preparing cyanamide by dehydrating urea and its preparation method |
| CN105984888A (en) * | 2015-02-16 | 2016-10-05 | 福建金东阳化工工贸有限公司 | Process for preparing hydrogen cyanamide by utilizing urea |
Non-Patent Citations (3)
| Title |
|---|
| BOYD, G. V ET AL: "Product class 12: oxazoles", 《SCIENCE OF SYNTHESIS》 * |
| 汪多仁: "尿素常压脱水制备氰胺", 《四川化工与腐蚀控制》 * |
| 汪多仁编: "《绿色农药与化肥中间体》", 30 April 2009, 北京科学技术文献出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527144A (en) * | 2021-08-06 | 2021-10-22 | 四川金象赛瑞化工股份有限公司 | Production method of cyanamide |
| CN113511988A (en) * | 2021-08-20 | 2021-10-19 | 四川金象赛瑞化工股份有限公司 | System and method for preparing dicyandiamide by using urea |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI685488B (en) | Method for preparing intermediate of Azotomin (Azoxystyrin) | |
| CN107840811A (en) | A kind of preparation method of dicyandiamide | |
| CN103755739A (en) | Continuous production method for N-NBPT | |
| CN101486481A (en) | Method for coproduction of ammonia sulfate and superfine light calcium carbonate from fluorgypsum | |
| CN103664717A (en) | Preparation method of cheap and environmentally friendly D, L-2- hydroxyl-4-methylthio butyric acid | |
| CN102382034B (en) | Synthetic method of N-amino-3-azabicyclo[3,3,0]octane hydrochloride | |
| CN105503842A (en) | Method for preparing nebivolol hydrochloride epoxy intermediate 6-fluoro-2-epoxy ethyl chroman | |
| CN102503810B (en) | Method for recovering and recycling L-tartaric acid | |
| CN117447427A (en) | Preparation method of furosemide | |
| CN109180532B (en) | High-efficiency preparation method of D-dencichine | |
| CN111440171A (en) | Method for synthesizing guanine by hydrolysis of guanosine | |
| CN111718370A (en) | Preparation method of O, O' -dimethyl thiophosphoryl amide | |
| CN103896941A (en) | Synthesis method of 6-chloroimidazo[1,2-a]pyridine-3-formonitrile | |
| CN102531945A (en) | Preparation method of 3, 5-binitro-2-methyl benzamide | |
| CN105348254A (en) | Method for preparing 1,3-propane sultone | |
| CN112645813B (en) | Preparation method of (R) -3-cyclohexene carboxylic acid | |
| CN113307729A (en) | Preparation method of high-performance aluminum acetylacetonate | |
| CN110283067B (en) | Synthetic method of 2, 4-dihydroxy-3, 3-dimethylbutyric acid | |
| CN103664729B (en) | Method for preparing L-pyroglutamic acid | |
| CN113636941A (en) | Synthesis process of dimethyl diallyl ammonium chloride | |
| CN107556260B (en) | A kind of etoxazole preparation method | |
| CN103193609B (en) | Synthesizing process of (S)-2-benzyloxy-pentan-3-one | |
| CN102718739B (en) | Method for preparing (2S)-2-[[(9H-fluorene-9-yl methoxy) carbonyl] amino]-3-(2,2-dimethyl-1,3-benzo dioxol-5-yl)propionate | |
| CN107602487B (en) | 2,4,5- triamido -6- hydroxy pyrimidine formates, preparation method and application | |
| CN107089928A (en) | The synthetic method of N Boc L propargylglycines |
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 | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200717 Address after: 256500 Boxing Economic Development Zone, Binzhou, Shandong Applicant after: SHANDONG EFIRM BIOCHEMISTRY AND ENVIRONMENTAL PROTECTION Co.,Ltd. Address before: 256500 Boxing Economic Development Zone, Binzhou, Shandong Applicant before: YELLOW RIVER DELTA JINGBO RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180327 |
|
| RJ01 | Rejection of invention patent application after publication |