CN102304065A - Process for producing guanidine nitrate - Google Patents
Process for producing guanidine nitrate Download PDFInfo
- Publication number
- CN102304065A CN102304065A CN201110110268A CN201110110268A CN102304065A CN 102304065 A CN102304065 A CN 102304065A CN 201110110268 A CN201110110268 A CN 201110110268A CN 201110110268 A CN201110110268 A CN 201110110268A CN 102304065 A CN102304065 A CN 102304065A
- Authority
- CN
- China
- Prior art keywords
- reaction
- nitrate
- guanidine nitrate
- product
- dicyandiamide
- 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
- 238000000034 method Methods 0.000 title claims abstract description 16
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 title abstract 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 25
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- MJFQUUWPZOGYQT-UHFFFAOYSA-O diaminomethylideneazanium;nitrate Chemical compound NC(N)=[NH2+].[O-][N+]([O-])=O MJFQUUWPZOGYQT-UHFFFAOYSA-O 0.000 claims description 18
- 229910021529 ammonia Inorganic materials 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 238000007086 side reaction Methods 0.000 abstract description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 abstract 4
- 239000003223 protective agent Substances 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007810 chemical reaction solvent Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a process for producing guanidine nitrate, which comprises the following steps: reacting ammonium nitrate and dicyandiamide, which serve as raw materials, obtaining a guanidine nitrate product after reaction, cooling the guanidine nitrate product to obtain solid guanidine nitrate, crushing and grinding to obtain a finished product. The process is characterized in that continuous circulating ammonia gas is added into the reaction solution as an assistant in a reaction process. In the processing procedure of each produced guanidine nitrate, the ratio of ammonia gas to ammonium nitrate to dicyandiamide in reaction is (5-10)kg:1,000kg:500kg. The ammonia gas serves as an alkaline protective agent in the reaction solution to improve the quality of the coarse guanidine nitrate formed by an initial reaction and improve the stability of the product. The decomposition of dicyandiamide and other side reaction caused by the decomposition of dicyandiamide in an improper environment are prevented. The reaction speed and efficiency are increased.
Description
Technical field
The present invention relates to a kind of Guanidinium nitrate production technique that adds catalyst aid.
Background technology
In the production technique of existing disclosed Guanidinium nitrate; What mainly adopt is that raw material is ammonium nitrate and Dyhard RU 100; Wherein, Raw material ammonium nitrate reacts in strict accordance with carry out proportioning than the mass ratio of classifying 2:1 as with the mass ratio of Dyhard RU 100; In reaction process; Add proper amount of sodium hydroxide as reaction solvent, the alkaline ph value that guarantees solution and also will be controlled at temperature in certain scope in the reaction process about 9.5.Adopt original reaction process, need strict control reaction process, when entire reaction process when too fierceness or temperature are too high, Dyhard RU 100 can decompose, and causes other side reaction.
Summary of the invention
Technical problem to be solved by this invention provides a kind of Guanidinium nitrate production technique that makes its sufficient reacting, improves product stability.
The present invention solves the technical scheme that its technical problem takes: a kind of Guanidinium nitrate production technique; Its processing step is: with ammonium nitrate and Dyhard RU 100 is raw material; React; Obtain the Guanidinium nitrate product after the reaction, it is carried out cooling process, obtain the Guanidinium nitrate solids; After the processing of crushing; Obtain finished product after the grinding, in reaction process, add continuous round-robin ammonia as auxiliary agent to reaction soln.
In the reaction solvent of concrete every part of Guanidinium nitrate, said ammonia auxiliary agent in participating in reaction with the mass distribution of ammonium nitrate and Dyhard RU 100 is: ammonium nitrate 1000Kg, Dyhard RU 100 500Kg, ammonia 5～10Kg.
The invention has the beneficial effects as follows: the reaction promoter ammonia is in reaction process; The mode that adopts circulation to inject; Guarantee that reaction soln is the requirement of alkalescence; And; The volatilization of gas also can be taken away a large amount of heats that a certain amount of reaction produces; Make reaction be unlikely to too fierce, improve the thick Guanidinium nitrate quality that initial reaction generates, and improved the stability of product.Prevent under the unsuitable environment other side reactions that the decomposition of Dyhard RU 100 causes with it.Also accelerate speed of response, improved efficient.
Description of drawings:
Fig. 1 is a production technique synoptic diagram of the present invention.
Embodiment
A kind of Guanidinium nitrate production technique shown in Figure 1; Its processing step is: with ammonium nitrate and Dyhard RU 100 is raw material; React; Obtain the Guanidinium nitrate product after the reaction, it is carried out cooling process, obtain the Guanidinium nitrate solids; After the processing of crushing; Obtain finished product after the grinding, in reaction process, add continuous round-robin ammonia as auxiliary agent to reaction soln.
In the reaction solvent of concrete every part of Guanidinium nitrate, said ammonia auxiliary agent in participating in reaction with the mass distribution of ammonium nitrate and Dyhard RU 100 is: ammonium nitrate 1000Kg, Dyhard RU 100 500Kg, ammonia 5～10Kg.
Reaction promoter ammonia of the present invention is in reaction process; The mode that adopts circulation to inject; Guarantee that reaction soln is the requirement of alkalescence; And; The volatilization of gas also can be taken away a large amount of heats that a certain amount of reaction produces, and makes reaction be unlikely to too fierce, improves the thick Guanidinium nitrate quality that initial reaction generates; Improve quality product and reached more than 3.0%, and improved the stability of product.Prevent under the unsuitable environment other side reactions that the decomposition of Dyhard RU 100 causes with it.Also accelerate speed of response, improved efficient.
Claims (2)
1. Guanidinium nitrate production technique; Its processing step is: with ammonium nitrate and Dyhard RU 100 is raw material; React; Obtain the Guanidinium nitrate product after the reaction, it is carried out cooling process, obtain the Guanidinium nitrate solids; After the processing of crushing; Obtain finished product after the grinding, it is characterized in that: in reaction process, add continuous round-robin ammonia as auxiliary agent to reaction soln.
2. Guanidinium nitrate production technique according to claim 1 is characterized in that: said ammonia auxiliary agent in participating in reaction with the mass distribution of ammonium nitrate and Dyhard RU 100 is: ammonium nitrate 1000Kg, Dyhard RU 100 500Kg, ammonia 5～10Kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110110268A CN102304065A (en) | 2011-04-29 | 2011-04-29 | Process for producing guanidine nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110110268A CN102304065A (en) | 2011-04-29 | 2011-04-29 | Process for producing guanidine nitrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102304065A true CN102304065A (en) | 2012-01-04 |
Family
ID=45378006
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110110268A Pending CN102304065A (en) | 2011-04-29 | 2011-04-29 | Process for producing guanidine nitrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102304065A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924337A (en) * | 2012-11-02 | 2013-02-13 | 南通天泽化工有限公司 | Production process of guanidine nitrate |
| CN103450048A (en) * | 2013-08-06 | 2013-12-18 | 南通天泽化工有限公司 | Continuous synthesis process of guanidine nitrate |
| CN103951592A (en) * | 2014-05-19 | 2014-07-30 | 宁夏贝利特化工有限公司 | Production technique of guanidine nitrate |
| CN103951591A (en) * | 2014-05-19 | 2014-07-30 | 宁夏贝利特化工有限公司 | Production technique of guanidine hydrochloride |
| CN104235608A (en) * | 2014-09-25 | 2014-12-24 | 南通天泽化工有限公司 | Liquid ammonia afterheat gasification device for guanidine nitrate ammonia feeding reaction |
| CN106167469A (en) * | 2016-07-15 | 2016-11-30 | 南通天泽化工有限公司 | A kind of method of synthesis 2 amino 4,6 dihydroxy-pyrimidines |
| CN112851554A (en) * | 2019-11-28 | 2021-05-28 | 昆山昆化有限公司 | Preparation method of guanidine nitrate |
| CN113292459A (en) * | 2021-06-17 | 2021-08-24 | 湖南吴赣药业有限公司 | Continuous nitration method of guanidine nitrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB634725A (en) * | 1947-03-05 | 1950-03-29 | American Cyanamid Co | Improvements in or relating to the preparation of guanidine salts |
| GB639940A (en) * | 1946-01-18 | 1950-07-12 | Koppers Co Inc | Improvements in or relating to the production of guanidine nitrate |
| JPS5439020A (en) * | 1977-08-30 | 1979-03-24 | Kashiwa Kagaku Kogyo Kk | Process for preparing quanidine salts |
| JPS57167956A (en) * | 1981-04-09 | 1982-10-16 | Chisso Corp | Continuous preparation of guanidine sulfamate |
-
2011
- 2011-04-29 CN CN201110110268A patent/CN102304065A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB639940A (en) * | 1946-01-18 | 1950-07-12 | Koppers Co Inc | Improvements in or relating to the production of guanidine nitrate |
| GB634725A (en) * | 1947-03-05 | 1950-03-29 | American Cyanamid Co | Improvements in or relating to the preparation of guanidine salts |
| JPS5439020A (en) * | 1977-08-30 | 1979-03-24 | Kashiwa Kagaku Kogyo Kk | Process for preparing quanidine salts |
| JPS57167956A (en) * | 1981-04-09 | 1982-10-16 | Chisso Corp | Continuous preparation of guanidine sulfamate |
Non-Patent Citations (1)
| Title |
|---|
| 韩长日，宋小平: "精细有机中间体制造技术", 《精细有机中间体制造技术》, 29 February 2004 (2004-02-29), pages 522 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924337A (en) * | 2012-11-02 | 2013-02-13 | 南通天泽化工有限公司 | Production process of guanidine nitrate |
| CN103450048A (en) * | 2013-08-06 | 2013-12-18 | 南通天泽化工有限公司 | Continuous synthesis process of guanidine nitrate |
| CN103450048B (en) * | 2013-08-06 | 2015-09-23 | 南通天泽化工有限公司 | A kind of serialization synthesis technique of Guanidinium nitrate |
| CN103951592A (en) * | 2014-05-19 | 2014-07-30 | 宁夏贝利特化工有限公司 | Production technique of guanidine nitrate |
| CN103951591A (en) * | 2014-05-19 | 2014-07-30 | 宁夏贝利特化工有限公司 | Production technique of guanidine hydrochloride |
| CN103951592B (en) * | 2014-05-19 | 2016-05-25 | 宁夏贝利特化工有限公司 | A kind of process for producing guanidine nitrate |
| CN103951591B (en) * | 2014-05-19 | 2016-05-25 | 宁夏贝利特化工有限公司 | A kind of guanidine hydrochloride production technology |
| CN104235608A (en) * | 2014-09-25 | 2014-12-24 | 南通天泽化工有限公司 | Liquid ammonia afterheat gasification device for guanidine nitrate ammonia feeding reaction |
| CN104235608B (en) * | 2014-09-25 | 2018-01-05 | 南通天泽化工有限公司 | Guanidine nitrate, which leads to ammonia reaction liquefied ammonia waste hot air makeup, to be put |
| CN106167469A (en) * | 2016-07-15 | 2016-11-30 | 南通天泽化工有限公司 | A kind of method of synthesis 2 amino 4,6 dihydroxy-pyrimidines |
| CN112851554A (en) * | 2019-11-28 | 2021-05-28 | 昆山昆化有限公司 | Preparation method of guanidine nitrate |
| CN113292459A (en) * | 2021-06-17 | 2021-08-24 | 湖南吴赣药业有限公司 | Continuous nitration method of guanidine nitrate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102304065A (en) | Process for producing guanidine nitrate | |
| RU2604064C2 (en) | Clean method of preparing d, l-methionine | |
| SG175132A1 (en) | Process for beta-lactone production | |
| CN101318855B (en) | High-efficiency high-concentration sulphur based complex fertilizer | |
| BRPI0607836A2 (en) | ferronìquel production | |
| CN104529562A (en) | Method used for preparing potash magnesium sulphate fertilizer and potassium chloride fertilizer from carnallite | |
| CN104529794B (en) | The preparation method of Boscalid intermediate 2-(4-chlorphenyl) aniline | |
| CN105289624B (en) | A kind of low-pressure synthetic ammonia catalyst and preparation method thereof | |
| CN102658148A (en) | Fischer-Tropsch synthesis iron-based catalyst and preparation method thereof | |
| CN104480326A (en) | Method for producing nickel by using nickel hydroxide being intermediate product of nickel laterite ore | |
| CN111268657B (en) | A kind of method and system for continuous production of nitrosyl sulfuric acid | |
| CN103450048A (en) | Continuous synthesis process of guanidine nitrate | |
| CN104557553A (en) | Novel process for producing dimethyl carbonate and synthesis ammonia | |
| BRPI1010000A2 (en) | process for preparing a porous metal-organic structure based on magnesium formate | |
| CN105218431A (en) | A kind of synthetic method of 2-picoline | |
| CN100357268C (en) | Process for synthesizing sec-butyl urea | |
| CN104557721A (en) | Method for producing 5,5-dimethylhydantoin | |
| KR101249734B1 (en) | Mineral carbonation method using carbonic anhydrase | |
| CN109627183B (en) | Preparation method of chloroacetaldehyde oxime | |
| EP2688842B1 (en) | Process for production of nickel carbonate" | |
| CN102295585A (en) | Preparation method of 2-naphthylamine 6,8 disulfonic acid | |
| CN102059117B (en) | Two types of catalysts for synthesizing methyl chlorosilane and preparation method thereof | |
| CN104817462A (en) | Producing method of triisopropanolamine | |
| CN105859592B (en) | A kind of method that by-product hydrochloric acid recycles in ADC foaming agents producing process | |
| CN104370830A (en) | Synthetic method of 5-trifluoromethyl uracil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120104 |
|
| RJ01 | Rejection of invention patent application after publication |