CN102924337A - Production process of guanidine nitrate - Google Patents
Production process of guanidine nitrate Download PDFInfo
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- CN102924337A CN102924337A CN201210431159XA CN201210431159A CN102924337A CN 102924337 A CN102924337 A CN 102924337A CN 201210431159X A CN201210431159X A CN 201210431159XA CN 201210431159 A CN201210431159 A CN 201210431159A CN 102924337 A CN102924337 A CN 102924337A
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Abstract
The invention discloses a production process of guanidine nitrate. Ammonium nitrate and dicyandiamide serving as raw materials are reacted to make guanidine nitrate. The production process is characterized in that a batch feeding mode is adopted, ammonium nitrate and dicyandiamide are mixed and then added into a reaction kettle in batches, the feeding times is 5-10, and the feeding reaction temperature is controlled to be 130-140 DEG C; when feeding of one batch of raw materials is finished and a reaction mixture is in a molten state and the reaction temperature is 130-140 DEG C, a next batch of raw materials are added until feeding of the reaction raw materials is finished; after feeding is finished, thermal insulation reactions are continued to be performed for 30-60min at 145-155 DEG C until an addition reaction is over, then the temperature is continued to be warmed to 210-220 DEG C within 20-30min, and guanidine nitrate products are obtained when a cracking reaction is over after reaction for 30min. The production process has the advantages that by batch feeding and by controlling corresponding feeding temperature and feeding amount well, the aim of improving the yield coefficient of guanidine nitrate is achieved, the content of the produced guanidine nitrate is larger than 92%, and the mol yield coefficient is larger than 96%.
Description
Technical field
The present invention relates to a kind of production technique of Guanidinium nitrate.
Background technology
Guanidinium nitrate is white crystalline powder or particle, and is soluble in water and pure, and eyes, skin, mucous membrane and the upper respiratory tract are had hormesis.Guanidinium nitrate is not only the raw material of pesticide imidacloprid at agricultural chemicals, for the synthesis of next step intermediate nitroguanidine, also can be used as the intermediate of multiple sulfonylurea herbicide,, chlorimuronethyl grand such as benbbensulfuronmethyl, pyridine sulphur etc.In addition, it is also for the synthesis of sulfa drugs and as the raw material of making explosive, photographic material, sterilizing agent.
At present, the Guanidinium nitrate synthetic method of report is mainly made by the reaction of ammonium nitrate and Dyhard RU 100, and content and the yield of its product are lower, content approximately 88%, and yield is 87%.
Summary of the invention
The production technique that the purpose of this invention is to provide a kind of Guanidinium nitrate.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of production technique of Guanidinium nitrate, as reacting, raw material makes Guanidinium nitrate take ammonium nitrate and Dyhard RU 100, it is characterized in that: the mode that adopts batch charging, to add in batches reactor after ammonium nitrate and the mixing of Dyhard RU 100 two raw materials, charging times is 5-10 time, control charging reaction temperature is at 130-140 ℃, treat that a raw material adds, reaction mixture is in molten state and temperature of reaction in the time of 130-140 ℃, then adds lower a raw material, until reaction raw materials finishes, continue at 145-155 ℃ of insulation reaction 30-60 minute after finishing material, reaction finishes, and is last, in 20-30 minute, be warming up to 210-220 ℃, reacted 30 minutes, scission reaction finishes, and obtains the Guanidinium nitrate product.
Preferably, the mol ratio of described Dyhard RU 100 and ammonium nitrate is 1:2.1-2.2.
The invention has the advantages that: the present invention is by batch charging, and controls corresponding charge temperature and feeding quantity well and reach the purpose that improves the Guanidinium nitrate yield, and the Guanidinium nitrate content of producing is greater than 92%, and molar yield is greater than 96%.
Embodiment
In order to make the public can fully understand technical spirit of the present invention and beneficial effect; the applicant will describe in detail the specific embodiment of the present invention below; but the applicant is not restriction to technical scheme to the description of embodiment, anyly makes form and immaterial variation all should be considered as protection scope of the present invention according to the present invention's design.
Embodiment 1
With 1050Kg (13.125Kmol) ammonium nitrate and 525Kg(6.25Kmol) Dyhard RU 100 is divided into 7 five equilibriums, then to stirring, in 2000 liters of enamel reaction stills of thermometer, add first part of Dyhard RU 100, ammonium nitrate, temperature of reaction is controlled between 130-140 ℃ when reinforced, treat that a raw material adds, reaction mixture is in molten state and temperature of reaction in the time of 130-140 ℃, then add lower a raw material, add with raw material to reacting, approximately need 80-90 minute, then temperature of reaction was brought up between 145-155 ℃ insulation reaction 60 minutes, the last temperature of reaction that further improves is reacted after 30 minutes to 210-220 ℃, reaction finishes, through cooling, obtain the Guanidinium nitrate product after the section: 1563 Kg, content: 94.5 %, molar yield: 96.85%.
Embodiment 2
Process is with embodiment 1, and difference is that raw material consists of 1100Kg (13.75Kmol) ammonium nitrate and 525Kg(6.25Kmol), obtain the Guanidinium nitrate product after the reaction: 1610 Kg, content: 92.3 %, molar yield: 97.44%.
Claims (2)
1. the production technique of a Guanidinium nitrate, as reacting, raw material makes Guanidinium nitrate take ammonium nitrate and Dyhard RU 100, it is characterized in that: the mode that adopts batch charging, to add in batches reactor after ammonium nitrate and the mixing of Dyhard RU 100 two raw materials, charging times is 5-10 time, control charging reaction temperature is at 130-140 ℃, treat that a raw material adds, reaction mixture is in molten state and temperature of reaction in the time of 130-140 ℃, then add lower a raw material, until reaction raw materials finishes, finish and expect rear the continuation at 145-155 ℃ of insulation reaction 30-60 minute, reaction finishes, at last, in 20-30 minute, be warming up to 210-220 ℃, reacted 30 minutes, scission reaction finishes, and obtains the Guanidinium nitrate product.
2. the production technique of a kind of Guanidinium nitrate according to claim 1, it is characterized in that: the mol ratio of described Dyhard RU 100 and ammonium nitrate is 1:2.1-2.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210431159XA CN102924337A (en) | 2012-11-02 | 2012-11-02 | Production process of guanidine nitrate |
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| CN201210431159XA CN102924337A (en) | 2012-11-02 | 2012-11-02 | Production process of guanidine nitrate |
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| CN102924337A true CN102924337A (en) | 2013-02-13 |
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| CN201210431159XA Pending CN102924337A (en) | 2012-11-02 | 2012-11-02 | Production process of guanidine nitrate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112742308A (en) * | 2020-12-30 | 2021-05-04 | 宁夏嘉峰化工有限公司 | Full-automatic cross proportioning feeding method and system for guanidine nitrate production |
| CN112939816A (en) * | 2021-01-11 | 2021-06-11 | 宁夏贝利特生物科技有限公司 | Production method for refining guanidine nitrate by one-step method |
| CN113292459A (en) * | 2021-06-17 | 2021-08-24 | 湖南吴赣药业有限公司 | Continuous nitration method of guanidine nitrate |
| CN114105826A (en) * | 2021-09-28 | 2022-03-01 | 宁夏贝利特生物科技有限公司 | Method for directly producing guanidine nitrate by using liquid ammonia and dilute nitric acid |
| CN114163357A (en) * | 2021-09-28 | 2022-03-11 | 宁夏贝利特生物科技有限公司 | Production process for continuously producing guanidine nitrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2109934A (en) * | 1935-04-05 | 1938-03-01 | Hercules Powder Co Ltd | Method of producing guanidine nitrate |
| JPS5439020A (en) * | 1977-08-30 | 1979-03-24 | Kashiwa Kagaku Kogyo Kk | Process for preparing quanidine salts |
| US4535185A (en) * | 1982-09-30 | 1985-08-13 | Industrie Chemie Thoma Gmbh & Co Produktions Kg | Process for the production of guanidine nitrate from a mixture of urea and ammonium nitrate |
| CN102304065A (en) * | 2011-04-29 | 2012-01-04 | 苏州市吴赣药业有限公司 | Process for producing guanidine nitrate |
-
2012
- 2012-11-02 CN CN201210431159XA patent/CN102924337A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2109934A (en) * | 1935-04-05 | 1938-03-01 | Hercules Powder Co Ltd | Method of producing guanidine nitrate |
| JPS5439020A (en) * | 1977-08-30 | 1979-03-24 | Kashiwa Kagaku Kogyo Kk | Process for preparing quanidine salts |
| US4535185A (en) * | 1982-09-30 | 1985-08-13 | Industrie Chemie Thoma Gmbh & Co Produktions Kg | Process for the production of guanidine nitrate from a mixture of urea and ammonium nitrate |
| CN102304065A (en) * | 2011-04-29 | 2012-01-04 | 苏州市吴赣药业有限公司 | Process for producing guanidine nitrate |
Non-Patent Citations (2)
| Title |
|---|
| 《火炸药》 19860331 秦元生 "关于硝酸胍生产的工艺路线选择" 第46页, 第2、4段 1-2 , * |
| 秦元生: ""关于硝酸胍生产的工艺路线选择"", 《火炸药》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112742308A (en) * | 2020-12-30 | 2021-05-04 | 宁夏嘉峰化工有限公司 | Full-automatic cross proportioning feeding method and system for guanidine nitrate production |
| CN112939816A (en) * | 2021-01-11 | 2021-06-11 | 宁夏贝利特生物科技有限公司 | Production method for refining guanidine nitrate by one-step method |
| CN113292459A (en) * | 2021-06-17 | 2021-08-24 | 湖南吴赣药业有限公司 | Continuous nitration method of guanidine nitrate |
| CN114105826A (en) * | 2021-09-28 | 2022-03-01 | 宁夏贝利特生物科技有限公司 | Method for directly producing guanidine nitrate by using liquid ammonia and dilute nitric acid |
| CN114163357A (en) * | 2021-09-28 | 2022-03-11 | 宁夏贝利特生物科技有限公司 | Production process for continuously producing guanidine nitrate |
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Application publication date: 20130213 |