CN102304065A - Process for producing guanidine nitrate - Google Patents

Process for producing guanidine nitrate Download PDF

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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
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CN
China
Prior art keywords
reaction
nitrate
guanidine nitrate
product
dicyandiamide
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Pending
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CN201110110268A
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Chinese (zh)
Inventor
施方浩
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SUZHOU WUGAN PHARMACEUTICAL CO Ltd
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SUZHOU WUGAN PHARMACEUTICAL CO Ltd
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Priority to CN201110110268A priority Critical patent/CN102304065A/en
Publication of CN102304065A publication Critical patent/CN102304065A/en
Pending legal-status Critical Current

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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

A kind of Guanidinium nitrate production technique
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.
CN201110110268A 2011-04-29 2011-04-29 Process for producing guanidine nitrate Pending CN102304065A (en)

Priority Applications (1)

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CN201110110268A CN102304065A (en) 2011-04-29 2011-04-29 Process for producing guanidine nitrate

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Application Number Priority Date Filing Date Title
CN201110110268A CN102304065A (en) 2011-04-29 2011-04-29 Process for producing guanidine nitrate

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Cited By (8)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

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