CN103012217A - Method for preparing high-purity aminoguanidine bicarbonate - Google Patents
Method for preparing high-purity aminoguanidine bicarbonate Download PDFInfo
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- CN103012217A CN103012217A CN2012105516455A CN201210551645A CN103012217A CN 103012217 A CN103012217 A CN 103012217A CN 2012105516455 A CN2012105516455 A CN 2012105516455A CN 201210551645 A CN201210551645 A CN 201210551645A CN 103012217 A CN103012217 A CN 103012217A
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Abstract
The invention relates to a method for preparing high-purity aminoguanidine bicarbonate. The technological process comprises the steps that hydrazine hydrate and water are mixed firstly; hydrogen cyanamide is added after the temperature rises to 66-80 DEG C; a mixed solution is heated continuously to 80 DEG C; then heating is stopped, so that the temperature of the solution drops naturally to 75-77 DEG C; heat preservation is conducted for 4 hours; then ammonium bicarbonate is added, carbon dioxide gas is introduced at the same time, and heat preservation is conducted for 4 hours; and suction filtration, separation, ethanol rinsing and drying are performed to obtain the high-purity aminoguanidine bicarbonate. According to the method, cyanamide, the hydrazine hydrate and the ammonium bicarbonate serve as raw materials to produce the aminoguanidine bicarbonate, and the carbon dioxide gas is introduced into the mother liquid for adjusting the pH value of the mother liquid during the process for producing the aminoguanidine bicarbonate simultaneously, so that the product purity is improved. The product purity of the aminoguanidine bicarbonate produced through the method ranges from 98.5% to 99%.
Description
Technical field
The present invention relates to chemical production technical field, particularly relate to the preparation method of the amino guanidine carbonate of a kind of high purity.
Background technology
The technique of existing domestic production aminoguanidine sulfate generally adopts synthetic take lime nitrogen, hydrazine hydrate, bicarbonate of ammonia or sodium bicarbonate as raw material, and the aminoguanidine sulfate content average out to 98% that this explained hereafter goes out can not satisfy high-end product client's requirement.
Summary of the invention
The object of the invention is to overcome the defective of above-mentioned prior art, the preparation method of the amino guanidine carbonate of a kind of high purity is provided.
The technical measures of taking for achieving the above object are:
The preparation method of the amino guanidine carbonate of a kind of high purity, it is characterized in that its technological process is: at first hydrazine hydrate and water are mixed, add cyanamide after being warming up to 66-68 ℃, the solution that mixes continues to heat to 80 ℃ again, and then stopped heating makes solution temperature naturally drop to 75-77 ℃, is incubated 4 hours, then add bicarbonate of ammonia, pass into simultaneously carbon dioxide, be incubated 4 hours, suction filtration, separation, ethanol clean, dry getting final product.
Above-mentioned CO
2Gas concentration is not less than 24%.
Above-mentioned various amount of substance is calculated according to stoichiometry.
The present invention adopts take cyanamide, hydrazine hydrate and bicarbonate of ammonia as the raw material production aminoguanidine sulfate, carries out the adjustment of mother liquor acid basicity in the middle of in its production process carbon dioxide being passed into mother liquor simultaneously, thereby improves product purity.The aminoguanidine sulfate product purity that adopts the method to produce is 98.5%-99%.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below by embodiment the present invention is described.It should be understood that embodiments of the invention are for explanation the present invention rather than limitation of the present invention.Scope of the present invention and core content are determined according to claims.
Specific embodiment is:
This production technique is batch feed intake (the finished product 3-3.5 ton of every batch of system of feeding intake), every batch of concrete technology that feeds intake is: add entry (8 tons) in the reactor and hydrazine hydrate (1.6 tons) is warming up to 66-68 ℃, add again cyanamide (3.8 tons), the solution that mixes continues to heat to 80 ℃ again, then stopped heating makes solution temperature drop to 75-77 ℃ again, be incubated 4 hours this moment, fully after the reaction this solution is put into to add bicarbonate of ammonia (2.6 tons) in another reactor again and pass into carbon dioxide (CO
2Gas concentration must be not less than 24%, the amount that passes into is at the 100-150 liter), (at this moment product has begun crystallization) this moment, this solution was incubated 4 hours again, after solution is put into the suction filtration bucket and carries out suction filtration after, material passes through solid-liquid separating equipment again---and whizzer carries out filtering separation, and it is the finished product that isolated white crystalline powder is carried out the ethanol cleaning-drying resulting again.The aminoguanidine sulfate product purity that adopts the method to produce is 98.5%--99%.
Claims (2)
1. the preparation method of the amino guanidine carbonate of a high purity, it is characterized in that its technological process is: at first hydrazine hydrate and water are mixed, add cyanamide after being warming up to 66-68 ℃, the solution that mixes continues to heat to 80 ℃ again, and then stopped heating makes solution temperature naturally drop to 75-77 ℃, is incubated 4 hours, then add bicarbonate of ammonia, pass into simultaneously carbon dioxide, be incubated 4 hours, suction filtration, separation, ethanol clean, dry getting final product.
2. according to the preparation method of the amino guanidine carbonate of high purity claimed in claim 1, it is characterized in that: above-mentioned CO
2Gas concentration is not less than 24%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012105516455A CN103012217A (en) | 2012-12-19 | 2012-12-19 | Method for preparing high-purity aminoguanidine bicarbonate |
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| CN2012105516455A CN103012217A (en) | 2012-12-19 | 2012-12-19 | Method for preparing high-purity aminoguanidine bicarbonate |
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| CN103012217A true CN103012217A (en) | 2013-04-03 |
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| CN2012105516455A Pending CN103012217A (en) | 2012-12-19 | 2012-12-19 | Method for preparing high-purity aminoguanidine bicarbonate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384661A (en) * | 2015-12-04 | 2016-03-09 | 湖北航天化学技术研究所 | Triaminoguanidine nitrate synthetic method applicable to industrial production |
| CN105481727A (en) * | 2015-12-04 | 2016-04-13 | 湖北航天化学技术研究所 | Synthesis method for industrialized production of triaminoguanidinium nitrate |
| CN110183358A (en) * | 2019-04-28 | 2019-08-30 | 西安航洁化工科技有限责任公司 | Hydrazine hydrochloride is as the purposes of production aminoguanidine carbonate and the combine production method of aminoguanidine carbonate and ammonium chloride |
| CN113214117A (en) * | 2020-12-01 | 2021-08-06 | 胡东林 | Industrial preparation method of aminoguanidine bicarbonate |
Citations (5)
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| SU981314A1 (en) * | 1981-03-17 | 1982-12-15 | Чебоксарское производственное объединение "Химпром" | Process for producing aminoguanidine carbonate |
| DD249009A1 (en) * | 1986-04-16 | 1987-08-26 | Piesteritz Agrochemie | METHOD FOR PRODUCING AMINOGUANIDINE HYDROGEN CARBONATE |
| NZ281400A (en) * | 1994-01-21 | 1998-10-28 | Picower Inst Med Res | Aromatic amidino-hydrazone derivatives and medicaments |
| CN1361764A (en) * | 1999-07-16 | 2002-07-31 | 阿托菲纳公司 | Aminoguanidine bicarbonate with particular properties and method for making same |
| CN102093365A (en) * | 2011-02-26 | 2011-06-15 | 西陇化工股份有限公司 | Method for producing 4-hydroxy-6-methyl-1,3,3a,7-tetraazaindene |
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2012
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| SU981314A1 (en) * | 1981-03-17 | 1982-12-15 | Чебоксарское производственное объединение "Химпром" | Process for producing aminoguanidine carbonate |
| DD249009A1 (en) * | 1986-04-16 | 1987-08-26 | Piesteritz Agrochemie | METHOD FOR PRODUCING AMINOGUANIDINE HYDROGEN CARBONATE |
| NZ281400A (en) * | 1994-01-21 | 1998-10-28 | Picower Inst Med Res | Aromatic amidino-hydrazone derivatives and medicaments |
| CN1361764A (en) * | 1999-07-16 | 2002-07-31 | 阿托菲纳公司 | Aminoguanidine bicarbonate with particular properties and method for making same |
| CN102093365A (en) * | 2011-02-26 | 2011-06-15 | 西陇化工股份有限公司 | Method for producing 4-hydroxy-6-methyl-1,3,3a,7-tetraazaindene |
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| 王彦林: "氨基胍碳酸氢盐的合成", 《河南化工》, no. 4, 31 December 1989 (1989-12-31) * |
| 章思规: "《精细有机化学品技术手册 上》", 31 December 1992, article "氨基胍碳酸氢盐" * |
| 蒋华江等: "氨基胍碳酸氢盐的合成方法改进", 《台州师专学报》, vol. 20, no. 6, 31 December 1998 (1998-12-31) * |
| 赵声贵等: "胍基化合物的制备方法及其应用", 《精细化工中间体》, vol. 36, no. 3, 30 June 2006 (2006-06-30) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384661A (en) * | 2015-12-04 | 2016-03-09 | 湖北航天化学技术研究所 | Triaminoguanidine nitrate synthetic method applicable to industrial production |
| CN105481727A (en) * | 2015-12-04 | 2016-04-13 | 湖北航天化学技术研究所 | Synthesis method for industrialized production of triaminoguanidinium nitrate |
| CN110183358A (en) * | 2019-04-28 | 2019-08-30 | 西安航洁化工科技有限责任公司 | Hydrazine hydrochloride is as the purposes of production aminoguanidine carbonate and the combine production method of aminoguanidine carbonate and ammonium chloride |
| CN113214117A (en) * | 2020-12-01 | 2021-08-06 | 胡东林 | Industrial preparation method of aminoguanidine bicarbonate |
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Application publication date: 20130403 |