CN102329261A - Production process of N-chlorosuccinimide - Google Patents
Production process of N-chlorosuccinimide Download PDFInfo
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- CN102329261A CN102329261A CN201110174757A CN201110174757A CN102329261A CN 102329261 A CN102329261 A CN 102329261A CN 201110174757 A CN201110174757 A CN 201110174757A CN 201110174757 A CN201110174757 A CN 201110174757A CN 102329261 A CN102329261 A CN 102329261A
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- Prior art keywords
- succimide
- weight ratio
- raw material
- chlorosuccinimide
- succinic acid
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Abstract
The invention discloses a production process of N-chlorosuccinimide, which is characterized by comprising the following steps: by using succinic acid as a main raw material, sequentially carrying out an amination reaction on the succinic acid and urea to obtain a succimide intermediate product, and carrying out a chlorination reaction on succimide and sodium hypochlorite to generate the N-chlorosuccinimide. By using the process provided by the invention, through effectively controlling a dripping temperature and heat-preserving time in a production process, the particle size of a product can be controlled reasonably, and the applicability of the product is improved. Being detected by a test, the yield of the process provided by the invention is above 85%; the content of the prepared product is more than 99.0%; and the distribution of the particle size is optimal.
Description
Technical field
The present invention relates to a kind of technology of the N-of preparation chlorosuccinimide.
Background technology
Prior art is when preparation N-chlorosuccinimide, because process step is unreasonable, the granularity of the product that causes being produced is difficult to control, has influenced the quality of product.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to prior art, and the production technique that a kind of process step is more reasonable, product granularity is prone to the N-chlorosuccinimide of control is provided.
Technical problem to be solved by this invention is to realize through following technical scheme.The present invention is a kind of production technique of N-chlorosuccinimide, is characterized in, its step is following:
(1) ammonification: Succinic Acid and urea are dropped into the ammonification still, begin when being warming up to 150 ℃ to stir, continue to be warming up to 240～250 ℃, insulation 5～10min, discharging is stirred crystallization and is got the succimide bullion to basin; The weight ratio of raw material Succinic Acid and urea is 1: 0.2～0.4;
(2) refining: in the decolouring still, add entry, succimide and gac are warming up to 55～65 ℃ of decolourings;
Decolouring finishes after-filtration, and filtrating is gone into the chlorination reaction still; The weight ratio of raw water, succimide and gac is 2.8～3.2: 1: 0.04～0.06;
(3) chlorination: when the chlorination reaction still is cooled to 20～25 ℃, add Glacial acetic acid min. 99.5, begin to drip the chlorine bleach liquor that mass concentration is 10-14% when continuing to be cooled to 0～5 ℃, the reaction finish after, centrifugal, the washing, dry finished product; The weight ratio of raw material Glacial acetic acid min. 99.5, Youxiaolin and succimide is 1.3～1.7: 5.5～6.5: 1.
In the production technique of above-described N-chlorosuccinimide: the weight ratio of raw material Succinic Acid and urea is preferably 1: 0.3 in the step (1); The weight ratio of raw water, succimide and gac is preferably 3: 1: 0.05 in the step (2); The weight ratio of raw material Glacial acetic acid min. 99.5, Youxiaolin and succimide is preferably 1.5: 6: 1 in the step (3).
The main chemical reactions equation that relates in the reaction process of the present invention is following:
1. aminating reaction:
2. chlorination reaction:
3. neutralization reaction (pair)
CH
3COOH+NaOH→CH
3COONa+H
2O
Decomposition reaction (pair)
2NaNO
2+(NH
2)
2CO→2NaOH+CO
2+2N
2+H
2O
Prior art is compared, and the advantage of the present invention's technology is: technology of the present invention can reasonably be controlled the granularity of product through dropping temperature in the production process and soaking time are controlled effectively, has improved the suitability of product.Detect through test, the yield of technology of the present invention is more than 85%, and the content of prepared product is greater than 99.0%, and size-grade distribution is good.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1, a kind of production technique of N-chlorosuccinimide, and its step is following:
(1) ammonification: Succinic Acid and urea are dropped into the ammonification still, begin when being warming up to 150 ℃ to stir, continue to be warming up to 240 ℃, insulation 5min, discharging is stirred crystallization and is got the succimide bullion to basin; The weight ratio of raw material Succinic Acid and urea is 1: 0.2;
(2) refining: in the decolouring still, add entry, succimide and gac are warming up to 55 ℃ of decolourings; Decolouring finishes after-filtration, and filtrating is gone into the chlorination reaction still; The weight ratio of raw water, succimide and gac is 2.8: 1: 0.04;
(3) chlorination: when the chlorination reaction still is cooled to 20 ℃, add Glacial acetic acid min. 99.5, begin to drip mass concentration when continuing to be cooled to 0 ℃ and be 10% chlorine bleach liquor, centrifugal after reaction finishes, washing, dry finished product; The weight ratio of raw material Glacial acetic acid min. 99.5, Youxiaolin and succimide is 1.3: 5.5: 1; Through detecting, the yield of present embodiment is 85%, and the content of prepared product is greater than 99.1%.
Embodiment 2, a kind of production technique of N-chlorosuccinimide, and its step is following:
(1) ammonification: Succinic Acid and urea are dropped into the ammonification still, begin when being warming up to 150 ℃ to stir, continue to be warming up to 250 ℃, insulation 10min, discharging is stirred crystallization and is got the succimide bullion to basin; The weight ratio of raw material Succinic Acid and urea is 1: 0.4;
(2) refining: in the decolouring still, add entry, succimide and gac are warming up to 65 ℃ of decolourings; Decolouring finishes after-filtration, and filtrating is gone into the chlorination reaction still; The weight ratio of raw water, succimide and gac is 3.2: 1: 0.06;
(3) chlorination: when the chlorination reaction still is cooled to 25 ℃, add Glacial acetic acid min. 99.5, begin to drip mass concentration when continuing to be cooled to 5 ℃ and be 14% chlorine bleach liquor, centrifugal after reaction finishes, washing, dry finished product; The weight ratio of raw material Glacial acetic acid min. 99.5, Youxiaolin and succimide is 1.7: 6.5: 1;
Through detecting, the yield of present embodiment is 85.8%, and the content of prepared product is greater than 99.25%.
Embodiment 3, a kind of production technique of N-chlorosuccinimide, and its step is following:
(1) ammonification: Succinic Acid and urea are dropped into the ammonification still, begin when being warming up to 150 ℃ to stir, continue to be warming up to 245 ℃, insulation 7min, discharging is stirred crystallization and is got the succimide bullion to basin; The weight ratio of raw material Succinic Acid and urea is 1: 0.3;
(2) refining: in the decolouring still, add entry, succimide and gac are warming up to 58 ℃ of decolourings; Decolouring finishes after-filtration, and filtrating is gone into the chlorination reaction still; The weight ratio of raw water, succimide and gac is 3.0: 1: 0.05;
(3) chlorination: when the chlorination reaction still is cooled to 22 ℃, add Glacial acetic acid min. 99.5, begin to drip mass concentration when continuing to be cooled to 2 ℃ and be 12% chlorine bleach liquor, centrifugal after reaction finishes, washing, dry finished product; The weight ratio of raw material Glacial acetic acid min. 99.5, Youxiaolin and succimide is 1.5: 6: 1;
Through detecting, the yield of present embodiment is 86%, and the content of prepared product is greater than 99.4%.
Claims (2)
1. the production technique of a N – chlorosuccinimide is characterized in that, its step is following:
(1) ammonification: Succinic Acid and urea are dropped into the ammonification still, begin when being warming up to 150 ℃ to stir, continue to be warming up to 240 ~ 250 ℃, insulation 5 ~ 10min, discharging is stirred crystallization and is got the succimide bullion to basin; The weight ratio of raw material Succinic Acid and urea is 1: 0.2 ~ 0.4;
(2) refining: in the decolouring still, add entry, succimide and gac are warming up to 55 ~ 65 ℃ of decolourings; Decolouring finishes after-filtration, and filtrating is gone into the chlorination reaction still; The weight ratio of raw water, succimide and gac is 2.8 ~ 3.2: 1: 0.04 ~ 0.06;
(3) chlorination: when the chlorination reaction still is cooled to 20～25 ℃, add Glacial acetic acid min. 99.5, begin to drip the chlorine bleach liquor that mass concentration is 10-14% when continuing to be cooled to 0 ~ 5 ℃, the reaction finish after, centrifugal, the washing, dry finished product; The weight ratio of raw material Glacial acetic acid min. 99.5, Youxiaolin and succimide is 1.3 ~ 1.7: 5.5 ~ 6.5: 1.
2. the production technique of N – chlorosuccinimide according to claim 1 is characterized in that: the weight ratio of middle raw material Succinic Acid of step (1) and urea 1: 0.3; The weight ratio of raw water, succimide and gac is 3: 1: 0.05 in the step (2); The weight ratio of raw material Glacial acetic acid min. 99.5, Youxiaolin and succimide is 1.5: 6: 1 in the step (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110174757A CN102329261A (en) | 2011-06-24 | 2011-06-24 | Production process of N-chlorosuccinimide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110174757A CN102329261A (en) | 2011-06-24 | 2011-06-24 | Production process of N-chlorosuccinimide |
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| CN102329261A true CN102329261A (en) | 2012-01-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732457A (en) * | 2016-04-01 | 2016-07-06 | 江西科技师范大学 | Method for preparing succinimide with succinic acid fermentation liquor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1317890A1 (en) * | 1985-03-20 | 1995-05-10 | Армянский филиал Всесоюзного научно-исследовательского института химических реактивов и особо чистых веществ | Method of succinimide synthesis |
| CN101712644A (en) * | 2008-10-06 | 2010-05-26 | 天津市化学试剂研究所 | Method for preparing N-chlorosuccinimide |
-
2011
- 2011-06-24 CN CN201110174757A patent/CN102329261A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1317890A1 (en) * | 1985-03-20 | 1995-05-10 | Армянский филиал Всесоюзного научно-исследовательского института химических реактивов и особо чистых веществ | Method of succinimide synthesis |
| CN101712644A (en) * | 2008-10-06 | 2010-05-26 | 天津市化学试剂研究所 | Method for preparing N-chlorosuccinimide |
Non-Patent Citations (1)
| Title |
|---|
| 徐博刚等: "N-氯代丁二酰亚胺的合成工艺研究", 《天津化工》, vol. 20, no. 2, 31 March 2006 (2006-03-31), pages 56 - 57 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732457A (en) * | 2016-04-01 | 2016-07-06 | 江西科技师范大学 | Method for preparing succinimide with succinic acid fermentation liquor |
| CN105732457B (en) * | 2016-04-01 | 2018-09-11 | 江西科技师范大学 | A method of preparing succimide using succinic acid fermentation liquor |
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Application publication date: 20120125 |