CN101712644A - Method for preparing N-chlorosuccinimide - Google Patents
Method for preparing N-chlorosuccinimide Download PDFInfo
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- CN101712644A CN101712644A CN 200810151988 CN200810151988A CN101712644A CN 101712644 A CN101712644 A CN 101712644A CN 200810151988 CN200810151988 CN 200810151988 CN 200810151988 A CN200810151988 A CN 200810151988A CN 101712644 A CN101712644 A CN 101712644A
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- chlorosuccinimide
- glacial acetic
- acetic acid
- preparation
- succimide
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Abstract
The invention relates to a method for preparing N-chlorosuccinimide, which comprises the following steps of: (1) placing succinic acid and ammonia water into a reactor to be stirred till fully reacting; (2) placing the reaction liquid of the succinic acid and the ammonia water into a distillation kettle and dehydrating to obtain a succinimide solid; (3) adding the succinimide solid into a glacial acetic acid aqueous solution to be stirred till fully dissolving; (4) cooling a mixed solution of succinimide and glacial acetic acid below 0 DEG C, maintaining the temperature, adding a sodium hypochlorite solution and stirring for 0.5-1.5 hours to obtain a mixed solution; (5) filtering the mixed solution and washing till neutrality to obtain white solid powder, namely a N-chlorosuccinimide finished product. The invention has high reaction yield, is suitable for industrial production, achieves the market requirement, terminates the state that the north in China does not produce the product, and improves the market competitive capacity of enterprises so that the product can be more greatly popularized and applied in the market.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of preparation method of N-chlorosuccinimide.
Background technology
The N-chlorosuccinimide has another name called the succinyl chlorimide, is a kind of medicine intermediate, can be used for the production of antibiotic, can also be used to differentiate reagent and the chlorizating agent and the sterilant of the brothers tertiary alcohol.At present, the synthetic method of N-chlorosuccinimide is reported in documents more both domestic and external.These synthetic methods are roughly the same, but the product yield that adopts this method to synthesize is not high, is unsuitable for suitability for industrialized production, can not reach market demands.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of new N-chlorosuccinimide is provided.Adopt the reaction yield height of the prepared N-chlorosuccinimide of this preparation method, be more suitable in industrial requirement.
The present invention solves its technical problem and is achieved through the following technical solutions:
A kind of preparation method of N-chlorosuccinimide is characterized in that: preparation process is:
(1). place reactor to be stirred to abundant reaction Succinic Acid and ammoniacal liquor, keeping temperature of reaction is 20～25 ℃;
(2). the reaction solution of Succinic Acid and ammoniacal liquor is placed still kettle, and dehydration obtains the succimide solid in the time of 275～290 ℃;
(3). will be stirred to dissolving fully in the succimide solid adding glacial acetic acid aqueous solution;
(4). the mixing solutions of succimide and Glacial acetic acid is cooled to below 0 ℃, keeps this temperature and add the chlorine bleach liquor, stirred 0.5～1.5 hour, obtain mixing solutions;
(5). with the mixing solutions suction filtration, be washed till neutrality, obtain the white solid powder, be N-chlorosuccinimide finished product.
And the ratio of weight and number of described Succinic Acid and ammoniacal liquor is 1: 1.4～1.8.
And the concentration of described Glacial acetic acid is 15～20%.
And the clorox ratio of weight and number among described succimide and the chlorine bleach liquor is 1: 3～3.5.
And described reactor is for having heating unit, and electricity stirs, thermometer, the reactor of dropping funnel.
Advantage of the present invention and beneficial effect are:
The present invention is by research that the synthesis technique of existing N-chlorosuccinimide is compared, determined the optimum concn of Glacial acetic acid, so reaction yield is improved, make it more appropriate to industrial requirement, thereby reach market demands, and finish northern China and do not have the state that this product is produced.In addition, improved the market competitiveness of enterprise, made this product can on market, obtain bigger applying.
Embodiment
The invention will be further described below by specific embodiment.Following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
A kind of preparation method of N-chlorosuccinimide is characterized in that its preparation process is:
Embodiment 1:
(1). in 200 liters of reactors, add ammoniacal liquor 70kg, under the state of cooling, keep temperature of reaction at 20～25 ℃.The 50kg Succinic Acid stirred add down among the ammoniacal liquor in batches.Described reactor is for having heating unit, and electricity stirs, thermometer, the reactor of dropping funnel.
(2). after adding, Succinic Acid continued stirring reaction 40 minutes.Then reaction solution is changed in the still kettle, the cut between collecting 275～290 ℃ obtains the succimide of 15kg, and dry back is stand-by.
(3). thermometer is being housed, is adding 85kg water and 15kg Glacial acetic acid in the reactor of whipping appts and dropping funnel, be stirred into 15% glacial acetic acid solution.Stir down 15kg succimide solid is added in the glacial acetic acid aqueous solution, to its whole dissolvings.
(4). be reduced to below 0 ℃ with icy salt solution cooling system to temperature, low temperature adds the solution that contains the 45kg clorox in the mixing solutions of succimide and Glacial acetic acid.The control rate of addition no longer raises system temperature.After adding the solution of clorox, stirred 0.5 hour, obtain mixing solutions.
(5). separate finished product
Mixing solutions is filtered, be washed till neutrality, obtain the white solid powder, be N-chlorosuccinimide finished product.
Embodiment 2:
(1). in 200 liters of reactors, add ammoniacal liquor 80kg, under the state of cooling, keep temperature of reaction at 20～25 ℃.The 50kg Succinic Acid stirred add down among the ammoniacal liquor in batches.Described reactor is for having heating unit, and electricity stirs, thermometer, the reactor of dropping funnel.
(2). after adding, Succinic Acid continued stirring reaction 40 minutes.Then reaction solution is changed in the still kettle, the cut between collecting 275～290 ℃ obtains the succimide of 15kg, and dry back is stand-by.
(3). thermometer is being housed, is adding 83kg water and 17kg Glacial acetic acid in the reactor of whipping appts and dropping funnel, be stirred into 17% glacial acetic acid solution.Stir down 15kg succimide solid is added in the glacial acetic acid aqueous solution, to its whole dissolvings.
(4). be reduced to below 0 ℃ with icy salt solution cooling system to temperature, low temperature adds the solution that contains the 50kg clorox in the mixing solutions of succimide and Glacial acetic acid.The control rate of addition no longer raises system temperature.After adding the solution of clorox, stirred 1 hour, obtain mixing solutions.
(5). separate finished product
Mixing solutions is filtered, be washed till neutrality, obtain the white solid powder, be N-chlorosuccinimide finished product.
Embodiment 3:
(1). in 200 liters of reactors, add ammoniacal liquor 90kg, under the state of cooling, keep temperature of reaction at 20～25 ℃.The 50kg Succinic Acid stirred add down among the ammoniacal liquor in batches.Described reactor is for having heating unit, and electricity stirs, thermometer, the reactor of dropping funnel.
(2). after adding, Succinic Acid continued stirring reaction 40 minutes.Then reaction solution is changed in the still kettle, the cut between collecting 275～290 ℃ obtains the succimide of 15kg, and dry back is stand-by.
(3). thermometer is being housed, is adding 80kg water and 20kg Glacial acetic acid in the reactor of whipping appts and dropping funnel, be stirred into 20% glacial acetic acid solution.Stir down 15kg succimide solid is added in the glacial acetic acid aqueous solution, to its whole dissolvings.
(4). be reduced to below 0 ℃ with icy salt solution cooling system to temperature, low temperature adds the solution that contains the 52.5kg clorox in the mixing solutions of succimide and Glacial acetic acid.The control rate of addition no longer raises system temperature.After adding the solution of clorox, stirred 1.5 hours, obtain mixing solutions.
(5). separate finished product
Mixing solutions is filtered, be washed till neutrality, obtain the white solid powder, be N-chlorosuccinimide finished product.
Embodiment 4:
(1). in 200 liters of reactors, add ammoniacal liquor 70kg, under the state of cooling, keep temperature of reaction at 20～25 ℃.The 50kg Succinic Acid stirred add down among the ammoniacal liquor in batches.Described reactor is for having heating unit, and electricity stirs, thermometer, the reactor of dropping funnel.
(2). after adding, Succinic Acid continued stirring reaction 40 minutes.Then reaction solution is changed in the still kettle, the cut between collecting 275～290 ℃ obtains the succimide of 15kg, and dry back is stand-by.
(3). thermometer is being housed, is adding 83kg water and 17kg Glacial acetic acid in the reactor of whipping appts and dropping funnel, be stirred into 17% glacial acetic acid solution.Stir down 15kg succimide solid is added in the glacial acetic acid aqueous solution, to its whole dissolvings.
(4). be reduced to below 0 ℃ with icy salt solution cooling system to temperature, low temperature adds the solution that contains the 20kg clorox in the mixing solutions of succimide and Glacial acetic acid.The control rate of addition no longer raises system temperature.After adding the solution of clorox, stirred 1 hour, obtain mixing solutions.
(5). separate finished product
Mixing solutions is filtered, be washed till neutrality, obtain the white solid powder, be N-chlorosuccinimide finished product.
Claims (5)
1. the preparation method of a N-chlorosuccinimide, it is characterized in that: preparation process is:
(1). place reactor to be stirred to abundant reaction Succinic Acid and ammoniacal liquor, keeping temperature of reaction is 20～25 ℃;
(2). the reaction solution of Succinic Acid and ammoniacal liquor is placed still kettle, and dehydration obtains the succimide solid in the time of 275～290 ℃;
(3). will be stirred to dissolving fully in the succimide solid adding glacial acetic acid aqueous solution;
(4). the mixing solutions of succimide and Glacial acetic acid is cooled to below 0 ℃, keeps this temperature and add the chlorine bleach liquor, stirred 0.5～1.5 hour, obtain mixing solutions;
(5). with the mixing solutions suction filtration, be washed till neutrality, obtain the white solid powder, be N-chlorosuccinimide finished product.
2. the preparation method of N-chlorosuccinimide according to claim 1 is characterized in that: the ratio of weight and number of described Succinic Acid and ammoniacal liquor is 1: 1.4～1.8.
3. the preparation method of N-chlorosuccinimide according to claim 1 is characterized in that: the concentration of described Glacial acetic acid is 15～20%.
4. the preparation method of N-chlorosuccinimide according to claim 1 is characterized in that: the clorox ratio of weight and number among described succimide and the chlorine bleach liquor is 1: 3～3.5.
5. the preparation method of N-chlorosuccinimide according to claim 1 is characterized in that: described reactor is for having heating unit, and electricity stirs, thermometer, the reactor of dropping funnel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810151988 CN101712644A (en) | 2008-10-06 | 2008-10-06 | Method for preparing N-chlorosuccinimide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810151988 CN101712644A (en) | 2008-10-06 | 2008-10-06 | Method for preparing N-chlorosuccinimide |
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| CN101712644A true CN101712644A (en) | 2010-05-26 |
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| CN 200810151988 Pending CN101712644A (en) | 2008-10-06 | 2008-10-06 | Method for preparing N-chlorosuccinimide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329261A (en) * | 2011-06-24 | 2012-01-25 | 灌南伊斯特化工有限公司 | Production process of N-chlorosuccinimide |
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2008
- 2008-10-06 CN CN 200810151988 patent/CN101712644A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329261A (en) * | 2011-06-24 | 2012-01-25 | 灌南伊斯特化工有限公司 | Production process of N-chlorosuccinimide |
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Open date: 20100526 |