CN101397262A - Preparation method of N-butoxymethyl acrylamide - Google Patents
Preparation method of N-butoxymethyl acrylamide Download PDFInfo
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- CN101397262A CN101397262A CNA200710061285XA CN200710061285A CN101397262A CN 101397262 A CN101397262 A CN 101397262A CN A200710061285X A CNA200710061285X A CN A200710061285XA CN 200710061285 A CN200710061285 A CN 200710061285A CN 101397262 A CN101397262 A CN 101397262A
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- butoxymethyl acrylamide
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Abstract
The invention relates to an N-butoxyl methacrylamide preparation method including three steps: (1) etherification; (2) washing which includes three steps: A salt water is added into a mixture obtained from the reaction of the step (1), then stirred evenly and statically placed for layering, and water layer is removed; B alkali water is added into the mixture washed by the salt water, then stirred evenly and statically placed for layering, and the water layer is removed; and C clear water is added into the mixture washed by the alkali water, then stirred evenly and statically placed for layering, and the water layer is removed; and (3) decompression for desolvation: benzene is steamed out from the mixture by using a water jet pump and the remaining reagent is the final product. The method adopts the step of washing to displace the traditional decompression refining step so as to largely reduce the manufacturing cost, enhance the market competence of enterprises; in addition, the washing step can be easily operated and realized, can reduce work time effectively and enhance the manufacturing efficiency.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of preparation method of N-butoxymethyl acrylamide.
Background technology
The N-butoxymethyl acrylamide is used widely as a kind of important organic intermediate.The step of making the N-butoxymethyl acrylamide at present is generally: 1. etherification reaction makes this product; 2. decompression desolventizing; 3. decompression purified product.Wherein the 2nd step and the 3rd step all are underpressure distillation, but the vacuum tightness of the 2nd step needs is low, that is to say that vacuum pump low for equipment requirements, general can meet the demands.And the 3rd the vacuum tightness height that step needs, common vacuum pump can't meet the demands, and must use the high equipment of price during production.Therefore increase the production time of product, reduced production efficiency, and caused production cost to rise, be unfavorable for the raising of business economic benefit.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and needn't adopt the underpressure distillation purification step, can save man-hour, reduce cost and the preparation method of the N-butoxymethyl acrylamide that production efficiency is high.
The present invention solves its technical problem and is achieved through the following technical solutions:
A kind of preparation method of N-butoxymethyl acrylamide the steps include:
(1). etherification reaction
Acrylamide, Paraformaldehyde 96, butanols and benzene are mixed reflux water-dividing reaction 8-12 hour;
(2). washing
1.. add salt solution in mixture after etherification, stir, standing demix discards water layer then;
2.. add buck in the mixture after the salt washing, stir, standing demix discards water layer then;
3.. add clear water in the mixture after buck is washed, stir, standing demix discards water layer then;
(3). the decompression desolventizing
With water jet pump benzene in the mixture is steamed, remaining reagent is N-butoxymethyl acrylamide finished product.
And the ratio of weight and number of described acrylamide, Paraformaldehyde 96, butanols and benzene is 2:1:4:0.4.
And the reaction vessel in the described etherification reaction work step is the reactor that has condenser, water trap and agitator.
And described salt solution is that concentration is the sodium chloride solution of 8-12%, and the ratio of weight and number of this sodium chloride solution and acrylamide is 2:1.
And described buck is that concentration is the sodium carbonate solution of 0.8-1.2%, and the ratio of weight and number of this sodium carbonate solution and acrylamide is 2:1.
And the ratio of weight and number of described clear water and acrylamide is 2:1.
And described water jet pump is the water jet pump of 35mmHg.
Advantage of the present invention and beneficial effect are:
1. the present invention adopts water-washing step to substitute traditional decompression purification step, and all qualified by the every index of product after the water-washing step processing.Owing to needn't adopt expensive specific equipment again when producing, therefore greatly reduced production cost, improved the market competitiveness of enterprise, make this product can on market, obtain bigger applying.
2. the water-washing step that the present invention increased newly is simple, processing ease, is easy to realize that industrialization production and process for processing time are short, has greatly improved production efficiency, has shortened man-hour.
3. the present invention replaces traditional decompression purification step by adopting water-washing step, greatly reduced production cost, improved the market competitiveness of enterprise, and this water-washing step simple to operate, be easy to realize and can shorten man-hour effectively, enhance productivity.
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.
The preparation method of this N-butoxymethyl acrylamide is characterized in that its preparation process is:
Embodiment 1:
(1). etherification reaction
Get the 100Kg acrylamide, the 50Kg Paraformaldehyde 96, the 200Kg butanols, in the stirred autoclave of 0.2Kg solvent benzol input band condenser and water trap, reflux water-dividing reaction 8 hours.
(2). washing
1.. adding concentration is 8% sodium chloride solution 200Kg in the mixture of reaction back gained in step (1), stirs, and standing demix then is at last with water layer discarded;
2.. add concentration in the mixture after sodium chloride solution is washed and be 0.8% sodium carbonate solution 200Kg, stir, standing demix then is at last with water layer discarded;
3.. add clear water 200Kg in the mixture after sodium carbonate solution is washed, stir, standing demix then is at last with water layer discarded.
(3). the decompression desolventizing
Water jet pump with 35mmHg steams solvent benzol in the mixture, and remaining reagent is finished product, can pack sale.
Embodiment 2
(1). etherification reaction
Get the 100Kg acrylamide, the 50Kg Paraformaldehyde 96, the 200Kg butanols, in the stirred autoclave of 0.2Kg solvent benzol input band condenser and water trap, reflux water-dividing reaction 10 hours.
(2). washing
1.. adding concentration is 10% sodium chloride solution 200Kg in the mixture of reaction back gained in step (1), stirs, and standing demix then is at last with water layer discarded;
2.. add concentration in the mixture after sodium chloride solution is washed and be 1% sodium carbonate solution 200Kg, stir, standing demix then is at last with water layer discarded;
3.. add clear water 200Kg in the mixture after sodium carbonate solution is washed, stir, standing demix then is at last with water layer discarded.
(3). the decompression desolventizing
Water jet pump with 35mmHg steams solvent benzol in the mixture, and remaining reagent is finished product, can pack sale.
Embodiment 3
(1). etherification reaction
Get the 100Kg acrylamide, the 50Kg Paraformaldehyde 96, the 200Kg butanols, in the stirred autoclave of 0.2Kg solvent benzol input band condenser and water trap, reflux water-dividing reaction 12 hours.
(2). washing
1.. adding concentration is 12% sodium chloride solution 200Kg in the mixture of reaction back gained in step (1), stirs, and standing demix then is at last with water layer discarded;
2.. add concentration in the mixture after sodium chloride solution is washed and be 1.2% sodium carbonate solution 200Kg, stir, standing demix then is at last with water layer discarded;
3.. add clear water 200Kg in the mixture after sodium carbonate solution is washed, stir, standing demix then is at last with water layer discarded.
(3). the decompression desolventizing
Water jet pump with 35mmHg steams solvent benzol in the mixture, and remaining reagent is finished product, can pack sale.
Claims (7)
1. the preparation method of a N-butoxymethyl acrylamide, it is characterized in that: preparation process is:
(1). etherification reaction
Acrylamide, Paraformaldehyde 96, butanols and benzene are mixed reflux water-dividing reaction 8-12 hour;
(2). washing
1.. add salt solution in mixture after etherification, stir, standing demix discards water layer then;
2.. add buck in the mixture after the salt washing, stir, standing demix discards water layer then;
3.. add clear water in the mixture after buck is washed, stir, standing demix discards water layer then;
(3). the decompression desolventizing
With water jet pump benzene in the mixture is steamed, remaining reagent is N-butoxymethyl acrylamide finished product.
2. the preparation method of N-butoxymethyl acrylamide according to claim 1 is characterized in that: the ratio of weight and number of described acrylamide, Paraformaldehyde 96, butanols and benzene is 2: 1:4:0.4.
3. the preparation method of N-butoxymethyl acrylamide according to claim 1 is characterized in that: the reaction vessel in the described etherification reaction work step is the reactor that has condenser, water trap and agitator.
4. the preparation method of N-butoxymethyl acrylamide according to claim 1 is characterized in that: described salt solution is that concentration is the sodium chloride solution of 8-12%, and the ratio of weight and number of this sodium chloride solution and acrylamide is 2:1.
5. the preparation method of N-butoxymethyl acrylamide according to claim 1 is characterized in that: described buck is that concentration is the sodium carbonate solution of 0.8-1.2%, and the ratio of weight and number of this sodium carbonate solution and acrylamide is 2:1.
6. the preparation method of N-butoxymethyl acrylamide according to claim 1 is characterized in that: the ratio of weight and number of described clear water and acrylamide is 2:1.
7. the preparation method of N-butoxymethyl acrylamide according to claim 1 is characterized in that: described water jet pump is the water jet pump of 35mmHg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710061285XA CN101397262B (en) | 2007-09-28 | 2007-09-28 | Preparation method of N-butoxymethyl acrylamide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710061285XA CN101397262B (en) | 2007-09-28 | 2007-09-28 | Preparation method of N-butoxymethyl acrylamide |
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| CN101397262A true CN101397262A (en) | 2009-04-01 |
| CN101397262B CN101397262B (en) | 2012-06-27 |
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| CN200710061285XA Expired - Fee Related CN101397262B (en) | 2007-09-28 | 2007-09-28 | Preparation method of N-butoxymethyl acrylamide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315624A (en) * | 2021-11-26 | 2022-04-12 | 浙江鑫甬生物化工股份有限公司 | Synthesis and purification method of high-purity N-N-butoxy methacrylamide (NBMA) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002265424A (en) * | 2001-03-08 | 2002-09-18 | Mitsubishi Rayon Co Ltd | N-alkoxymethylacrylamide, method for producing the same and method for producing crystal and aqueous solution of n-methylolacrylamide |
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- 2007-09-28 CN CN200710061285XA patent/CN101397262B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315624A (en) * | 2021-11-26 | 2022-04-12 | 浙江鑫甬生物化工股份有限公司 | Synthesis and purification method of high-purity N-N-butoxy methacrylamide (NBMA) |
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| CN101397262B (en) | 2012-06-27 |
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Owner name: TIANJING CHEMICAL REAGENT RESEARCH INSTITUTE CO., Free format text: FORMER NAME: TIANJIN CHEMICAL RESEARCH INSTITUTE |
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Address after: 300240 Tianjin Admiralty street Dongli District Xu Zhuangzi Patentee after: TIANJIN CHEMICAL REAGENT RESEARCH INSTITUTE CO., LTD. Address before: 300240 Xu Zhuangzi, Dongli District, Tianjin Patentee before: Tianjin chemical research institute |
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