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Method for preparing N-dimethylamino propyl methyl acrylamide

A dimethylaminopropyl methacrylamide, catalytic cracking technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid amides, etc., can solve problems affecting product quality, blockage of reaction equipment, production and operation difficulties, etc. problems, to achieve the effect of less three wastes, less by-products and less polymers

Inactive Publication Date: 2008-05-14
本溪万哈特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The advantage of this method is that the steps are short and the conversion rate is high; the disadvantage is that the excess methyl methacrylate is easy to polymerize and difficult to recycle, and the produced polymer not only affects the product quality, but also blocks the reaction equipment, making the production operation difficult

Method used

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  • Method for preparing N-dimethylamino propyl methyl acrylamide
  • Method for preparing N-dimethylamino propyl methyl acrylamide
  • Method for preparing N-dimethylamino propyl methyl acrylamide

Examples

Experimental program
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Effect test

Embodiment 1

[0037] step 1:

[0038] 100 grams of methyl methacrylate, 300 grams of N,N-dimethyl-1,3-propanediamine were added into the reaction kettle, and 8 grams of carbon dioxide were introduced into the reactor, stirred and heated to 100°C for 6 hours, then cooled and evaporated under reduced pressure. Excessive N, N-dimethyl-1,3-propanediamine is the intermediate product N-dimethylaminopropyl-β-dipropylaminomethacrylamide.

[0039] Step 2:

[0040] 1 g Ca(NO 3 ) 2 4H 2 0, 18 grams of above-mentioned intermediate products are added in the reaction flask that has vacuum distillation unit, decompression is to 10mmHg, when stirring is warming up to 220 ℃, raw material and product are distilled out, intermediate product and Ca(NO 3 ) 2 4H 2O was slowly dripped into the reaction flask, and the cracked products and raw materials were also distilled out during the dropping process. After 5 hours, the reaction was completed, and the distillate contained 31.1% of the raw material N,N-di...

Embodiment 2

[0044] step 1:

[0045] Pass 20 grams of carbon dioxide into the reactor, stir and heat up to 90°C for 7 hours, and the others are the same as in Example 1;

[0046] Step 2:

[0047] 0.9 g Ca(NO 3 ) 2 4H 2 0, 18 gram intermediate products add in the reaction bottle that has vacuum distillation unit, stir and be warming up to 240 ℃, other are with embodiment one;

[0048] Step 3:

[0049] 1.3 gram of p-hydroxyanisole is added in the reaction bottle of rectification tower, other is the same as embodiment one.

Embodiment 3

[0051] step 1:

[0052] Feed 14 grams of carbon dioxide into the reactor, stir and heat up to 96°C for 6.5 hours, and the others are the same as in Example 1;

[0053] Step 2:

[0054] 0.95 g Ca(NO 3 ) 2 4H 2 0, 18 gram intermediate products add in the reaction flask that has vacuum distillation unit, stir and be warming up to 230 ℃, other are with embodiment one;

[0055] Step 3:

[0056] 1 gram of p-hydroxyanisole is added in the reaction flask of the rectifying tower, and the others are the same as in Example 1.

[0057] As a result of implementation, the total yield can reach 70%, and the product content is 98%.

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Abstract

The invention relates to a method for preparing N-dimethylamino propyl methacrylamide by catalyzing and cracking, which comprises the following technical steps: A. two incipient ingredients methyl methacrylate and N, N-dimethyl-1, 3-propane diamine are sealed in an autoclave for catalyzing and condensing, so as to generate the intermediate N-dimethylamino-Beta-dimethylamino methacrylamide; B. putting the intermediate N-dimethylamino-Beta-dimethylamino methacrylamide into a reactor with distilling apparatus and driving off the crude products of N-dimethylamino propyl methacrylamide through catalyzing and cracking; C. adding the crude products of N-dimethylamino propyl methacrylamide and polymerization inhibitor into a rectifying tower to generate the finished products. The invention has the advantages of less reaction steps, high conversion rate, small amount of byproducts, low cost for post treatment, and ability to meet application demand.

Description

technical field [0001] The invention relates to a preparation method of N-dimethylaminopropyl methacrylamide. Background technique [0002] N-(3-dimethylamino)propyl methacrylamide (DMAPMA) is a very important fine chemical intermediate and monomer. The polymer synthesized from it as the main intermediate belongs to the fourth generation flocculant and The third generation of oil extraction additives, which are widely used in coatings, resins, electroplating, printing and dyeing, water treatment flocculants, membrane technology, medicine, cosmetics and other industries. The global development and application of this product began in the 1960s. However, by the end of the last century, the application of this product was still not very extensive. After entering the 21st century, foreign countries have successively developed a large number of very good quality fine New chemical products, including cosmetics, shampoo products, high-grade coatings, ionic membranes, etc., have ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/38C07C231/02
Inventor 马臣孟明扬马瑛谭立哲杨文东高晓春柴义沈宝林
Owner 本溪万哈特化工有限公司
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