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After-reaction processing method for preparation of diacetone-acrylamide

A technology of acetone acrylamide and acrylamide, applied in the separation/purification of carboxylic acid amide, organic chemistry and other directions, can solve the problems of reduced DAAM yield, high energy consumption, large investment, etc., to reduce the difficulty of subsequent purification, reduce decomposition, avoid The effect of investment and high cost

Inactive Publication Date: 2016-11-16
张华堂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Dealing with a large amount of inorganic wastewater produced in the process of preparing diacetone acrylamide in the prior art requires large investment and high energy consumption, and at the same time, environmental problems such as wastewater discharge are prone to occur
At the same time, due to the preparation of diacetone acrylamide, various side reactions will occur and various by-products will be formed, causing DAAM to be difficult to separate, thereby bringing the problem of DAAM yield reduction

Method used

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  • After-reaction processing method for preparation of diacetone-acrylamide
  • After-reaction processing method for preparation of diacetone-acrylamide
  • After-reaction processing method for preparation of diacetone-acrylamide

Examples

Experimental program
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Embodiment approach

[0039] (1) Use saturated ammonium sulfate aqueous solution to mix with the reaction mixture, feed ammonia gas to neutralize the hydrolysis mixture, separate out ammonium sulfate solid in the neutralization process, separate out ammonium sulfate solid (i.e. by-product), ammonium sulfate aqueous solution (return to Hydrolysis process recycling) and organic layer (neutralization product, ie diacetone acrylamide crude product).

[0040] (2) Use saturated ammonium sulfate aqueous solution to mix with the reaction mixture, then stand still or separate the heavy phase and the light phase with continuous chromatography. The heavy phase is neutralized with ammonia gas, and ammonium sulfate solid is precipitated during the neutralization process, and ammonium sulfate solid (i.e. by-product), ammonium sulfate aqueous solution (returned to the hydrolysis process for recycling) and organic layer are separated separately, and air can be introduced before phase separation The organic matter ...

Embodiment 1

[0048] Take 200 g of the reaction mixture obtained by reacting acrylonitrile and acetone under the action of concentrated sulfuric acid, add it into a four-neck flask with a thermometer, and start stirring. Slowly add 600 g of saturated ammonium sulfate aqueous solution into the four-neck flask, and continue stirring for 30 minutes after the addition is complete. Ammonia gas was introduced slowly, the temperature was controlled below 20°C, the pH value at the end point of neutralization was 8.5, and the stirring was continued for 30 minutes to stop. All the materials were added to the separatory funnel, and allowed to stand for 60 minutes, and the ammonium sulfate solid, ammonium sulfate aqueous solution and organic layer were separated successively. 97g of organic layer (containing water) was obtained, which contained 60g of DAAM.

Embodiment 2

[0050] Take 200 g of the reaction mixture obtained by reacting acrylonitrile and diacetone alcohol under the action of concentrated sulfuric acid, add it into a four-neck flask with a thermometer, and start stirring. Get 400g of 40% ammonium sulfate aqueous solution and add slowly into the four-necked flask, and stop stirring after adding and continuing to stir for 30 minutes. All the hydrolyzed materials were added to the separatory funnel and allowed to stand for 60 minutes. Separate the heavy phase, add it to a four-necked bottle with a thermometer, start stirring, slowly introduce ammonia gas, control the temperature below 50°C, neutralize to pH 7.5, continue stirring for 15 minutes, stop stirring, and add all the materials to the liquid funnel, put air into it for flotation for 30 minutes, let it stand for 60 minutes, separate the ammonium sulfate solid, ammonium sulfate aqueous solution and organic layer in sequence; % ammonia water, the temperature is controlled below ...

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Abstract

The invention discloses an after-reaction processing method for preparation of diacetone-acrylamide. The method comprises the steps that a hydrolysis medium is added into a protonic acid containing diacetone-acrylamide reaction mixture for a hydrolysis reaction, and a hydrolysis mixture is obtained; alkaline matter is added into the hydrolysis mixture and carries out a neutralization reaction with protonic acid, and a neutralization mixture is obtained; the neutralization mixture is layered, and separation is conducted to obtain a protonic acid salt solid, a protonic acid salt water solution and a diacetone-acrylamide containing organic layer. The method can be used for processing the reaction mixture obtained during preparation of diacetone-acrylamide and can also be used for processing diacetone-acrylamide or acrylamide containing mixtures obtained in other ways.

Description

technical field [0001] The invention relates to a reaction mixture containing diacetone acrylamide, generally a method for post-processing the reaction mixture for preparing diacetone acrylamide. In particular, the present invention relates to a process for treating a reaction mixture for the preparation of diacetone acrylamide comprising hydrolysis and neutralization steps. Background technique [0002] Diacetone Acrylamide (English name Diacetone Acrylamide, referred to as DAAM) is a reactive multifunctional monomer, which can be polymerized with unsaturated monomers such as acrylic acid, acrylate and styrene to form copolymers through carbon-carbon double bonds. The ketone carbon group in the molecular chain of the polymer can react with the hydrazine group at room temperature to improve the crosslinking performance of the polymer. Diacetone acrylamide occupies an important position in the chemical industry, so since it was first synthesized in 1965, it has received more...

Claims

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Application Information

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IPC IPC(8): C07C231/22C07C231/24C07C233/31
CPCC07C231/22C07C231/24
Inventor 张华堂
Owner 张华堂
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