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Synthesis technology of diacetone acrylamide

A technology of diacetone acrylamide and acetone acrylamide, which is applied in the field of synthesis technology of diacetone acrylamide, can solve the problems of low product yield, difficult waste liquid treatment, complex production process, etc., simplify the purification steps and reduce product loss , the effect of solving environmental pollution

Inactive Publication Date: 2011-05-18
FUZHOU NINGCHUANG AGRI RESOURCES DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many side reactions in the prior art synthesis of this product, and the by-products are difficult to remove, so there are many post-treatment steps, and the production process is complicated, the product yield is low, the product quality is unstable, and the waste liquid is difficult to handle.
Due to the limitation of production technology, the current domestic production capacity of this product is far from meeting the needs of the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 3

[0014] Embodiment 3: Mechanical stirring, reflux condenser, dropping funnel, and thermometer are installed in the four-necked bottle. Take 32g (0.55 mol) of acetone, 26.5g (0.5 mol) of acrylonitrile, and 49g (0.5 mol) of sulfuric acid. Add concentrated sulfuric acid into the four-neck flask. Start stirring, and drop the mixed mixture of acrylonitrile and acetone evenly and slowly within 1-1.5 hours into the reaction bottle equipped with concentrated sulfuric acid, and keep T during the dropping process. 1 = 3°C. Then the temperature was slowly raised to the reaction temperature T 2 =45°C, keep the temperature for reaction time t=4h. Cool down to 15°C. Slowly add 20% sodium hydroxide aqueous solution to neutralize to PH=7.0 within 0.5 hours, and cool down to 0-5oC. Filter to obtain 149 g of sodium sulfate hydrate crystals. After suction filtration, the filtrate was allowed to stand and separate layers to obtain the crude product P1 of the organic layer = 81.2 g. P was me...

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PUM

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Abstract

The invention relates to a synthesis technology of diacetone acrylamide, belonging to the technical field of chemical materials. The synthesis technology comprises the following steps: reacting acetone and acrylonitrile in concentrated sulfuric acid, neutralizing by sodium hydroxide, filtering and layering the filtrate to obtain the crude product of diacetone acrylamide. The synthesis technology is characterized by also comprising the following steps: extracting the crude product of diacetone acrylamide with water; extracting with cyclohexane; salting out by NaCl; under a vacuum condition of 666KPa, separating the acrylamide byproduct by reduced pressure distillation according to the characteristic that the difference between the boiling points of acrylamide and diacetone acrylamide is higher than 40 DEG C; after diluting by toluene, drying by anhydrous sodium sulfate and decolorizing by activated carbon, carrying out reduced pressure distillation again, and collecting the distillate at 120-130 DEG C / 666Pa; and finally obtaining the finished product of diacetone acrylamide the quality purity of which is above 98% and the melting point of which is 54-56 DEG C. The invention omits a caustic washing step in the purification process, thus simplifying the purification step and reducing the product loss. The yield of the product is close to 70%, the purity of the product exceeds 98%, and the yield is higher than that (40-50%) of the existing technology.

Description

technical field [0001] The invention relates to a synthesis process of diacetone acrylamide, which belongs to the technical field of chemical materials. Background technique [0002] Diacetone acrylamide is a new type of multifunctional additive that has attracted much attention in recent years. It has been used in the following fields: 1) as a substitute for industrial gelatin; Used in water-based wood paint and interior wall paint. In addition, it has good application prospects in the fields of water-based paint additives, adhesives, epoxy resin curing agents, photosensitive resin additives, textile additives, etc., and the market demand for this product is increasing. However, there are multiple side reactions in the prior art synthesis of this product, and the by-products are difficult to remove, so there are many post-treatment steps, and the production process is complicated, the product yield is low, the product quality is unstable, and the waste liquid is difficult ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/31C07C231/06
Inventor 苏彩秀崔月芝危冬发曾爱民
Owner FUZHOU NINGCHUANG AGRI RESOURCES DEV
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