A kind of preparation method of diallyl isophthalate

A technology of diallyl isophthalate and dimethyl isophthalate, applied in the field of preparation of diallyl isophthalate, can solve the problem of increasing the process of separating water-carrying agent and the low product yield , long reaction time and other problems, to achieve the effect of saving additive costs, high product yield, and easy recycling

Active Publication Date: 2021-02-26
SHOUGUANG NUOMENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing disclosed diallyl isophthalate production method is few, mainly contains two kinds, and a kind of is that isophthalic acid and methanol are reacted with toluene or hexanaphthene as water-carrying agent under the catalysis of sulfuric acid , this method increases the process of separating the water-carrying agent, and a part of the material is brought out with the water-carrying agent to increase the consumption. In addition, the existence of the water-carrying agent also affects the quality of the product. This method has a long reaction process and is harmful to the equipment. High requirements, high production cost, low product yield (about 80%), and poor quality
The second is to use isophthalic acid and methanol as raw materials, use concentrated sulfuric acid as a catalyst, put them into the reaction kettle, stir fully and evenly; then, obtain isophthalic acid through heating, synthesis, dealcoholization, alkali washing and rectification Dimethyl ester products, this method has many steps and a long reaction time, basically more than 6 hours, and the product yield is still not high (80-90%), with obvious color

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 300 grams of dimethyl isophthalate, 300 grams of propylene alcohol, and 1.5 grams of potassium carbonate powder into the reactor, start stirring, heat up the reaction, control the reaction temperature in the reactor between 90 and 145 ° C, and rectify the column top Temperature is between 60-95°C, heat preservation reaction for 2-4 hours, sampling test, stop heating when the content of dimethyl isophthalate is less than 0.5%, lower the temperature to below 100°C, add 100 grams of water, continue to cool down to 60°C, Add 0.03 g of decolorizing agent, keep stirring for 0.5 hours, add 0.06 g of reducing agent, stir for 0.5 hours, let stand for 30 minutes, separate layers, add 100 g of water for washing, separate layers, heat up and vacuum distill to remove a small amount of water, and obtain the product. The rate is 99.2%.

Embodiment 2

[0020] Example 2: Add 300 grams of dimethyl isophthalate, 450 grams of propylene alcohol, and 4.5 grams of potassium carbonate powder into the reactor, start stirring, heat up the reaction, and control the reaction temperature in the reactor between 90 and 145 ° C. The temperature at the top of the rectification column is between 60 and 95°C, heat preservation reaction for 2-4 hours, take a sample test, stop heating when the content of dimethyl isophthalate is less than 0.5%, lower the temperature to below 100°C, add 150 grams of water, and continue to cool down to 60°C, add 0.015 g of decolorizing agent, keep stirring for 0.5 hours, add 0.003 g of reducing agent, stir for 0.5 hours, let it stand for 30 minutes, separate layers, add 150 g of water to wash, separate layers, heat up and vacuum distill to remove a small amount of water, The product was obtained with a yield of 99.5%.

Embodiment 3

[0021] Example 3: Add 300 grams of dimethyl isophthalate, 360 grams of propylene alcohol, and 3 grams of potassium carbonate powder into the reactor, start stirring, heat up the reaction, and control the reaction temperature in the reactor between 90 and 145 ° C. The temperature at the top of the rectification column is between 60 and 95°C, keep it warm for 2-4 hours, take a sample test, stop heating when the content of dimethyl isophthalate is less than 0.5%, lower the temperature to below 100°C, add 90 grams of water, and continue to cool down to 60°C, add 0.02 g of decolorizing agent, keep stirring for 0.5 hours, add 0.03 g of reducing agent, stir for 0.5 hours, let it stand for 30 minutes, separate layers, add 90 g of water to wash, separate layers, heat up and vacuum distill to remove a small amount of water, The product was obtained with a yield of 99.8%.

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Abstract

The invention relates to a method for preparing diallyl isophthalate. The method comprises the steps: adding dimethyl isophthalate, propenol, calcium methoxide and/or calcium ethoxide into a reactor,starting to carry out stirring, heating the temperature of the mixture to 90 DEG C to 145 DEG C for a reaction, carrying out a reaction while preserving the temperature of the top of a rectification column to 60 DEG C to 95 DEG C, carrying out sampling for detection, and stopping heating when the content of dimethyl isophthalate is lower than 0.5%; cooling the temperature of the product to 100 DEGC or below, adding water and acid, continuing to cool the temperature of the mixture to 60 DEG C, adding a decolorant, carrying out stirring while carrying out heat preservation, adding a reducer, carrying out stirring, and carrying out standing for layering; and washing a lower layer, carrying out layering, and carrying out reduced pressure distillation while heating to remove a small volume ofwater, thereby obtaining the diallyl isophthalate. According to the method, the efficiency of an ester exchange reaction is greatly increased, the time of the ester exchange reaction is shortened, thereaction time is short and is one third of that of an original process, and thus, the processing cost can be greatly reduced; the product yield reaches 99% or more, the catalyst is soluble in water,and the recovery treatment is facilitated; and the process is simple, filter pressing operation is not required during production, and thus, the method is more adaptable to advanced operating processes such as automated production.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing diallyl isophthalate. Background technique [0002] Existing disclosed diallyl isophthalate production method is few, mainly contains two kinds, and a kind of is that isophthalic acid and methanol are reacted with toluene or hexanaphthene as water-carrying agent under the catalysis of sulfuric acid , this method increases the process of separating the water-carrying agent, and a part of the material is brought out with the water-carrying agent to increase the consumption. In addition, the existence of the water-carrying agent also affects the quality of the product. This method has a long reaction process and is harmful to the equipment. The requirements are high, the production cost is high, the product yield is low (about 80%), and the quality is poor. The second is to use isophthalic acid and methanol as raw materials, use concentrated sulfuric a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/80C07C67/03C07C67/48
CPCC07C67/03C07C67/48C07C69/80
Inventor 刘在成李庆山王光明
Owner SHOUGUANG NUOMENG CHEM
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