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Preparation method of ethoxylated trimethylolpropane triacrylic ester

A technology of ethoxylated trimethylolpropane triacrylate and cyclohexane, which is applied in the field of preparation of ethoxylated trimethylolpropane triacrylate, can solve the problems of not having product adjustment functions, and achieve Reduce environmental damage, less irritation, and less environmental damage

Inactive Publication Date: 2011-09-07
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the production method of ethoxylated trimethylolpropane triacrylate involved in the existing patent, activated carbon is used as the adsorbent, and the activated carbon only has adsorption function, and does not have the function of product regulation, and the prepared product also has certain limitations in use

Method used

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  • Preparation method of ethoxylated trimethylolpropane triacrylic ester
  • Preparation method of ethoxylated trimethylolpropane triacrylic ester
  • Preparation method of ethoxylated trimethylolpropane triacrylic ester

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A preparation method of ethoxylated trimethylolpropane triacrylate, the steps are:

[0026] (1). Put the following components into the reaction kettle in turn according to the following weight ratio:

[0027]

[0028] (2) Then put the following components into the reaction kettle in sequence according to the content:

[0029] Phenothiazine 50ppm

[0030] Hydroquinone 150ppm

[0031] Copper sulfate 800ppm

[0032] (3) The above-mentioned components are fully mixed and stirred in the reactor, and the steam valve is opened to heat slowly, and the heating rate is controlled so that the vapor pressure is 0.3-0.5MPa; the reaction temperature is controlled at 70°C within 1 hour and reacted for 4 hours; Continue the reaction when the temperature rises to 110-116° C., and the reaction ends when the reflux reaches about 6 hours. Take a sample for detection. When the acid value is about 10-40, it indicates that the reaction is over.

[0033] (4) add 15% strongly basic anion...

Embodiment 2

[0037] A preparation method of ethoxylated trimethylolpropane triacrylate, the steps are:

[0038] (1). Put the following components into the reaction kettle in turn according to the following weight ratio:

[0039]

[0040] (2) Then put the following components into the reaction kettle in sequence according to the content:

[0041] Phenothiazine 300ppm

[0042] Hydroquinone 100ppm

[0043] Copper sulfate 550ppm

[0044] (3) Mix the above components in the reactor, then open the steam valve to heat slowly, and control the air pressure to 0.3-0.5MPA; within 1 hour, the reaction temperature is controlled at 80°C and reacted for 3 hours, when the temperature rises to 110-116°C React for 5 hours and the reaction ends when the temperature rises to 118-120°C. Take a sample for inspection. When the acid value is about 10-40, it indicates that the reaction is over;

[0045] (4) Add 20% strongly basic anion exchange resin (D296 type) to the reaction kettle to neutralize to neutr...

Embodiment 3

[0048] A preparation method of ethoxylated trimethylolpropane triacrylate, the steps are:

[0049] (1). Put the following components into the reaction kettle in turn according to the following weight ratio:

[0050]

[0051] (2) Then put the following components into the reaction kettle in sequence according to the content:

[0052] Phenothiazine 300ppm

[0053] Hydroquinone 100ppm

[0054] Copper sulfate 800ppm

[0055] (3) The above-mentioned components are fully mixed and stirred in the reactor, and the steam valve is opened to heat slowly, and the heating rate is controlled so that the vapor pressure is 0.3-0.5MPa; the reaction temperature is controlled at 90°C within 1 hour and reacted for 4 hours; When the temperature rises to 110-116°C, continue to react for 6 hours, take a sample for detection, and when the acid value is about 10-40, it indicates that the reaction is over;

[0056] (4) Add 25% strongly basic anion exchange resin (D296 type) to neutralize to neut...

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Abstract

The invention relates to a preparation method of ethoxylated trimethylolpropane triacrylic ester. The preparation method comprises the following steps of: (1) mixing raw materials and reacting under heat by stages; (2) adding resin to neutralize; and (3) removing a solvent at the temperature of between 70 and 90 DEG C and under the vacuum degree of -0.09 to -0.1 MPa, and cooling to obtain the finished product. On the basis of the conventional production method, the original active carbon is replaced by strong-basicity anion exchange resin, wherein the newly adopted resin has adsorption effect and can also serve as solid alkali to neutralize the residual acidic crylic acid and para-toluenesulfonic acid; the effect not only is the simple replacement of an adsorbent and but also relates to adjustment of pH value of the product solution; 3 tons of waste water is reduced in the production process of each ton of finished products; damage to the environment caused by the discharged substances is reduced; and no 'three wastes' exist so the finished products are more environment-friendly.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a preparation method of ethoxylated trimethylolpropane triacrylate. Background technique [0002] Acrylate is an important acrylic functional monomer, which is widely used in many fields such as coatings, adhesives, electronics and composite materials. The cured film formed by it has strong wear resistance and corrosion resistance, and is currently the most widely used multifunctional reactive diluent monomer. However, the existing acrylates adopt the method of direct esterification of alkyd to produce high acid value, large irritation, large amount of waste water, high production cost and many other disadvantages. Examples: 1. Great irritation to human skin; 2. High viscosity; 3. Large shrinkage rate; 4. Poor environmental protection performance. The advantages of ethoxylated trimethylolpropane triacrylate are less irritation to human skin, low shrinkage, low viscosity, high acti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/08
Inventor 赵德章
Owner TIANJIN CHEM REAGENT RES INST
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