Method for preparing 2-methyl-2-propenoic acid 2-ethyl-2-[[(2-methyl-1-oxo-2-propenyl)oxy]methyl]-1,3-propanediyl ester

A technology of trimethylolpropane trimethacrylate and methylolpropane trimethacrylate, which is applied in the field of synthesis and preparation of chemical products, can solve the problem of inability to meet the needs of high-quality products, low product yield, and material Polymerization and other problems, to achieve the effect of convenient control, high product purity, and increase product yield

Inactive Publication Date: 2011-08-10
天津市天骄化工有限公司
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Problems solved by technology

[0002] At present, the preparation and production technology of trimethylolpropane methacrylate adopts the method of atmospheric pressure esterification, the reaction process is easy to cause material polymerization, the product color is dark, the color number is usually greater than 70, the product yield is low, and the product yield is average Less than 70%, cannot meet the needs of preparing and producing high-quality products

Method used

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  • Method for preparing 2-methyl-2-propenoic acid 2-ethyl-2-[[(2-methyl-1-oxo-2-propenyl)oxy]methyl]-1,3-propanediyl ester

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Embodiment Construction

[0012] In order to further understand the content of the invention, features and effects of the present invention, the following examples are given hereby, and the details are as follows:

[0013] A preparation method of trimethylolpropane trimethacrylate, comprising the following steps:

[0014] (1) The same as the existing atmospheric pressure esterification method, the main ingredients trimethylolpropane and methacrylic acid are put into the esterification reaction container, according to the mass percentage of the total amount of trimethylolpropane and methacrylic acid 50-90% of toluene is added, p-toluenesulfonic acid is added according to 1.2-4.2% of the total mass percentage of trimethylolpropane and methacrylic acid, and p-toluenesulfonic acid is added according to 0.3-0.5% of the total mass percentage of trimethylolpropane and methacrylic acid % add phenothiazine, stir for 2-9 hours, carry out esterification reaction, obtain reaction material;

[0015] (2) Turn on th...

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Abstract

The invention discloses a method for preparing 2-methyl-2-propenoic acid 2-ethyl-2-[[(2-methyl-1-oxo-2-propenyl)oxy]methyl]-1,3-propanediyl ester, which comprises the following steps of: (1) putting main materials of trimethylolpropane and methacrylic acid into an esterification reaction container, adding a solvent, adding a catalyst and a polymerization inhibitor A, and performing mixing reaction to obtain a reaction material; (2) controlling the pressure in the esterification reaction container to be -0.04 to -0.08MPa, raising the temperature in the esterification reaction container until reflux flows out, keeping the temperature, and beginning cooling to normal temperature until no reflux flows out or an acid value in reaction solution is detected to be 30-50mgKOH / g; (3) transferring the reaction material to a washing container, adding alkali liquor, controlling the pH value of the reaction material to be 7-8, standing until the reaction material is layered, and discharging wastewater on the lower layer; and (4) transferring the reaction material of which the wastewater is removed to a distillation container, adding a polymerization inhibitor B, vacuumizing the distillation container, and distilling to remove methylbenzene to obtain the product. The product is high in purity, good in color, and high in yield.

Description

technical field [0001] The invention relates to a synthesis and preparation technology of chemical products, in particular to a preparation method of trimethylolpropane methacrylate, which is suitable for use as a radiation curing reactive diluent. Background technique [0002] At present, the preparation and production technology of trimethylolpropane methacrylate adopts the method of atmospheric pressure esterification, the reaction process is easy to cause material polymerization, the product color is dark, the color number is usually greater than 70, the product yield is low, and the product yield is average Less than 70%, can not meet the needs of preparing and producing high-quality products. Contents of the invention [0003] The invention provides a method for preparing trimethylolpropane trimethacrylate to solve the technical problems in the known technology. The method can reduce the generation of polymers, and the product has light color, high quality and high y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54
Inventor 黄凤岐李健
Owner 天津市天骄化工有限公司
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