Method for preparing triethylene glycol dimethacrylate

A technology of triethylene glycol dimethacrylate and triethylene glycol, which is applied in the field of synthesis and preparation of chemical products, can solve problems such as low product yield, material polymerization, and inability to meet the needs of high-quality products. Achieve high product purity, increase product yield, and facilitate control

Inactive Publication Date: 2011-08-10
天津市天骄辐射固化材料有限公司
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Problems solved by technology

[0002] At present, the preparation and production technology of triethylene glycol dimethacrylate adopts the method of normal pressure esterification, the reaction process is easy to cause material polymerization, the product color is dark, the color number is usually greater than No. 70, the product yield is low, and the product yield is low. The rate is generally lower than 70%, which cannot meet the needs of preparing and producing high-quality products

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  • Method for preparing triethylene glycol dimethacrylate

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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 triethylene glycol dimethacrylate, comprising the following steps:

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

[0015] (2) Turn on the vacuum pump on the esterification reaction vessel, control t...

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Abstract

The invention discloses a method for preparing triethylene glycol dimethacrylate, which comprises the following steps of: (1) putting main materials of triethylene glycol 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 3-5mgKOH / 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 triethylene glycol dimethacrylate. Triethylene glycol dimethacrylate is suitable for radiation curing reactive dilution. agent. Background technique [0002] At present, the preparation and production technology of triethylene glycol dimethacrylate adopts the normal pressure esterification method. The reaction process can easily cause material polymerization. The product color is dark, and the color number is usually greater than No. 70. The product yield is low, and the product yield is low. The rate is generally less than 70%, which cannot meet the needs of preparing and producing high-quality products. Contents of the invention [0003] In order to solve the technical problems existing in the known technology, the present invention provides a preparation method of triethylene glycol dimethacrylate. This method can reduce ...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08
Inventor 黄凤岐李健
Owner 天津市天骄辐射固化材料有限公司
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