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Pentaerythrite tetra(2-methyl-1,2-dibromoacrylate) and preparation method thereof

A technology of pentaerythritol tetramethyl methacrylate and dibromoacrylate, which is applied in the field of synthesis of pentaerythritol tetramethacrylate and its preparation, can solve the problems of high equipment material requirements, decreased product yield, cumbersome reaction operations, etc., and achieve special performance, structure Regular and simple operation requirements

Inactive Publication Date: 2012-01-04
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above method, pentaerythritol is used as a nucleophile to attack the carbon atom on the 2-dichloroacetyl chloride carbonyl to undergo a nucleophilic addition reaction. Although it is easier to introduce a halogen atom, due to the very active chemical properties of the acid chloride, it is easy to dissolve in water in the air. Explain that hydrogen chloride is released, so that the above reaction is not easy to occur, resulting in a decrease in product yield
Therefore, the above reaction must be dewatered before the reaction, and in order to prevent the intrusion of water vapor in the air, the reaction must be carried out under a dry nitrogen or argon atmosphere, which leads to cumbersome reaction operations and high requirements for equipment materials, which will undoubtedly increase cost of production

Method used

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  • Pentaerythrite tetra(2-methyl-1,2-dibromoacrylate) and preparation method thereof
  • Pentaerythrite tetra(2-methyl-1,2-dibromoacrylate) and preparation method thereof
  • Pentaerythrite tetra(2-methyl-1,2-dibromoacrylate) and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Get 1.28g (8mmol) liquid bromine and be dissolved in 10mL carbon tetrachloride, be mixed with the solution that mass percent is 7.4%, 0.816g (2mmol) pentaerythritol tetramethylmethacrylate is joined in the above-mentioned configured solution, in Sealed and refluxed at 30°C for 12 hours. During the experiment, the reddish-brown color of bromine gradually faded and solids formed. After the reaction, the solid-liquid mixture was directly filtered, and the solid product was washed with carbon tetrachloride until the washing liquid became colorless, and a light yellow, powdery solid was obtained. After vacuum drying at room temperature for 24 hours, the mass was 1.595 g, and the product was measured. The melting rate was 76.68%, and its melting point was measured to be 198.2° C. to 201.1° C., and finally it was packaged for use.

Embodiment 2

[0032] Get 1.92g (12mmol) liquid bromine and dissolve in 10mL carbon tetrachloride, be mixed with the solution that mass fraction is 11.1%, 0.816g (2mmol) pentaerythritol tetramethacrylate is added in the above-mentioned configured solution, at 30 It was sealed and refluxed at ℃ for 12 hours. During this experiment, the reddish brown color of bromine gradually became lighter, and solids were formed. After the reaction, the solid-liquid mixture was directly filtered, and the solid product was washed with carbon tetrachloride until the washing liquid became colorless, and a light yellow, powdery solid was obtained. After vacuum drying at room temperature for 24 hours, the weighed mass was 1.680 g, the measured yield was 80.80%, and the measured melting point was 198.3° C. to 200.9° C., and finally packaged for use.

Embodiment 3

[0034] Get 2.56g (16mmol) liquid bromine and be dissolved in 10mL carbon tetrachloride, be mixed with the solution that mass fraction is 14.8%, 0.816g (2mmol) pentaerythritol tetramethacrylate is added in the above-mentioned configured solution, at 30 It was sealed and refluxed at ℃ for 12 hours. During this experiment, the reddish brown color of bromine gradually became lighter, and solids were formed. After the reaction, the solid-liquid mixture was directly filtered, and the solid product was washed with carbon tetrachloride until the washing liquid became colorless, and a light yellow, powdery solid was obtained. After vacuum drying at room temperature for 24 hours, the mass was 1.695 g, measured The yield rate is 81.49%, and its melting point is measured to be 199° C. to 201.8° C., and finally packaged for use.

[0035] Can find out from above three kinds of embodiments, the productive rate of the product that embodiment three obtains is the highest, can reach 81.49%, but...

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Abstract

The invention relates to pentaerythritol tetra(2-methyl-1,2-dibrom acrylic ester) and a method for preparing the same. The technical proposal comprises: according to certain mass ratio, pentaerythritol tetramethyl acrylic ester and liquid bromine are picked up and dissolved in carbon tetrachloride for reaction at a certain temperature for some time, and solid products are filtered, washed and vacuum-dried to obtain light yellow powdery products with melting point of between 198.3 and 200.9 DEG C. The product can initialize the polymerization of majority of monomers with double bond functionalgroup to form various star-shaped polymers.

Description

technical field [0001] The invention relates to a synthesis of pentaerythritol tetrakis(2-methyl-1,2-dibromoacrylate) by using pentaerythritol tetramethylmethacrylate and liquid bromine in a solvent of carbon tetrachloride and a preparation method thereof. Background technique [0002] Pentaerythritol tetraester is an important plasticizer, lubricant and surfactant. It is an important class of fine chemicals. It is often used in the fields of coatings, inks, adhesives, polymers, etc., as crosslinking agents, Rubber and resin modifier, anaerobic adhesive, with high reactivity, high cross-linking density, good hardness, high gloss and so on. Methyl pentaerythritol tetramethacrylate is more used in the synthesis of star-shaped polymers with special structures because of its functional functional groups. But when it is only used as a star-shaped polymer monomer, the degree of polymerization that initiates methyl methacrylate and styrene polymerization is not high, so the presen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/653C07C67/307C08F4/32
Inventor 王云普魏玉丽王冰田震坤申永前张守村
Owner NORTHWEST NORMAL UNIVERSITY
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