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Preparation method of heat-resisting stabilizing agent of bisphenolmonoacryates
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A technology of heat-resistant stabilizers and acrylates, which is applied in the field of preparation of bisphenol monoacrylate heat-resistant stabilizers, and can solve the problems of complex and cumbersome pretreatment process of bisphenol compounds, low yield, and large energy consumption.
Inactive Publication Date: 2013-02-20
SHANXI WANHUA SCI & TECH
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[0005] At present, bisphenol monoacrylate compounds are generally synthesized directly from bisphenol compounds and acryloyl chloride, and the pretreatment process of the raw material bisphenol compounds is complicated and cumbersome; in addition, when the reaction is completed, the crude product needs to be cooled and processed at a lower temperature. Recrystallization, high energy consumption, and low yield
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example 1
[0011] First, 328.4g (2.0mol) of 2-tert-butyl-p-cresol, 75g (1.0mol) of 40% formaldehyde solution, and 3.3g of emulsifier (sodium dodecylsulfonate) are dropped into the bisphenol synthesis kettle, and the Ionized water, start stirring and heat up to 70°C, time the reaction for 3 hours, stop heating and cool to room temperature, adjust the pH value to 7-8, and separate the reaction mixture through a vacuum filter to obtain the intermediate antioxidant 2246; In the second step, put the synthesized intermediate antioxidant 2246 into the esterification reaction kettle, add toluene solvent at the same time, heat and reflux, and remove the water in the bisphenol until no more water is separated. Stop heating, and cool to about 30°C, add 72g (1.0mol) of acrylic acid, 303g (3.0mol) of triethylamine, start stirring, and dropwise add 153g (1.0mol) of phosphorus oxychloride within 30 minutes, start to heat up Reflux, maintain the reaction for 3 hours, cool to room temperature, neutralize...
example 2
[0013] First, 328.4g (2.0mol) of 2-tert-butyl-p-cresol, 75g (1.0mol) of 40% formaldehyde solution, and 3.5g of emulsifier (sodium dodecylbenzenesulfonate) are dropped into the bisphenol synthesis kettle, and Deionized water, start stirring and heat up to 75°C, time the reaction for 4 hours, stop heating and cool to room temperature, adjust the pH value to 7-8, and separate the reaction mixture through a vacuum filter to obtain the intermediate antioxidant 2246; In the second step, put the synthesized intermediate antioxidant 2246 into the esterification reaction kettle, add toluene solvent at the same time, heat to reflux, and remove the water in the bisphenol until no more water is separated. Stop heating, and cool to about 30°C, add 75.6g (1.05mol) of acrylic acid, 303g (3.0mol) of triethylamine and 0.5g of polymerization inhibitor (hydroquinone), start stirring, and add dropwise within 30 minutes Complete 153g (1.0mol) of phosphorus oxychloride, start to heat up and reflux,...
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Abstract
The invention relates to a preparation method of a heat-resisting stabilizing agent of bisphenolmonoacryates. According to the documents, the bisphenolmonoacryates compound is usually directly synthesized by a bisphenols compound and acryloyl chloride at present, wherein the preprocessing of the bisphenols compound of the raw material is complex and troublesome, and the subsequent recrystallization process has complexity, high energy consumption, serious pollution of operation environment, and lower yield. The yield of the heat-resisting stabilizing agent of bisphenolmonoacryates, which is synthesized by using 2-butylhydroxytoluene, paraformaldehyde, crylic acid and phosphorus oxychloride as raw materials and triethylamine as a dehydrochlorination solvent as well as sodium dodecyl sulfonate as an emulsifying agent and methyl alcohol as a refining agent, can reach 80.8 percent. The method has simple process, and achieves the purposes of lowering equipment investment, improving the operation environment, saving energy and reducing consumption, and protecting the environment.
Description
technical field [0001] The invention relates to a preparation method of a bisphenol monoacrylate heat-resistant stabilizer, which is used in the field of capturing polymer carbon free radicals and improving the heat-resistant processing stability of polyolefin and butadiene resins. Background technique [0002] Bisphenol monoacrylate compounds contain two functional groups, unsaturated double bonds and phenolic hydroxyl groups, which can capture carbon radicals through double bonds and undergo intramolecular hydrogen transfer to generate stable phenolic oxygen radicals (i.e., bifunctional stabilization mechanism). The purpose of stabilizing polymers. The chemical name of the bisphenol monoacrylate heat-resistant stabilizer prepared by the present invention is 2-tert-butyl-6-[(3-tert-butyl-2-hydroxyl-5-methylphenyl) methyl-4- Methylphenyl] acrylate is mainly used in synthetic rubbers such as high-impact polystyrene (HIPS), heat-resistant ABS plastics, superplastic elastomer ...
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