Background and overview[1]
Ethylene glycol phenyl ether acetate is an ester compound that can be used as an intermediate for pharmaceutical and chemical synthesis.
Structure
Apply[1-4]
1) Used to synthesize compounds containing 4-(2-hydroxyethoxy)benzophenone structure or its acetate.
It includes the following steps:
a. Dissolve ethylene glycol phenyl ether acetate (compound 2) in an organic solvent under the catalysis of a Lewis acid catalyst, and then add R substituent benzoyl chloride (compound 2) dropwise at 0 to 20°C under stirring conditions. Compound 1), then react at room temperature for 1-5 hours until the reaction is complete, add ice water to stir, and separate the aqueous phase and the organic phase; the molar ratio of the ethylene glycol phenyl ether acetate and the R substituent benzoyl chloride is 1:1.0 ~1.2; the molar ratio of ethylene glycol phenyl ether acetate and Lewis acid catalyst is 1:1.05~3;
b. Remove the solvent from the organic phase obtained in step a to obtain the acetate ester (compound 3) containing 4-(2-hydroxyethoxy)benzophenone structure; or, use the organic phase obtained in step a to Add an alcohol solvent and perform a hydrolysis reaction under the catalysis of acid or alkali to precipitate a solid. The solid obtained after filtration is a compound containing a 4-(2-hydroxyethoxy)benzophenone structure (compound 4);
2) Used to prepare 2-hydroxy-1-{4-(2-hydroxyethoxy)phenyl}-2-methyl-1-propanone.
It is a UV curing initiator. It is the only photoinitiator allowed by the FDA certification system. It can be used in adhesives that are not in direct contact with food. It has low odor, low volatility, low yellowing, and has active hydroxyethyl alcohol. The oxygen-terminated hydroxyl group can participate in the reaction. It can be used in water-based light-curing systems with high melting points, and can also be used in UV-curing powder coatings.
The preparation method is: using ethylene glycol phenyl ether acetate as raw material, and conducting Friedel-Crafts reaction with isobutyryl chloride with a molar ratio of 1 to 1.2 times the equivalent under the catalysis of Lewis acid. The reaction temperature is -5°C~ 5℃, the reaction time is 3~6 hours; bromination reaction is carried out under the catalysis of N, N-dimethylformamide or iodine; the bromination product is catalytically hydrolyzed using a phase transfer catalyst at room temperature; finally it is prepared by purification and crystallization product. In the present invention, dichloromethane or dichloroethane is used as a solvent during the bromination process, and acetic acid is no longer used. The reaction occurs under the catalysis of DMF or I2, thereby greatly shortening the reaction time. Introducing a phase transfer catalyst during the hydrolysis process allows the brominated intermediate product to react directly with alkali in water, avoiding the use of a large amount of ethanol as a solvent, simplifying the process, reducing production costs, and increasing yield.
3) Prepare a power cord for electronic equipment with good flame retardant performance.
It is characterized in that it consists of the following components by weight: 40-80 parts of EPDM rubber, 12-18 parts of water-based polyurethane resin, 2-8 parts of ethylene glycol phenyl ether acetate, and silicone resin microspheres 3-7 parts, ultrafine activated carbon 5-8 parts, titanium dioxide 2-6 parts, zinc borate 3-7 parts, polyethylene wax 2-7 parts, boehmite powder 1-3 parts, calcium hydroxide 1-5 parts, 2-6 parts of polyethylene wax, 1-4 parts of antioxidant DMTDP, 3-7 parts of flame retardant particles. The oxygen index of the power cord produced by the invention is as high asMore than 37%, it has good flame retardancy and antibacterial properties. At the same time, the tensile strength of the sheath material is as high as 19.8MPa, which meets the application needs and user experience, and protects the safety performance of users when using electronic equipment.
4) Prepare a polyphenylene ether material for the outer sheath of power cords in humid environments.
It is made of the following raw materials by weight: polyphenylene ether-31-46, polyparaben-23-37, polyvinylcarbazole-18-29, hexachlorocyclotriphosphazene- 8-12. Silicone resin microspheres-5-10, p-chlorom-xylenol-2-4, dihydroxyaluminum stearate-3-6, nickel slag powder-15-20, hexadecyl bromide Pyridine 10-15, 2-nitrobiphenyl-2-4, jojoba oil-3-6, ethylene glycol phenyl ether acetate-5-10, sodium tungstate 4-7, barium myristate 2- 3. Barium laurate 1-2, calcined andalusite micro powder – 15-20, flame retardant particles – 10-15. The outer sheath material prepared by the invention has excellent water resistance, moisture resistance, mildew resistance, corrosion resistance, flame retardancy, aging resistance and mechanical properties, and fully meets the use requirements in humid environments.
Main reference materials
[1] CN201310712555.4 Synthetic method of compound containing 4-(2-hydroxyethoxy)benzophenone structure or its acetate ester
[2] CN201010167255.9 A preparation method of 2-hydroxy-1-{4-(2-hydroxyethoxy)phenyl}-2-methyl-1-propanone
[3] CN201810446999.0 A power cord for electronic equipment with good flame retardant performance
[4] CN201510534985.0 A polyphenylene ether material used for the outer sheath of power cords in humid environments and its preparation method
