Preparation method of 2,4-dichlorobenzoyl peroxide_Kain Industrial Additive

Background and overview^[1]

It is well known that diacyl peroxides can be produced by reacting acid chlorides and hydrogen peroxide in alkaline solutions, but it is difficult to produce powdered products and has problems such as low content and low yield. The preparation method of 2.4-dichlorobenzoyl peroxide (DCPB for short) is to prepare paste DCPB, such as the method described in USP4151106, which requires complex equipment, is inconvenient to operate and cannot obtain high-purity products.

Preparation^[1]

The manufacturing method of 2.4-dichlorobenzoyl peroxide is characterized by including the following steps in sequence:

(1) Mix NaOH aqueous solution and hydrogen peroxide to prepare sodium peroxide aqueous solution. The mass concentration of the sodium peroxide aqueous solution is 5 to 10%;

(2) Add the dispersant to the sodium peroxide solution and stir evenly. The dispersant is an aqueous solution of gelatin or PVA (polyvinyl alcohol) with a mass concentration of 5 to 10%. The dispersant occupies the aqueous phase solution. (sodium peroxide aqueous solution + dispersant) 0.1 to 1% of the total mass;

(3) Mix acid chloride (2,4-dichlorobenzoyl chloride) and an alkane solvent to prepare an acid chloride solution, in which the acid chloride accounts for 80 to 85% of the total mass of the acid chloride solution;

(4) Under stirring, slowly drop the prepared acid chloride solution into the sodium peroxide solution with dispersant for reaction (acyl chloride and sodium peroxide can be measured according to the reaction molar ratio), and the temperature is controlled at 10~ 40°C, add the acid chloride within 40 minutes to 2 hours, then stir for another 30 minutes to end the reaction;

(5) After the reaction is completed, stop stirring and extract the reaction mother liquor. The product is washed once with 30°C hot water, then washed 2 to 3 times with desalted water, and finally dehydrated and dried to obtain a powdered product. The alkane solvent is preferably isododecane, mineral spirits or silicone oil.

Apply^[2-5]

Examples of application of 2.4-dichlorobenzoyl peroxide are as follows:

1) Prepare a low-voltage power cable rubber material. The raw materials include: 55-65 parts by weight of EPDM rubber, 20-35 parts of silicone rubber, 10-15 parts of chlorosulfonated polyethylene, oxidized 3-5 parts of zinc, 0.8-1.2 parts of stearic acid, 8-13 parts of metallocene elastomer, 15-20 parts of organic montmorillonite, 20-35 parts of thermal carbon black, 5-10 parts of zinc methacrylate , 2-3 parts of 2,4-dichlorobenzoyl peroxide, 2-4 parts of vulcanizing agent DCP-0.5-1.3 parts of anti-aging agent MC, active cross-linking assistant N,N’-bisfurnylene acetone 0.2-0.6 parts, polyisobutylene 15-20 parts, red phosphorus 1-3 parts, magnesium hydroxide 0.5-1.5 parts, accelerator CZ-0.8-1.3 parts. The low-voltage power cable rubber material proposed by the present invention has excellent heat aging resistance, and at the same time, the mechanical strength and flame retardancy are also improved.

2) Prepare an adhesive, which includes the following components by weight: 25 parts of epoxy-modified hydroxyacrylic resin, and 25 parts of thermoplastic acrylic resin with a weight average molecular weight of about 70,000-75,000 , 20 parts of silicone modified acrylic resin, 10 parts of 6-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline, 10 parts of melamine resin, 7 parts of phenyltrichlorosilane, 10 parts of 2,4-dichlorobenzoyl peroxide, 5 parts of vinyltrimethoxysilane, 7 parts of titanium dioxide, 5 parts of attapulgite powder, 5 parts of dichlorotetrafluoroethane, 20 parts of ethylene glycol monobutyl ether parts; the above components are prepared by mixing and stirring. The adhesive of the present invention not only improves the temperature adaptability range, but also significantly improves the shear strength.

3) Prepare a high-performance fluororubber composite material, whose raw materials include: fluororubber, methylvinylphenyl silicone rubber, ethylene acrylate rubber, polyvinylidene fluoride, polycaprolactone, compatibilizer, 2,4-Dichlorobenzoyl peroxide, tert-butyl peroxybenzoate, triallyl cyanurate, zinc oxide, stearic acid, calcium hydroxide, fumed silica, graphene, diatoms Soil, boron nitride, molybdenum disulfide, hydroxyl silicone oil, antioxidant, accelerator, silane coupling agent. The high-performance fluororubber composite material proposed by the invention has good heat resistance, aging resistance, low temperature resistance and oil resistance, excellent processing performance and long service life.

4) Prepare an oil-resistant and flame-retardant cable for oil platforms, including a cable core and a sheath. The sheath is made of modified nitrile rubber composite material. The raw materials of nitrile rubber composite material include: nitrile rubber, ternary rubber Ethylene propylene rubber, ethylene vinyl acetate, chlorinated polyethylene, stearic acid, zinc oxide, p-tert-butylphenol formaldehyde resin, 2,4-dichlorobenzoyl peroxide, trimethylolpropane trimethyl Acrylate, silicon-aluminum carbon black, nano-silica, wollastonite, nano-zinc stannate, melamine phosphate, 6-chloro-N,N-diethyl-1,3,5-triazine-2,4 -Diamine, phosphorus silicon nitrogen flame retardant, diglycol distearate, 2-deoxy-2,2difluoro-pentofuranose-1-one-3,5-dibenzoate, anti-aging Agent, accelerator, silane coupling agent. The oil-resistant and flame-retardant cable for oil platforms proposed by the invention has excellent mechanical properties, good aging resistance and low-temperature resistance, and excellent flame-retardant and oil-resistant properties.

Main reference materials

[1] CN200910015117.62.4-Method for manufacturing dichlorobenzoyl peroxide

[2] CN201410719582.9 Preparation method of adhesive

[3] CN201410424604.9 A low-voltage power cable rubber material

[4] CN201510895017.2 A high-performance fluorine rubber composite material

[5] CN201610278227.1 An oil-resistant and flame-retardant cable dedicated to oil platforms