Method using glycerol and silicon tetrachloride to prepare epichlorohydrin and white carbon black

A technology of epichlorohydrin and silicon tetrachloride, applied in the directions of silicon oxide, silicon dioxide, organic chemistry, etc., can solve the problems of inhibition and high energy consumption, and achieve the advantages of preventing clogging, improving reaction selectivity and reducing product cost. Effect

Inactive Publication Date: 2012-07-18
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although high-quality white carbon black can be prepared by this process, a large amount of hydrochloric acid is produced as a by-product in the production process, and the energy consumption is high, which inhibits the application of this process

Method used

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  • Method using glycerol and silicon tetrachloride to prepare epichlorohydrin and white carbon black
  • Method using glycerol and silicon tetrachloride to prepare epichlorohydrin and white carbon black

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Example 1. Continuous operation in a tubular reactor

[0039] Dissolve adipic acid (catalyst) in crude glycerol with a glycerin content of 89% (mass ratio) (obtained from the crude glycerol produced by-product of biodiesel production and treated with acid clay, the mass composition is: glycerin 89%, water 7%, 0.8% of salt, 3.2% of others), and a 5% (mass ratio) crude glycerol solution of the catalyst was prepared. Use a metering pump to press the crude glycerol containing the catalyst into a tubular reactor with a total volume of 75L at a rate of 8.0kg / h. The tubular reactor is divided into two parts, the front part and the former. The tube is 24m long), and the reaction temperature is controlled at 80°C; the volume of the latter part of the tubular reactor is 45L (DN40mm tube, 36m long), and the reaction temperature is controlled at 120°C.

[0040] SiCl with a mass content of 96% 4Dissolved in 1,2-dichloroethane to make 40% (mass ratio) SiCl 4 dichloroethane solut...

Embodiment 2

[0046] Embodiment 2. Tank reactor batch operation

[0047] at a volume of 0.25 m 3 Add 70kg of industrial glycerin with a content of 95% (mass ratio) (obtained from biodiesel by-product glycerol through vacuum distillation) into the external circulation reactor, and add 10 kg of glacial acetic acid. Close the feeding port and start the circulation pump.

[0048] 71kg of SiCl with a content of 96% (mass ratio) 4 Dissolved with 34kg N,N-dimethylformamide to make 65% (mass ratio) SiCl 4 Dimethylformamide solution 105kg. Press the SiCl at a rate of 35kg / h through the feed pipe with a metering pump 4 The solution was cooled by jacket water to control the reaction temperature to 90°C for 1 hour. Subsequently, the reaction temperature was controlled to 120° C. to continue the reaction for 2 hours.

[0049] A total of 65% (mass ratio) of SiCl was pumped into 4 DMF solution 105kg, glycerin and SiCl 4 The molar ratio is 1.8:1, the operating pressure is 0.6~1.0MPa, and the tota...

Embodiment 3

[0053] Example 3. Tower reactor continuous operation

[0054] Dissolve phosphotungstic acid in 82% crude glycerin (by-product of biodiesel production) to make 4% catalyst glycerin solution. Use a metering pump to press the catalyst-containing crude glycerin into the tower reactor at a rate of 88 kg / h. The tower reactor consists of two parts connected in series with an external circulation pump, the volume of the first tower is 0.8m 3 , the volume of the second tower is 1.2m 3 .

[0055] SiCl with a mass content of 96% 4 Dissolved with ethylene glycol dimethyl ether to make 25% (mass ratio) SiCl 4 Ethylene glycol dimethyl ether solution. Use a metering pump to mix 25% SiCl 4 The solution is pressed into the above-mentioned tower reactor at a rate of 220kg / h. Glycerin and SiCl 4 The molar ratio is 2.3:1.

[0056] SiCl 4 The solution enters the tower reactor in two distribution ways, one of which is 40% SiCl 4 The solution is sent to the first tower reactor, and the ...

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Abstract

The invention relates to a method using glycerol and silicon tetrachloride to prepare epichlorohydrin and white carbon black, which belongs to the technical field of chemical industrial preparation. The method comprises using biomass glycerol in grease processing byproducts and silicon tetrachloride in polysilicon industry byproducts, hydrolyzing the silicon tetrachloride in a non-proton solvent to obtain silica gel and byproduct hydrochloric acid (HCl), chloridizing the glycerol in the present of a catalyst by the byproduct HCl to achieve glycerol dichloride and byproduct water which is used for hydrolysis of the silicon tetrachloride. The silica gel is thermally treated to obtain the white carbon black, and the glycerol dichloride is saponified to obtain the epichlorohydrin. The white carbon black and the epichlorohydrin can be prepared on the situation without external sources of water and HCl, so that the purposes of saving energy, reducing emission, cleaning production and reducing product cost are achieved. The method uses the non-proton solvent as a reaction medium, thereby improving heat and mass transfer in a coupling reaction process, improving reaction selectivity, preventing generated silica gel from being adhered to equipment and pipelines to block the equipment and the pipelines and enabling reaction to stably run for a long time.

Description

technical field [0001] The invention belongs to the technical field of chemical preparation, and specifically relates to a method for preparing epichlorohydrin and white carbon black by using biomass glycerin by-product of oil processing and silicon tetrachloride by-product of polysilicon industry as raw materials. Background technique [0002] Epichlorohydrin is an important basic chemical, which is widely used in the production of epoxy resins, coatings, surfactants, epichlorohydrin rubber, medicines and pesticides, etc. The global consumption is about 2 million tons. [0003] The traditional industrial production methods of epichlorohydrin include propylene high-temperature chlorination method and propylene acetate method. The former accounts for more than 90% of the world's total production capacity. Its production process requires high energy consumption, dangerous operation, and produces a large amount of difficult-to-treat saline wastewater (40-50 tons of wastewater / t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/02C01B33/12
Inventor 单玉华储海霞侯蓉巫丽君蒋晓丽毛翠霞
Owner CHANGZHOU UNIV
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