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Production method for epichlorohydrin

A technology for epichlorohydrin and a production method, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve pollution, strong equipment corrosion, large amount of waste water and waste, etc. problem, to achieve the effect of good technical effect, high catalyst activity and high product selectivity

Inactive Publication Date: 2016-01-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that there is a large amount of waste water and waste residue in the prior art, serious pollution, and strong corrosion of equipment. A new production method of epichlorohydrin is provided

Method used

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  • Production method for epichlorohydrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] At room temperature and under stirring, 150g of hexadecylamine was added to the solution containing 800ml of H 2 O and 600ml of ethanol mixed solution, stirred until the solution was one phase. Add 650 g of ethyl orthosilicate dissolved in 300 ml of ethanol to the above mixed solution, stir for 30 min and then crystallize for 24 h. The resulting solid was then filtered and washed with water. The washed material was dried at 110°C for 12 hours, and then calcined at 550°C for 4 hours to obtain a powder carrier with HMS structure characteristics. Using silica sol as a binder, a HMS molding carrier with a HMS weight percentage of 90% was prepared by using traditional extrusion molding technology.

[0036] Configuration contains 40gTiCl 4 500ml of cumene solution, the above-mentioned prepared catalyst shaped carrier is added to TiCl 4 In the solution, under slow stirring and reflux, the temperature was raised to 150°C, and the reaction was carried out at this temperature...

Embodiment 2

[0040] According to the method of [Example 1], an HMS shaped carrier with a HMS weight percentage of 90% was prepared. Take 100 grams of the shaped carrier prepared above and fill it into a quartz tube reactor, and heat it at 120° C. for 2 hours under dry air conditions. Raise the bed temperature to 200°C, under normal pressure, continuously feed TiCl 4 Dry air at 5.0% by volume for 6 hours. At this temperature and pressure, switch to air purge until the reactor outlet is TiCl-free 4 Check out. Then pass air with a water vapor volume content of 1.0% for 5 hours, and then switch to air to purge the residual water vapor in the system. Dry air with a hexamethyldisilazane volume content of 10.0% was continued for 6 hours. At this temperature and pressure, switch to nitrogen purge until no hexamethyldisilazane is detected at the outlet of the reactor, that is, a titanium-containing porous silica catalyst Ti- HMS.

[0041] The elemental analysis results showed that the weight ...

Embodiment 3

[0043] Add 150 g of fumed silica into 240 g of 25 wt % tetramethylammonium hydroxide aqueous solution, and continue stirring for 30 min to form a solution. Then, the above solution was added to 600 ml of aqueous solution containing 230 g of cetyltrimethylammonium bromide under stirring to form a transparent solution. The above mixed solution was transferred into a stainless steel autoclave lined with polytetrafluoroethylene at 100°C for static crystallization for 3 days. The crystallized product is washed and filtered, dried at 100°C for 24 hours, and calcined at 550°C for 6 hours to obtain a powder carrier with the structural characteristics of MCM-41. The MCM-41 molding carrier with the MCM-41 weight percentage of 90% is prepared by using silica sol as a binder and adopting traditional extrusion molding technology.

[0044] According to the method of [Example 2], the assembly of the active species titanium and the surface hydrocarbyl graft silanization treatment are carried...

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Abstract

The invention relates to a production method for epichlorohydrin. The method mainly solves the problems of large amounts of waste water and waste residues, serious pollution and strong corrosiveness to equipment in the prior art. A technical scheme of the invention adopts the production method which comprises the following steps: with chloropropene and ethylbenzene hydroperoxide as raw materials and ethylbenzene as a solvent, subjecting the raw materials and a titanium-contained porous silicon dioxide catalyst to contact reaction so as to obtain epichlorohydrin and alpha-methylbenzyl alcohol under the conditions that reaction temperature is 25 to 200 DEG C; reaction absolute pressure is 0.1 to 8.0 MPa; a molar ratio of chloropropene to ethylbenzene hydroperoxide is 1 to 15; and weight-space velocity of ethylbenzene hydroperoxide is 0.01 to 20 h<-1>. Thus, the problem is well solved, and the method can be applied in industrial production of epichlorohydrin.

Description

technical field [0001] The invention relates to a production method of epichlorohydrin. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical product with a wide range of uses. The epoxy resin prepared from it has the characteristics of strong adhesion, chemical corrosion resistance, low shrinkage, good chemical stability, high impact strength and excellent dielectric properties. It is used in coatings, adhesives, reinforcing materials, casting Industries such as materials and electronic laminates have a wide range of applications. In addition, epichlorohydrin can also be used to synthesize glycerin, nitroglycerin explosives, glass fiber reinforced plastics, electrical insulation products, surfactants, medicines, pesticides, coatings, rubber materials, ion exchange resins, plasticizers, (glycidin) derivatives , Chlorohydrin rubber and other products. [0003] The traditional production methods of epichlorohydrin main...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/19B01J31/02
Inventor 金国杰康陈军高焕新杨洪云黄政丁琳
Owner CHINA PETROLEUM & CHEM CORP
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