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Method of preparing and separating epichlorohydrin by chloropropene epoxidation

An epichlorohydrin and chloropropene technology, applied in chemical instruments and methods, organic chemistry, chemical recycling, etc., can solve the problems of complex regeneration, permanent deactivation, long process flow, etc., and achieve simplified process and process flow, Inhibition of side reaction products, reasonable effect of process route

Active Publication Date: 2007-08-15
BALING PETRO CHEM CO LTD SINOPEC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The third is that titanium-silicon molecular sieves are easy to deactivate and complex to regenerate
prone to permanent inactivation
[0008] The high-temperature chlorination of propylene in the existing epichlorohydrin (ECH) production process has high chlorine consumption, high material consumption, and large energy consumption; serious equipment corrosion and high maintenance costs; a large amount of chlorine-containing waste water (every production 1 1 ton of ECH produces about 50 to 60 tons of waste water)
However, the material consumption, energy consumption, amount of by-products and waste water of the propylene acetate method have all decreased, but the process is longer, and the corrosion of equipment and the discharge of waste water are still relatively serious.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]Embodiment 1: 5 grams of allyl chloride (ALC) with a content of 98% in 500 grams, 170 grams of 50% hydrogen peroxide and 5 grams of promoter alkylphenol polyoxyethylene ether (OP) are dropped into a 1000 milliliter three-necked bottle, and 40 Gram catalyst phosphotungstic acid (three) hexadecylpyridine, and slowly warming up to 40 ℃ to stop heating, react under reflux state, after 60 minutes, the still temperature reaches 55 ℃, reflux stops, at this moment, the still liquid is cooled to 5 Below ℃, stand still, separate the liquid and solid, and the solid catalyst can continue to be used for the reaction. The liquid is layered in the separatory funnel, the upper layer is water, the lower layer is a mixture of epichlorohydrin and chloropropene (oil phase), the water is sampled and discarded, and the oil phase is collected and analyzed by gas chromatography. The composition of the oil phase is: ALC56. 2%, ECH42.2%, by-product 1.6%, the water phase contains ALC0.29%, ECH2.5%...

Embodiment 2

[0029] Embodiment 2: Allyl chloride, hydrogen peroxide, and catalyst promoter were added according to Embodiment 1, and the catalyst was recovered in Embodiment 1. The reaction was 90 minutes, and the selectivity of epichlorohydrin was 99.6%.

Embodiment 3

[0030] Embodiment 3: The formula is the same as that of Embodiment 1, the catalyst is recovered and reused from the vacuum distillation epichlorohydrin tower kettle, and the reaction is 100 minutes, and the epichlorohydrin selectivity is 98.8%.

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PUM

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Abstract

The invention discloses an epoxidizing method of epoxy chloropropane through chloropropene, which comprises the following steps: adopting excessive chloropropene to produce epoxy chloropropane directly under phosphotungstic acid quaternaries as catalyst and alkyl phenol polyoxyethylene ester as adjuvant catalyst and hydrogen peroxide solution as oxidant to reflux; cooling reactant; recycling solid-phased catalyst; distilling oil phase of reacting liquid to recycle residual chloropropene; decompressing; distilling; obtaining the purified product.

Description

technical field [0001] The invention relates to a process for preparing, separating and purifying epichlorohydrin by using allyl chloride. Background technique [0002] The current production of epichlorohydrin is mainly based on the chlorohydrin method, but due to the large amount of sewage discharge in this process, it causes great pollution to the environment, high material consumption and high energy consumption in the process, so that the production cost of the product is too high. Therefore, all countries are researching environmentally friendly processes that can replace traditional processes. [0003] There are various processes currently being explored, but the most notable ones are only the titanium-silicon molecular sieve method and the phosphotungstic acid heteropolyacid method. Titanium silicon molecular sieve method has been done a lot of research at home and abroad, but there is no report of industrialization so far. [0004] In 1983, Venturello reported tha...

Claims

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Application Information

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IPC IPC(8): C07D301/12C07D303/08B01J31/02
CPCY02P20/584
Inventor 冯利民夏金魁刘彬熊远凡何思列邢质军李娟
Owner BALING PETRO CHEM CO LTD SINOPEC
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