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A kind of chloropropene oxidation method

A technology of chloropropene and oxidant, applied in organic chemistry and other directions, can solve the problems of many by-products, large production energy consumption, affecting product refining and separation, etc., to achieve stable oxidant conversion rate, prolong single-pass service life, and be suitable for large-scale application. Effect

Active Publication Date: 2018-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Propylene high-temperature chlorination method (also known as chloropropene method) is a classic method for producing epichlorohydrin. The main problems in this process are: serious corrosion of equipment, high energy consumption for production, high chlorine consumption, many by-products, and A large amount of wastewater containing calcium chloride and organic chloride seriously endangers the environment, and the investment in wastewater treatment accounts for about 20% of the total investment
[0006] When titanium-silicon molecular sieves are used as catalysts to oxidize chloropropene, the common problem is that with the prolongation of the reaction time, the catalytic activity of titanium-silicon molecular sieves will show a downward trend, resulting in a decrease in the conversion rate of the oxidant and the selectivity of the target oxidation product.
[0008] However, when the regenerated catalyst is put into operation again, especially after being regenerated in the device, the activity and selectivity of the catalyst fluctuate greatly, and it takes a long time to stabilize; at the same time, it is necessary to combine operations such as increasing the reaction temperature To achieve the smooth operation of the reaction, but this will further accelerate the deactivation of the catalyst and reduce the selectivity of the target oxidation product, affecting the refining and separation of subsequent products, and is also not conducive to safe production

Method used

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  • A kind of chloropropene oxidation method
  • A kind of chloropropene oxidation method
  • A kind of chloropropene oxidation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The reaction is carried out in two miniature fixed-bed reactors connected in series, wherein each reactor is filled with a catalyst bed with a circular cross-section and an equal diameter. Based on the flow direction of the liquid material, the first upstream The ratio of the inner diameter of the first catalyst bed in the first reactor to the inner diameter of the second catalyst bed in the downstream second reactor is 2:1, and the first catalyst bed is filled with a hollow titanium-silicon molecular sieve ( A spherical catalyst with a volume average particle size of 500 μm and a catalyst density of 0.70 g / cm 3 ), the second catalyst bed is filled with titanium-silicon molecular sieve TS-1 (a spherical catalyst with a volume average particle diameter of 500 μm and a density of 0.76 g / cm 3 ), the weight ratio of hollow titanium-silicon molecular sieve to titanium-silicon molecular sieve TS-1 is 2:1.

[0075] Allyl chloride, hydrogen peroxide (provided in the form of 30...

Embodiment 2

[0089] Adopt the same method as embodiment 1 to oxidize chloropropene, the difference is that the molding titanium-silicon molecular sieve TS-1 in the second catalyst bed uses the same amount of molding titanium-silicon molecular sieve Ti-MCM-41 (volume average particle diameter is 500 μm A spherical catalyst with a density of 0.61g / cm 3 )replace.

[0090] The results are listed in Table 1 for reaction times of 2 hours, 360 hours and 720 hours.

Embodiment 3

[0092] Adopt the same method oxidation chloropropene as embodiment 1, difference is, the molding titanium-silicon molecular sieve TS-1 in the second catalyst bed layer in the second reactor uses the same amount of molding titanium-silicon molecular sieve Ti-Beta (volume Spherical catalyst with an average particle size of 500 μm and a density of 0.77 g / cm 3 )replace.

[0093] The results are listed in Table 1 for reaction times of 2 hours, 360 hours and 720 hours.

[0094] Table 1

[0095]

[0096] Comparing the data of Example 1 with Comparative Examples 1-3, it can be seen that when the hollow titanium-silicon molecular sieve is used in combination with the titanium-silicon molecular sieve, and the hollow titanium-silicon molecular sieve is located upstream of the titanium-silicon molecular sieve, the liquid mixture flows through the hollow The superficial velocity of the titanium-silicon molecular sieve is lower than the superficial velocity of the titanium-silicon mole...

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Abstract

The invention provides a method for oxidizing allyl chloride, the method comprising: under oxidation reaction conditions, making a liquid mixture containing allyl chloride and an oxidizing agent flow through a catalyst bed; the catalyst bed includes a first catalyst bed and a second catalyst bed. The catalyst bed is based on the flow direction of the liquid mixture, the first catalyst bed is located upstream of the second catalyst bed, and the titanium-silicon molecular sieve packed in the first catalyst bed is a hollow titanium-silicon molecular sieve; The titanium-silicon molecular sieve packed in the second catalyst bed is a titanium-silicon molecular sieve different from the hollow titanium-silicon molecular sieve. By adopting the method for oxidizing chloropropene of the present invention, a relatively stable oxidant conversion rate and a relatively high selectivity of target oxidation products can be obtained during long-term continuous operation. In particular, by adopting the method of the present invention, the selectivity of epoxides is high, thereby reducing the difficulty of subsequent separation and purification.

Description

technical field [0001] The invention relates to a method for oxidizing propylene chloride. Background technique [0002] Epichlorohydrin (Epichlorohydrin, abbreviated as ECH), also known as 1-chloro-2,3-epoxypropane, commonly known as epichlorohydrin. There are epoxy groups and active chlorine in the ECH molecule, which is chemically active. The epoxy resin made from ECH has the characteristics of strong adhesion, corrosion resistance to chemical media, low shrinkage, good chemical stability, and high impact strength. [0003] Epichlorohydrin is an important and widely used organic chemical raw material and fine chemical product. Synthetic glycerin produced by hydrolysis of ECH is widely used in alkyd resin, medicine, tobacco, food and explosives industries; chlorohydrin produced by homopolymerization of ECH or dimerization and trimerization with ethylene oxide and propylene oxide Rubber, with heat resistance, oil resistance, ozone resistance, weathering resistance and ot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/08C07D303/04C07D301/12
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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