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Allyl chloride oxidation method

A technology of chloropropene and oxidant, which is applied in chemical instruments and methods, organic chemistry, molecular sieve catalysts, etc. It can solve problems such as reactor shutdown, equipment corrosion, and increase in device operating costs, so as to reduce regeneration frequency, prolong service life, and prolong The effect of one-way service life

Active Publication Date: 2017-07-21
CHINA PETROLEUM & CHEM CORP +1
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  • 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
However, with the prolongation of the reaction time, the catalytic activity of titanium-silicon molecular sieves will show a downward trend, resulting in a significant decrease in the selectivity of the target oxidation product.
When the reaction is carried out in a fixed-bed reactor, due to the reduction of the catalytic activity of the titanium-silicon molecular sieve, the titanium-silicon molecular sieve needs to be regenerated inside or outside the reactor, resulting in shutdown of the reactor, thereby affecting production efficiency and increasing the operating cost of the device

Method used

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Examples

Experimental program
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Effect test

Embodiment approach

[0068] According to the method of the present invention, the amounts (mass) of the titanium-silicon molecular sieves loaded in the first to nth catalyst beds may be the same or different. According to one implementation, when m is any integer in the interval [2, n], W m-1 / W m 0.1-20, W m-1 / W m Preferably it is 0.5 or more, More preferably, it is 1 or more, More preferably, it is 2 or more. Here, W m-1 is the quality of the catalyst packed in the upstream catalyst bed in any pair of adjacent catalyst beds from the first catalyst bed to the last nth catalyst bed, W m is the mass of the catalyst loaded in the downstream catalyst bed in any pair of adjacent catalyst beds from the first catalyst bed to the nth catalyst bed. W m-1 / W m Preferably it is 15 or less, and more preferably 10 or less. More preferably, W m-1 / W m for 2-8. W m-1 and W m It is determined by the content of the titanium-silicon molecular sieve in the shaped titanium-silicon molecular sieve. In ...

Embodiment 1

[0097] The catalyst used in this example is titanium-silicon molecular sieve TS-1, prepared according to the method described in Zeolites, 1992, Vol.12, pages 943-950, and the specific method is as follows.

[0098] At room temperature (20°C), mix 22.5g tetraethyl orthosilicate with 7.0g tetrapropylammonium hydroxide as a template, add 59.8g distilled water, stir and mix, then hydrolyze at normal pressure and 60°C for 1.0h , to obtain a hydrolysis solution of tetraethyl orthosilicate. Under vigorous stirring, a solution consisting of 1.1 g of tetrabutyl titanate and 5.0 g of anhydrous isopropanol was slowly added to the hydrolysis solution, and the resulting mixture was stirred at 75° C. for 3 h to obtain a clear transparent colloid. The colloid was placed in a sealed stainless steel reaction kettle, and kept at a constant temperature of 170° C. for 36 hours to obtain a mixture of crystallized products. The obtained mixture was filtered, the collected solid matter was washed ...

Embodiment 2

[0104] Propylene chloride was oxidized by the same method as in Example 1, except that the titanium-silicon molecular sieve TS-1 used was prepared by the following method.

[0105] Dissolve tetrabutyl titanate in the alkali source template agent tetrapropyl ammonium hydroxide aqueous solution first, then add silica gel (purchased from Qingdao Silica Gel Factory) to obtain a dispersion. In the dispersion, silicon source: titanium source: alkali source Template agent: water molar ratio is 100:4:12:400, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of alkali source template agent in N. Seal the above dispersion in the beaker with a parafilm and let it stand at room temperature (25°C, the same below) for 24h, then stir at 35°C for 2h with magnetic stirring to redisperse it. Transfer the re-dispersed dispersion liquid to a sealed reaction kettle, undergo the first stage of crystallization at 140°C for 6h, then cool the mixture down to 30°C and experience t...

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Abstract

The present invention discloses an allyl chloride oxidation method, which comprises that a reaction material containing allyl chloride, an oxidizing agent and a solvent sequentially flows through catalyst bed layers from 1 to n under an oxidation reaction condition, wherein n is an integer of more than 2, and the catalyst bed layer is filled with at least a titanium-silicon molecular sieve; and when the reaction material passes through the catalyst bed layers from 1 to n, at least a flow carrier is introduced into the position between at least a pair of the adjacent catalyst bed layers among the catalyst bed layers from 1 to n, such that the apparent velocity of the reaction stream positioned in the downstream catalyst bed layer is higher than the apparent velocity of the reaction stream positioned in the upstream catalyst bed layer in the pair of the adjacent catalyst bed layers by adopting the flowing direction of the reaction material as the reference. With the method of the present invention, the one-way service life of the titanium-silicon molecular sieve can be effectively prolonged, the effective utilization rate of the oxidizing agent can be improved, and the target product selectivity can be improved.

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. 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 other prope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D301/14C07D301/19C07D303/08B01J29/89
CPCB01J29/89B01J2229/10C07D301/12C07D301/14C07D301/19C07D303/08
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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