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Preparation method of super-crosslinked polymer supported molecular sieve and Fe catalyst and application of super-crosslinked polymer supported molecular sieve and Fe catalyst in production of divinylbenzene

A technology of loading molecules and divinylbenzene, applied in molecular sieve catalysts, including molecular sieve catalysts, carbon compound catalysts, etc., can solve the problems of mismatch between catalytic performance and production demand, product quality, long catalyst induction period, and reduced catalytic efficiency. Excellent pore shape selection function, avoiding high consumption and improving catalytic activity

Active Publication Date: 2021-08-03
JIANGSU EVERGREEN NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in actual production, the catalyst induction period is long, and in the middle and late stages of production, catalytic efficiency reduction and surface coking are prone to occur, and a large amount of water vapor needs to be continuously added during the reaction Catalyst regeneration, resulting in high energy consumption
[0004] The catalytic performance of the existing production process does not match the production requirements and product quality, which has become a development bottleneck and technical barrier for the production of highly selective divinylbenzene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation method of hypercrosslinked polymer-loaded ZSM-5 molecular sieve and Fe catalyst is: in a 50ml two-neck round bottom flask, add 0.9302g of bis-ferrocene, 0.39g of benzene and 0.4948g of 1,2-dichloro Ethane, then add the external crosslinking agent dimethoxymethane FDA, set up a condensing reflux device, continue to stir for 30min, then quickly add 0.8110g anhydrous FeCl3 to the above device to obtain the mixture K, and then heat the mixture K from room temperature React at 45°C for 5h, continue to heat up to 80°C for 19h, and complete the condensation polymerization reaction to form a microporous structure. After the reaction, the product is centrifugally washed with methanol, and vacuum-dried at 60°C for 24h to obtain an iron-based hypercrosslinked polymer. Dissolve the obtained iron-based hypercrosslinked polymer, add 1g of ZSM-5 molecular sieve, stir for 4h, let it stand for 12h, centrifuge dry for 12h, and roast at 500°C for 5h, finally get the hypercr...

Embodiment 2

[0031] Same as Example 1, the reaction temperature is set to 250°C, the space velocity is changed, and the reaction results are shown in Table 2,

[0032] Table 2

[0033] Volumetric space velocity / h -1

Embodiment 3-6

[0035] Same as Example 2, the reaction temperature is set to 250°C, the reaction pressure is changed, and the reaction results are shown in Table 3,

[0036] table 3

[0037] Reaction pressure / MPa Ethylbenzene conversion / % Divinylbenzene selectivity / % Divinyl benzene yield / % 0.1 75.12 90.39 67.90 0.3 74.47 90.28 67.23 0.4 75.39 91.56 69.03 0.5 76.92 90.98 69.98

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Abstract

The invention discloses a preparation method of a hyper-crosslinked polymer loaded molecular sieve and Fe catalyst and application of the hyper-crosslinked polymer loaded molecular sieve and Fe catalyst in production of divinylbenzene. The preparation method comprises the following step of: A1, constructing a reflux condensation device, sequentially adding 0.9302 g of diferrocene, 0.39 g of benzene and 0.4948 g of 1, 2-dichloroethane into a 50ml two-neck round-bottom flask, then adding an external crosslinking agent dimethoxymethane FDA, stirring for 30 minutes, then, rapidly adding 0.8110 g of anhydrous FeCl3 into the device to obtain a mixture K, and heating the mixture to complete condensation polymerization reaction to generate a microporous structure. According to the present invention, the super-crosslinked polymer is adopted as the carrier to load the ZSM-5 molecular sieve and the Fe, the prepared catalyst has high activity and high selectivity on the reaction of catalyzing the synthesis of divinylbenzene from ethylbenzene and diethyl carbonate, the preparation of divinylbenzene from ethylbenzene and diethyl carbonate is performed in a fixed bed reactor, and the whole catalytic reaction has the characteristics of low energy consumption, high selectivity, high activity and the like.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of a hypercrosslinked polymer loaded molecular sieve and an Fe catalyst and its application in the production of divinylbenzene. Background technique [0002] In recent years, with the rapid development of polymer materials, divinylbenzene, as a functional monomer, has been expanding its application fields. The divinylbenzene molecule contains two vinyl groups, forming three isomers: ortho, meta, and para. Refining divinylbenzene, increasing the content of intermediate and para-body in the mixture, and obtaining products with different purity levels have become the main controlling factors of market price. Low-purity divinylbenzene can be directly used as a functional chemical crosslinking agent, widely used in adhesives, professional plastics, and elastomers. Divinylbenzene and styrene are cross-linked and polymerized to produce ion-exchange resi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J29/40B01J31/22C07C2/86C07C15/02C07C5/333C07C15/44
CPCB01J31/06B01J29/40B01J31/2295C07C2/862C07C5/3337C07C2531/06C07C2531/22C07C2529/40B01J2531/842B01J2531/0225B01J2231/766C07C15/02C07C15/44Y02P20/52Y02P20/584
Inventor 孙秋新孙白新沈旭
Owner JIANGSU EVERGREEN NEW MATERIAL TECH
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