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A kind of catalyst with phosphorus modified ZSM-5 molecular sieve as carrier and its preparation method and application

A ZSM-5, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low selectivity of a single product, high selectivity synthesis of isobutene with methyl bromide, etc. The method is simple, the reaction conditions are mild, and the product selectivity is high.

Active Publication Date: 2018-10-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the technology with higher value-added low-carbon olefins as the target product, the selectivity of a single product is not high, and no relevant reports have been found on the synthesis of isobutene with high selectivity from methyl bromide

Method used

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  • A kind of catalyst with phosphorus modified ZSM-5 molecular sieve as carrier and its preparation method and application

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Effect test

Embodiment 1

[0029] Weigh an appropriate amount of hydrogen-type ZSM-5 molecular sieve (silicon-aluminum ratio 50) and place it in a certain concentration of ammonium dihydrogen phosphate aqueous solution, ultrasonically treat it for 40 minutes, then heat and stir in a water bath at 50°C for 3 hours, and let it stand for 12 hours. ℃ drying for 15 hours, and then roasting at 550 ℃ for 4 hours to obtain the phosphorus-modified ZSM-5 molecular sieve, which is denoted as 1P-ZSM-5.

[0030] Weigh an appropriate amount of zinc nitrate, zirconium nitrate, and ammonium dihydrogen phosphate, dissolve them in deionized water, and load them on 1P-ZSM-5 molecular sieve (pore volume: 0.42ml / g, specific surface area: 393m 2 / g, strip shape, equivalent diameter 1.5mm), dried at 80°C for 8h, and calcined at 600°C for 4h to prepare the catalyst precursor ZnO-Zr-P / 1P-ZSM-5. Put 5g of the catalyst precursor in a continuous flow fixed-bed reactor, and use methyl bromide to treat the catalyst precursor at 250°...

Embodiment 2

[0033] Weigh an appropriate amount of hydrogen-type ZSM-5 molecular sieve (silicon-aluminum ratio 100) and place it in a certain concentration of ammonium dihydrogen phosphate aqueous solution, ultrasonically treat it for 40 minutes, then heat and stir in a water bath at 60°C for 2 hours, and let it stand for 12 hours. ℃ drying for 12 hours, and then roasting at 550 ℃ for 4 hours to obtain phosphorus-modified ZSM-5 molecular sieve, which is denoted as 3P-ZSM-5.

[0034] Weigh an appropriate amount of zinc nitrate, zirconium nitrate, and ammonium dihydrogen phosphate, dissolve them in deionized water, and load them on 3P-ZSM-5 molecular sieves (the pore volume is 0.63ml / g, and the specific surface area is 427m 2 / g, strip shape, equivalent diameter 1.5mm), dried at 120°C for 4h, and calcined at 500°C for 8h to prepare the catalyst precursor ZnO-Zr-P / 3P-ZSM-5. Put 5g of the catalyst precursor in a continuous flow fixed-bed reactor, and use a mixed gas of methyl bromide and nitro...

Embodiment 3

[0037] Weigh an appropriate amount of hydrogen-type ZSM-5 molecular sieve (silicon-aluminum ratio 150) and place it in a certain concentration of ammonium dihydrogen phosphate aqueous solution, ultrasonically treat it for 40 minutes, then heat and stir in a water bath at 70°C for 1 hour, and let it stand for 12 hours. ℃ drying for 8 hours, and then roasting at 550 ℃ for 4 hours to obtain the phosphorus-modified ZSM-5 molecular sieve, which is denoted as 5P-ZSM-5.

[0038] Weigh an appropriate amount of zinc nitrate, zirconium nitrate, and ammonium dihydrogen phosphate, dissolve them in deionized water, and load them on 5P-ZSM-5 molecular sieves (the pore volume is 0.56ml / g, and the specific surface area is 441m 2 / g, strip shape, equivalent diameter 1.5mm), dried in vacuum at 100°C for 8h, and calcined at 400°C for 8h to prepare the catalyst precursor ZnO-Zr / 5P-ZSM-5. Put 5g of the catalyst precursor in a continuous flow fixed-bed reactor, use a mixed gas of methyl bromide and...

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Abstract

The invention discloses a catalyst taking a phosphorus-modified ZSM-5 molecular sieve as a carrier as well as a preparation method and an application of the catalyst. The catalyst is prepared from zinc oxide, zinc bromide and a phosphorus-modified hydrogen-form ZSM-5 molecular sieve carrier. The preparation method of the catalyst comprises steps as follows: (1) the hydrogen-form ZSM-5 molecular sieve is soaked and treated with a phosphorus-containing solution, and the phosphorus-modified hydrogen-form ZSM-5 molecular sieve carrier is obtained; (2) zinc oxide and / or an auxiliary oxide are / is introduced into the phosphorus-modified hydrogen-form ZSM-5 molecular sieve carrier; (3) bromination treatment is performed on the phosphorus-modified hydrogen-form ZSM-5 molecular sieve carrier with zinc oxide introduced. The catalyst is used for preparing isobutene from methyl bromide, and the selectivity of isobutene can be remarkably improved.

Description

technical field [0001] The invention relates to a catalyst with phosphorus-modified ZSM-5 molecular sieve as a carrier, a preparation method and application thereof. Background technique [0002] Isobutene is an important basic organic chemical raw material. Its derivative products are numerous, the upstream and downstream industrial chains are complicated, and the consumption structure shows a trend of diversification. A variety of high value-added products can be prepared from isobutylene, such as: butyl rubber, polyisobutylene, methyl tert-butyl ether, isoprene and organic glass and other organic chemical raw materials and fine chemical products. As the market scale of isobutene downstream products continues to expand, the contradiction between supply and demand will gradually become prominent, especially in the context of the depletion of oil resources, the output of isobutene has become a key bottleneck restricting the development of downstream industries. Therefore, i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40C07C11/09C07C1/26
Inventor 孙晓丹张舒冬张信伟李杰倪向前张喜文刘继华
Owner CHINA PETROLEUM & CHEM CORP
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