A kind of sulfonated zirconium phosphonate solid strong acid porous material and its preparation method

A technology of sulfonated zirconium phosphonate and porous materials, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as high heat resistance temperature, loss of sulfonic acid groups, deactivation, etc. , to achieve high mechanical stability, high hydrothermal stability, and good acid catalytic performance

Active Publication Date: 2017-01-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cationic exchange resin catalyst, as an industrialized macroporous solid acid catalyst, has been widely used in organic catalytic reactions such as etherification, alkylation, and polymerization. However, the operating temperature of resin catalysts is generally below 120°C. When the reaction temperature reaches At 140-150°C, it is easy to lose the sulfonic acid group and deactivate, which limits the application range of the resin catalyst
Another type of solid acid catalyst that is widely industrialized is microporous molecular sieve, which is widely used in high temperature reactions such as petroleum catalytic cracking because of its high heat resistance temperature, but its catalytic activity is not ideal for medium and low temperature reactions (room temperature-200°C).
In order to improve the catalytic activity of microporous molecular sieves at medium and low temperatures, it is generally used as a carrier, and then loaded with heteropolyacid (CN1289641A) or Al 2 o 3 (CN101298053A), etc., but these supported catalysts also have problems such as easy loss of active sites

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 1.0 g of 1-hydroxyethylidene-1,1-diphosphonic acid (abbreviated as HEDP) and 0.3 g of cetyl alcohol polyoxyethylene ether to 25 ml of water, stir at 35 °C for 1 hour, slowly drop Add 1.0 g of zirconium isopropoxide (purity: 99.9%, Bailingwei Technology Co., Ltd.), continue to stir at a slow speed for 1 hour, put it into a reaction kettle and crystallize at 80 ° C for 24 hours. The solid product was filtered and extracted with ethanol in a Soxhlet apparatus for 24 hours. Then it was added to 10 ml of a mixed solution of anhydrous pyridine (AR, Tianjin Concord Technology Co., Ltd.) and chlorosulfonic acid (AR, product of Gracia (Chengdu) Chemical Technology Co., Ltd.) in a volume ratio of 1:1, slowly After stirring for 5 hours, the mixture was filtered, washed with water and dried.

[0026] The material has a BET specific surface area of ​​610m 2 / g, the pore volume is 0.55cm 3 / g, the macropore pore size distribution is 300-500 nm, the mesopore pore size is 1.9 nm...

Embodiment 2

[0028] Using the preparation process of Example 1, 1.5 g of zirconium isopropoxide was added, and the mixture was crystallized at 60° C. for 48 hours.

[0029] The obtained material has a BET specific surface area of ​​480 m 2 / g, the pore volume is 0.45cm 3 / g, the mesopore diameter is 1.8nm, the macropore diameter distribution is mainly 300-500nm, and the hydrogen ion exchange capacity is 5.8mmol / g.

Embodiment 3

[0031] Using the preparation process of Example 1, 2.0 g of HEDP and 1.0 g of cetyl alcohol polyoxyethylene ether were added to 60 ml of water, and 1.5 g of zirconium isopropoxide was crystallized at 80° C. for 24 hours.

[0032] The obtained material has a BET specific surface area of ​​550 m 2 / g, the pore volume is 0.5cm 3 / g, the mesopore diameter is 2.1nm, the macropore diameter is 300-500nm, and the hydrogen ion exchange capacity is 6.0mmol / g.

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Abstract

The invention discloses a sulfated zirconium phosphonate solid strong acid porous material. The granule diameter of the material is from tens of microns to hundreds of microns, the material is in a mesoporous-macropore structure, the pore diameter of a macropore is 300-500nm, a pore wall of which the diameter is 1.6-2.2nm between macropores is in a mesoporous structure, the specific surface area is 400-650m<2> / g, and the exchange capacity of a hydrogen ion is 5.4-6.6mmol / g. The porous material has the advantages that the acidity is strong, and the porous material has a higher actual industrial production value.

Description

technical field [0001] The present invention relates to a solid strong acid material and a preparation method thereof, in particular to a sulfonated zirconium phosphonate solid strong acid porous material with a mesoporous-macroporous structure and its preparation. Background technique [0002] In recent years, with the continuous enhancement of people's awareness of environmental protection and the stricter requirements of environmental protection legislation, the pollution problem in the chemical industry has been paid more and more attention. Acid catalysts have been widely used in the field of catalysis, traditional liquid acid catalysts such as H 2 SO 4 ,HCl, H 3 PO 4 The wide application of the catalyst produces a large amount of waste liquid, and there are disadvantages such as serious equipment corrosion, difficult separation of catalyst and reactant, and difficulty in chemical technology to achieve continuous production. Solid acid catalysts can replace liquid a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/18B01J35/10
Inventor 袁忠勇林秀珍李永祥慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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