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Catalyst for selectively synthesizing 4-methyl-2,6-di-tert-butylphenol and application of catalyst

A technology of di-tert-butylphenol and p-cresol, which is applied in the field of catalysis, can solve the problems of reaching about 3% and is difficult to realize industrial application, and achieve the effects of long service life, easy industrial production, and good BHT selectivity

Active Publication Date: 2018-02-27
BAOJI UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Li Wenfeng et al. (Tianjin University, 2006, master's thesis) used metal cations to modify Hβ zeolite, and the p-cresol conversion rate reached 70.2%, and the 2-tert-butyl p-cresol selectivity was 93.6%, but the BHT yield only reached About 3%, it is difficult to realize industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 100g of Hβ molecular sieve into the reaction kettle, add 200g of ammonium phosphate aqueous solution with a mass concentration of 2.0%, stir at 70°C for 6 hours, drop to normal temperature, filter, wash, and dry at 60°C to obtain modified Hβ molecular sieve; Volume impregnation method, according to the loading of 3% of Co and 5% of phosphotungstic acid (both in terms of carrier), the modified Hβ molecular sieve and cobalt nitrate aqueous solution were first impregnated for 5 hours, and dried at 80°C for 10 hours after the impregnation was completed. Then impregnate with phosphotungstic acid aqueous solution for 5 hours, dry at 80°C for 10 hours after impregnation, and then bake at 400°C for 5 hours to obtain 3%Co-5%H 3 PO 40 W 12 / Hβ molecular sieve catalyst.

Embodiment 2

[0022] Add 100g of USY molecular sieve into the reaction kettle, add 300g of ammonium hydrogen phosphate aqueous solution with a mass concentration of 1.0%, stir at 70°C for 6 hours, drop to normal temperature, filter, wash, and dry at 60°C to obtain a modified USY molecular sieve; Equal-volume impregnation method, according to the loading capacity of 4% Co and 3% loading capacity of silicotungstic acid (both based on the carrier), first impregnate the modified USY molecular sieve and cobalt nitrate aqueous solution for 5 hours, and dry at 80°C for 10 hours after impregnation , and then impregnated with silicotungstic acid aqueous solution for 5 hours, dried at 80°C for 10 hours after impregnation, and then fired at 400°C for 5 hours to obtain 4%Co-3%H 6 SiO 39 W 12 / USY molecular sieve catalyst.

Embodiment 3

[0024] Add 100g of REY molecular sieve to the reaction kettle, add 400g of ammonium dihydrogen phosphate aqueous solution with a mass concentration of 0.5%, stir at 70°C for 6 hours, lower to normal temperature, filter, wash, and dry at 60°C to obtain modified REY molecular sieve; Using the equal-volume impregnation method, according to the loading of Co 2%, the loading of phosphotungstic acid 2%, and the loading of phosphomolybdic acid 2% (both based on carrier), the modified REY molecular sieve and cobalt nitrate aqueous solution were impregnated first. 5 hours, dry at 80°C for 10 hours after impregnation, then impregnate with aqueous solution of phosphotungstic acid and phosphomolybdic acid for 5 hours, dry at 80°C for 10 hours after impregnation, and then bake at 400°C for 5 hours to obtain 2% Co- 2%H 3 PO 40 W 12 -2%H 3 [P(Mo 3 o 10 )] 4 / REY molecular sieve catalyst.

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PUM

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Abstract

The invention discloses a catalyst for selectively synthesizing 4-methyl-2,6-di-tert-butylphenol and application of the catalyst. The catalyst is prepared from a molecular sieve as a carrier modifiedby any one of ammonium phosphate, ammonium hydrogen phosphate and ammonium dihydrogen phosphate, and an active component A and an active component B carried by the carrier, wherein the molecular sieveis an Hbeta molecular sieve, H-mordenite, an HY molecular sieve, an USY (Ultra-Stable Y Zeolit) molecular sieve, an REY molecular sieve or a SAPO-5 (Silicoaluminophosphate) molecular sieve; the active component A is Co, Cu, Ni or Fe; the active component B is at least one of phosphotungstic acid, silicotungstic acid, phosphomolybdic acid, silicomolybdic acid and sodium tungstate; by the carrier,the carrying amount of the active component A is 2-5%, and the carrying amount of the active component B is 2-10%. The catalyst disclosed by the invention is applied to p-methylphenol and isobutene ortertiary butanol to produce 4-methyl-2,6-ditertiary butyl phenol, and has the advantages of low catalyst cost, high raw material conversion rate, good product selectivity, long catalyst service life,simple use process and the like.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a catalyst for selectively synthesizing 4-methyl-2,6-di-tert-butylphenol by reacting p-cresol with isobutene or tert-butanol. Background technique [0002] 4-Methyl-2,6-di-tert-butylphenol (BHT) is an important hindered phenolic antioxidant, widely used in food processing, oil preservation, fuel oil preservation and food, medical supplies packaging materials, polymer Olefins, synthetic rubber, plastics and other fields. In recent years, the demand for BHT has been increasing year by year, and the market is in short supply. Scholars from various countries have carried out in-depth research on the catalytic synthesis of BHT. The main catalysts used are liquid acids, metal oxides, metal salts, ion exchange resins, solid superacids and heteropolyacids. [0003] Liquid acids such as sulfuric acid, sulfur trioxide, sulfosalicylic acid, benzenesulfonic acid, etc. At pres...

Claims

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Application Information

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IPC IPC(8): B01J29/16B01J29/26B01J29/78B01J29/85C07C37/11C07C37/14C07C39/06
CPCB01J27/188B01J29/166B01J29/26B01J29/7815B01J29/85B01J37/0207B01J37/024B01J2229/18C07C37/11C07C37/14C07C39/06
Inventor 冯国栋钱华明张锋罗小林王伟胡月桥苗康康
Owner BAOJI UNIV OF ARTS & SCI
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