Catalyst and application thereof to preparing 2, 2, 6, 6-tetramythl-4-piperidone

A technology of catalyst and piperidone, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, organic chemistry, etc., can solve problems such as complicated operation and explosion hazard, and achieve the goal of increasing specific surface area, not easy to lose, and good catalytic activity Effect

Active Publication Date: 2019-05-14
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, intermittent operation still inevitably brings disadvantages such as complicated operation. At the same time, solid sodium hydroxide needs to be used to remove ammonium nitrate in the post-treatment process of the reaction solution, which pollutes the environment and presents a danger of explosion.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Preparation of catalyst:

[0036] Using "precipitation-impregnation" two-step method: the first step is Zr(OH) 4 -Al(OH) 3 Preparation of carrier, ZrOCl 2 ·8H 2 O and Al(NO 3 ) 3 9H 2 O was dissolved in deionized water at a ratio of 20:1 (mass ratio of substances), and then ammonia water (20%, mass fraction) was added dropwise to the above solution to generate Zr(OH) 4 -Al(OH) 3 Precipitate; then continue to add ammonia water until the pH value is 8, and leave the obtained suspension to age at room temperature for 6 hours, then filter and wash with deionized water until the pH value of the filtrate is 7. Dry the resulting filter cake at 100°C for 10 h to obtain Zr(OH) 4 -Al(OH) 3 carrier.

[0037] Step 2: SO 4 2- Loading: for the above Zr(OH) 4 -Al(OH) 3 The carrier was impregnated with a sulfuric acid solution with a concentration of 1wt%, and the impregnation time was 3h; after filtration, the sample was dried at 100°C for 10h, and then calcined at 5...

Embodiment 2

[0042] (1) Preparation of catalyst:

[0043] Using "precipitation-impregnation" two-step method: the first step is Zr(OH) 4 -Al(OH) 3 Preparation of carrier, ZrOCl 2 ·8H 2 O and Al(NO 3 ) 3 9H 2 O was dissolved in deionized water at a ratio of 35:1 (mass ratio of substances), and then ammonia water (35%, mass fraction) was added dropwise to the above solution to generate Zr(OH) 4 -Al(OH) 3 Precipitate; then continue to add ammonia water until the pH value is 10, leave the obtained suspension at room temperature for 7 hours, filter, and wash with deionized water until the pH value of the filtrate is 7. Dry the resulting filter cake at 110°C for 12h to obtain Zr(OH) 4 -Al(OH) 3 carrier.

[0044] Step 2: SO 4 2- Loading: for the above Zr(OH) 4 -Al(OH) 3 The carrier is impregnated with a sulfuric acid solution with a concentration of 3wt%, and the impregnation time is 4h; after filtration, the sample is dried at 110°C for 12h, and roasted at 600°C for 6h in an air at...

Embodiment 3

[0049] (1) Preparation of catalyst:

[0050] Using "precipitation-impregnation" two-step method: the first step is Zr(OH) 4 -Al(OH) 3 Preparation of carrier, ZrOCl 2 ·8H 2 O and Al(NO 3 ) 3 9H 2 O was dissolved in deionized water at a ratio of 30:1 (mass ratio of substances), and then ammonia water (30%, mass fraction) was added dropwise to the above solution to generate Zr(OH) 4 -Al(OH) 3 Precipitate; then continue to add ammonia water until the pH value is 12, leave the obtained suspension at room temperature for 8 hours, filter, and wash with deionized water until the pH value of the filtrate is 7. Dry the obtained filter cake at 115°C for 15h to obtain Zr(OH) 4 -Al(OH) 3 carrier.

[0051] Step 2: SO 4 2- Loading: for the above Zr(OH) 4 -Al(OH) 3 The carrier is impregnated with a sulfuric acid solution with a concentration of 5wt%, and the impregnation time is 5h; after filtration, the sample is dried at 115°C for 15h, and roasted at 650°C for 5h in an air atm...

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Abstract

The invention provides a catalyst and application thereof to preparing 2, 2, 6, 6-tetramythl-4-piperidone. The catalyst comprises SO4<2->-supported zirconium-aluminum compound oxides, which are composed of ZrO and Al2O3. When applied to preparing the 2, 2, 6, 6-tetramythl-4-piperidone, the catalyst has the advantages of being safe, efficient, easy to recycle and the like.

Description

technical field [0001] The present invention relates to a catalyst and a preparation method thereof, and also relates to the application of the catalyst in the preparation of 2,2,6,6-tetramethyl-4-piperidone, and further relates to the use of the catalyst to catalyze acetone and ammonia to prepare 2, 2,6,6-tetramethyl-4-piperidone method. Background technique [0002] The hindered amine light stabilizer has always been the focus of attention and development because of its excellent light stabilizing effect. As the only source of hindered piperidine ring, 2,2,6,6-tetramethyl-4-piperidone is the most basic raw material for most hindered amine light stabilizers. The development of the stabilizer industry. [0003] US3943139 discloses a method for obtaining 2,2,6,6-tetramethyl-4-piperidone by reacting phorone with ammonia; US3953459 discloses a method for synthesizing 2,2, A method for 6,6-tetramethyl-4-piperidone; US4252958 discloses a method for synthesizing 2,2,6,6-tetrame...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053B01J35/10B01J37/02B01J37/03C07D211/74
Inventor 赵晶李俊平牟通张彦雨杜旺明王漭付松王锐边新建陈海波黎源
Owner WANHUA CHEM GRP CO LTD
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