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LDH catalyst for Tishchenko reaction and preparation method thereof

A catalyst, anionic clay technology, applied in the field of pillared hydrotalcite (LDH) catalyst and its preparation, can solve the problems of less by-products, equipment corrosion, more by-products, etc., and achieve less by-products, less equipment corrosion, and by-products less effect

Inactive Publication Date: 2010-12-29
江苏天音化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of LDH catalyst that is used for Tischenko reaction and preparation method thereof, can overcome the low product yield that exists in base catalyst in the existing Tischenko reaction, many by-products, the defects such as serious corrosion to equipment, in It is used as a catalyst in the synthesis of esters by the Jishchenko reaction to achieve the goals of high yield per pass, less by-products, low cost, and environmental friendliness

Method used

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  • LDH catalyst for Tishchenko reaction and preparation method thereof
  • LDH catalyst for Tishchenko reaction and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] The preparation method of the layered magnesium aluminum anion clay catalyst supported by tert-butoxy anion pillar comprises the following steps:

[0023] (1) Magnesium aluminum anion clay (MgAl-HT-NO 3 ) preparation

[0024] In a reaction kettle with a thermometer, a stirrer and a dropping funnel, under nitrogen protection, 30.8g (0.12mol) Mg(NO 3 ) 2 ·6H 2 0 and 15.0 g ( 0.04 mol) Al(NO 3 ) 3 9H 2 0 Dissolve completely in 100 mL of CO removal 2 deionized water; at room temperature and under stirring conditions, add 2 M NaOH solution dropwise, control the pH value of the slurry at about 10 during the dropping process, and keep the dropping time at about 1 h; continue stirring for 2 h after the dropping . After the reaction, carry out vacuum filtration, and wash the obtained filter cake with water until the filtrate is neutral; the washed filter cake is vacuum-dried at 80°C for 10 h to obtain about 15.2 g of magnesium-aluminum anion clay, marked as MgAl- HT-NO ...

Embodiment 2

[0028] The preparation method of the layered magnesium aluminum anion clay catalyst supported by tert-butoxy anion pillar comprises the following steps:

[0029] (1) Magnesium aluminum anion clay (MgAl-HT-NO 3 ) preparation

[0030] In a reaction kettle with a thermometer, a stirrer and a dropping funnel, under nitrogen protection, 30.8g (0.12mol) Mg(NO 3 ) 2 ·6H 2 0 and 12.8 g ( 0.035 mol) Al(NO 3 ) 3 9H 2 0 Dissolve completely in 100 mL of CO removal 2 deionized water; at room temperature and under stirring conditions, add 2 M NaOH solution dropwise, control the pH value of the slurry at about 10 during the dropping process, and keep the dropping time at about 1 h; continue stirring for 2 h after the dropping . After the reaction, carry out vacuum filtration, and wash the obtained filter cake with water until the filtrate is neutral; the washed filter cake is vacuum-dried at 80°C for 10 h to obtain about 14.7 g of magnesium-aluminum anion clay, marked as MgAl- HT-NO...

Embodiment 3

[0034] Using the layered magnesium-aluminum anion clay supported by tert-butoxy anion pillars obtained in Example 1 as a catalyst for the Jishchenko reaction, catalyzed synthesis of 2,2,4-trimethyl-1,3-pentanediol monoisobutyric acid ester, comprising the following steps:

[0035] 1) Isobutyraldehyde condensation reaction

[0036] In a reaction kettle with a thermometer, a reflux condenser and a constant pressure dropping funnel, under nitrogen protection, normal pressure, and 20°C, add 30 g of NaOH solution with a mass concentration of 2-5%, and continuously and slowly Add 90 g of isobutyraldehyde dropwise for 1 hour; after the dropwise addition, continue to react at 35°C for 4 hours; after stopping the reaction, let the layers stand for 2-3 hours, and after separation, the upper layer is an oil layer, wash with water until neutral , followed by 5 g of anhydrous MgSO 4 Drying yields a dry isobutyraldehyde condensation product. The lower layer is the water layer, which can ...

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Abstract

The invention provides an LDH catalyst for a Tishchenko reaction and a preparation method thereof. The catalyst is laminated magnalium anionic clay supported by a tertiary butoxy negative ion column, wherein the Mg / Al molar ratio in the laminated magnalium anionic clay is 4-2, and the exchange capacity of the tertiary butoxy negative ion is 5.0 to 12.0 percent. The method for preparing the catalyst comprises the following steps of: preparing the laminated magnalium anionic clay by adopting a coprecipitation method; and performing anion exchange on tertiary butanol metal salt and the laminated magnalium anionic clay so as to prepare the laminated magnalium anionic clay supported by the tertiary butoxy negative ion column. The LDH catalyst is used for preparing ester compounds in the Tishchenko reaction, and has the advantages of high yield of single pass, high selectivity of target product, a few side products, mild reaction condition, cycle use, and environment-friendly synthesizing technology.

Description

technical field [0001] The invention relates to a pillared hydrotalcite (LDH) catalyst and a preparation method thereof, in particular to an LDH catalyst used for Tishchenko reaction and a preparation method thereof. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate is a film-forming aid for water-based architectural coatings (usually latex paints), and its advantages are excellent film-forming effect, non-toxic and harmless , can replace other toxic coalescents, and the dosage in water-based latex paints is generally 2 to 6%. Therefore, the industrialization of this coalescent has important economic significance and broad application prospects. At the same time, this product is also an important fine chemical intermediate, which is widely used in industrial PVC plasticizers, lubricants and other related industries. 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate is mainly synthesized using isobutyraldehyde as raw material through a two-step meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C07C69/28C07C67/44
Inventor 秦怡生杨建国秦旭东陈荣福王伟哈健蒋大智张学军朱红伟段启伟
Owner 江苏天音化工有限公司
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