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Process for synthesizing tripentaerythritol

A technology for the synthesis of tripentaerythritol, which is applied in ether preparation, organic chemistry, etc., can solve the problems of a large amount of organic solvents, harsh reaction conditions, and low synthesis yield, and achieve the effects of cheap raw materials, low reaction temperature, and low energy consumption

Inactive Publication Date: 2003-04-09
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to disclose a synthesis method of tripentaerythritol. The present invention uses formaldehyde, acetaldehyde, dipentaerythritol or pentaerythritol as raw materials, and carries out the synthesis of tripentaerythritol under the action of a solid catalyst, and its synthesis yield is the highest. Increased to 39%, to overcome the harsh reaction conditions existing in the prior art, the need for a large amount of organic solvent and the lower defect of synthetic yield, and avoiding the environmental pollution caused by the use of sodium hydroxide liquid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 7.9g of MgO, 11g of pentaerythritol and 22g of water into a stainless steel reaction kettle, and place it in a water bath at 40°C; uniformly mix 15ml of 20% acetaldehyde aqueous solution and 27ml of 37% formaldehyde aqueous solution to form reaction solution A; Next, use a micro plunger pump to continuously drop the reaction solution A into the reaction kettle; the reaction solution A dripping time is 30min. After the dropwise addition was completed, the reaction was continued for 90 min. After the reaction, the hydrogenation reduction reaction of the aldehyde group was carried out, and the hydrogenation was carried out under normal pressure for two hours under the action of a hydrogenation catalyst 3% Pt / C. After all the reactions are completed, tripentaerythritol is obtained by crystallization. The yield of the reaction product was analyzed by liquid chromatography on the synthesized solution. Calculate the yield of each substance based on the moles of acetaldeh...

Embodiment 2

[0026] Add 3.6g of MgO, 5.5g of dipentaerythritol and 22g of water in a stainless steel reaction kettle, place in a water bath at 40°C; 15ml of 20% aqueous acetaldehyde solution and 27ml of 37% formaldehyde aqueous solution are evenly mixed to form reaction solution A; In the stirring state, use a micro plunger pump to continuously drop the reaction solution A into the reaction kettle; the time for adding the reaction solution A is 60 minutes. After the dropwise addition was completed, the reaction was continued for 90 min. After the reaction, the hydrogenation reduction reaction of the aldehyde group was carried out, and the hydrogenation was carried out under normal pressure for two hours under the action of a hydrogenation catalyst 3% Pt / C. The results are shown in Table 1

Embodiment 3

[0028] Add 3.6g of MgO, 11g of pentaerythritol and 22g of water into the stainless steel reaction kettle, and place it in a water bath at 60°C; mix 15ml of 20% acetaldehyde aqueous solution with 27ml of 37% formaldehyde aqueous solution to form the reaction solution A; Next, use a micro plunger pump to continuously drop the reaction solution A into the reaction kettle; the dropping time of the reaction solution A is 30min. After the dropwise addition was completed, the reaction was continued for 90 min. After the reaction, the hydrogenation reduction reaction of the aldehyde group was carried out, and the hydrogenation was carried out under normal pressure for two hours under the action of a hydrogenation catalyst 3% Pt / C. The results are shown in Table 1.

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Abstract

The synthesizing process of tripentaerythritol is one to drop the mixed solution of acetaldehyde and formaldehyde into the mixture of water, pentaerythritol and / or bipentaerythritol and solid catalyst to perform synthesis reaction. The solid catalyst is one of magnesia, calcium hydroxide, barium hydroxide, RE modified MgO or Al2O3, alkali metal hydroxide or alkali earth metal hydroxide modified MgO or Al2O3. The said process has the features of high tripentaerythritol yield, cheap reactant material, lower reaction temperature and lower power consumption. The solid alkali catalyst may be reused and the process may be performed directly in traditional pentaerythritol producing equipment and has excellent industrial application foreground.

Description

technical field [0001] The invention relates to a synthesis method of tripentaerythritol, in particular to a method for preparing tripentaerythritol by using formaldehyde, acetaldehyde, pentaerythritol or dipentaerythritol as raw materials under the action of a solid base. Background technique [0002] The use of tripentaerythritol is increasing day by day, and it has important applications in the fields of rosin ester, stabilizer material, flame retardant material coating, advanced lubricating oil, adhesive coating, textile softener, refrigerant, dispersant, etc. At present, there is no special preparation method for tripentaerythritol, and the processes involved in producing tripentaerythritol mainly include the following categories: [0003] (1) Patents Jp07165651, Jp07165653, Jp0776541, Jp07258139, Jp188086 and Jp07157450 propose a method for preparing dipentaerythritol under the action of an alkaline or acidic catalyst using pentaerythritol as a raw material, treated wi...

Claims

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Application Information

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IPC IPC(8): C07C41/01C07C43/13
Inventor 王幸宜李春香胡广侠卢冠忠
Owner EAST CHINA UNIV OF SCI & TECH
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