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Process for synthesizing tripentaerythritol

A technology for tripentaerythritol and a synthesis method is applied in the synthesis field of preparing tripentaerythritol, and can solve the problems of large amount of organic solvent, harsh reaction conditions, low yield of tripentaerythritol product and the like

Inactive Publication Date: 2006-04-19
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The main products of the above-mentioned method are pentaerythritol and dipentaerythritol, and tripentaerythritol is only a by-product. The method reaction conditions proposed by the patent Jp 07165652 are particularly harsh, and the amount of organic solvent is large, and mainly pentaerythritol and dipentaerythritol in the product, the product of tripentaerythritol is obtained Low rate, just a by-product

Method used

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  • Process for synthesizing tripentaerythritol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 8ml of 20% NaOH aqueous solution, 44g of dipentaerythritol and 44g of water into a stainless steel reaction kettle, and place it in a water bath at 50°C; mix 32ml of 20% aqueous solution of acetaldehyde with 80ml of 37% aqueous solution of formaldehyde to form reaction solution A ; Under stirring, use a micro plunger pump to continuously drop the reaction solution A and 32ml of 20% NaOH solution in the reactor; the time for adding the reaction solution A and NaOH is 60min. After the dropwise addition was completed, the reaction was continued for 120 min.

[0027] After the reaction, tripentaerythritol was separated by crystallization. The yield of the reaction product was analyzed by liquid chromatography on the synthesized solution. Based on the moles of acetaldehyde and converted dipentaerythritol (one molecule of dipentaerythritol is equivalent to 2 molecules of acetaldehyde), the yields of each substance were calculated, and the results are shown in Table 1.

Embodiment 2

[0029] Replace the 20% NaOH aqueous solution in Example 1 with 20% KOH aqueous solution, and carry out the synthesis of dipentaerythritol according to the same operation steps. The results are shown in Table 1

Embodiment 3

[0031] Add 4ml of 20% NaOH solution, 44g of dipentaerythritol and 44g of water to the stainless steel reaction kettle, place in a water bath at 70°C; mix 32ml of 20% aqueous solution of acetaldehyde with 80ml of 37% aqueous solution of formaldehyde to form reaction solution A ; Under stirring, use a micro plunger pump to continuously drip the 20% NaOH solution of reaction solution A and 28ml in the reactor; the time for adding reaction solution A is 50min, and the time for adding NaOH is 60min. After the dropwise addition was completed, the reaction was continued for 60 min. 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 and the strong alkali solution separately into mixed water solution containing catalyst. During the process, acetaldehyde and over a third of formaldehyde may be first mixed and dropped, while the rest of formaldehyde is added during the reaction. The said process has the features of high tripentaerythritol yield up to 96%, cheap reactant material, lower reaction temperature and lower power consumption. It 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 synthesis method for preparing tripentaerythritol by using formaldehyde, acetaldehyde and dipentaerythritol as raw materials under the action of alkali. 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 Jp 0716565l, Jp 07165653, Jp 0776541, Jp 07258139, Jp 188086 and Jp 07157450 propose a method for preparing dipentaerythritol under the action of an alkaline or acidic catalyst using pentaerythritol as a raw material, treated with car...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/13C07C41/06C07C41/02
Inventor 王幸宜李春香胡广侠卢冠忠
Owner EAST CHINA UNIV OF SCI & TECH