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Method for preparing pentaerythritol and dipentaerythritol

A technology of dipentaerythritol and monopentaerythritol, which is applied in the field of preparation of pentaerythritol, can solve the problems of low total yield of monopentaerythritol and dipentaerythritol, low yield of dipentaerythritol, complex reaction process, etc., achieve high total yield and reduce production cost , The effect of simple process

Active Publication Date: 2010-04-21
濮阳市鹏鑫化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method process is complicated, and the productive rate of producing dipentaerythritol is lower, and monopentaerythritol and dipentaerythritol total productive rate are also lower
In addition, the application number is 200810024057.X publication number is the patent application of CN101265166A, discloses a kind of production method of monopentaerythritol, dipentaerythritol and tripentaerythritol, need carry out pressurized precondensation with inert gas in the precondensation reactor during production, then Then transfer the reaction solution to the main condensation reactor pressurized with inert gas for reaction, the reaction process is more complicated

Method used

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  • Method for preparing pentaerythritol and dipentaerythritol
  • Method for preparing pentaerythritol and dipentaerythritol
  • Method for preparing pentaerythritol and dipentaerythritol

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Example 1: Preparation method of monopentaerythritol and dipentaerythritol, see attached figure 1 .

[0052] The reaction was carried out at a molar ratio of formaldehyde: acetaldehyde: sodium hydroxide = 5.5:1: 1.12, the acetaldehyde feeding amount was 15 Kmol, and the entire feeding time was 120 minutes. Add 10.5m formaldehyde solution with a temperature of 25℃ and a concentration of 15g / 100ml in the reactor 3 , And then add sodium hydroxide solution, acetaldehyde solution and the remaining formaldehyde solution while stirring and the reaction liquid is circulated with a pump. In the first 40 minutes, add 330L of sodium hydroxide solution with a concentration of 30g / 100ml, Two put 670L of 30g / 100ml sodium hydroxide solution in 40 minutes, put 1240L of 30g / 100ml sodium hydroxide solution in the third 40 minutes, and start adding acetaldehyde after 10 minutes of sodium hydroxide solution , 1650L of acetaldehyde solution with a concentration of 40g / 100ml was uniformly pour...

Embodiment 2

[0058] Example 2: Preparation method of monopentaerythritol and dipentaerythritol, see attached figure 1 .

[0059] The reaction was carried out at a molar ratio of formaldehyde: acetaldehyde: sodium hydroxide = 5.0:1:1.10, the feeding amount of acetaldehyde was 15Kmol, and the feeding time was 120 minutes. Add 10m formaldehyde solution with a temperature of 20℃ and a concentration of 15g / 100ml in the reactor in advance 3 , And then add sodium hydroxide solution, acetaldehyde solution and the remaining formaldehyde solution while stirring and the reaction solution is circulated with a pump. In the first 40 minutes, add 500L of sodium hydroxide solution with a concentration of 25g / 100ml. Two put 940L of 25g / 100ml sodium hydroxide solution in 40 minutes, put 1200L of 25g / 100ml sodium hydroxide solution in the third 40 minutes, and start adding acetaldehyde after 10 minutes of sodium hydroxide solution , 2640L of acetaldehyde solution with a concentration of 25g / 100ml is evenly put...

Embodiment 3

[0065] Example 3: Preparation method of monopentaerythritol and dipentaerythritol, see attached figure 1 .

[0066] The reaction was carried out at a molar ratio of formaldehyde: acetaldehyde: sodium hydroxide = 4.5:1: 1.08, the feeding amount of acetaldehyde was 20 Kmol, and the feeding time was 150 minutes. Add 15.8m formaldehyde solution with a temperature of 18℃ and a concentration of 13g / 100ml in the reactor in advance 3 , And then add sodium hydroxide solution, acetaldehyde solution and the remaining formaldehyde solution while stirring and the reaction solution is circulated with a pump. In the first 50 minutes, add 600L of sodium hydroxide solution with a concentration of 15g / 100ml. In the second 50 minutes, put in 1600L of sodium hydroxide solution with a concentration of 15g / 100ml, and put in 3560L of sodium hydroxide solution with a concentration of 15g / 100ml in the third 50 minutes, and start to add B after 10 minutes of sodium hydroxide solution. Aldehyde, 2933L of ...

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Abstract

The invention relates to a method for preparing pentaerythritol and dipentaerythritol, which comprises the steps of: taking formaldehyde, aldehyde and sodium hydroxide as raw materials, controlling the reaction temperature according to a reaction mechanism, adopting a specific feeding program to control the mixture ratio of the raw materials for a reaction, and using formic acid for neutralization after the reaction is finished; and reducing the temperature of a reaction solution through the cooling, filtering tripentearythritol, then crystallizing to separate the pentaerythritol and a crude dipentaerythritol product respectively at a specified temperature through rectification dealdehyding, pressurized hydrolysis and evaporation concentration, and obtaining a refined dipentaerythritol product by refining the crude dipentaerythritol product. The method has a simple process, and reduces the generation of the tripentearythritol as much as possible on the premise of ensuring the yield of the dipentaerythritol and the total yield by accurately controlling the mixture ratio and the concentration of the raw materials, the reaction temperature and the feeding program; and the obtained pentaerythritol and dipentaerythritol have high quality, particularly the dipentaerythritol has high content, the content of the dipentaerythritol can reach over 90 percent, and the ash content is low and is only between 0.01 and 0.03 percent.

Description

1. Technical Field: [0001] The invention relates to a preparation method of pentaerythritol, in particular to a method for preparing monopentaerythritol and dipentaerythritol by condensation reaction. 2. Background technology: [0002] At present, the production technology of pentaerythritol at home and abroad is basically obtained by condensation reaction of formaldehyde, acetaldehyde and sodium hydroxide or calcium hydroxide as raw materials, and then concentrated and separated. Due to the complexity of the reaction, the product produced during the reaction is a mixture containing monopentaerythritol, dipentaerythritol, tripentaerythritol, etc. If they are not separated, the pentaerythritol mixture with lower added value is obtained, which is commonly known as industrial pentaerythritol. If they are separated, high value-added monopentaerythritol, dipentaerythritol, especially dipentaerythritol will be obtained, the price of which is 4-6 times that of industrial pentaerythritol...

Claims

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Application Information

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IPC IPC(8): C07C43/13C07C41/01C07C31/24C07C29/38
Inventor 滕冬成谷同军盛和滨董学磊董雁如于永平马金芳王秀云周鹏程
Owner 濮阳市鹏鑫化工有限公司
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