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Method of preparation of pentaerythritol and co-production of sodium oxalate

A technology of pentaerythritol and sodium oxalate, applied in the field of chemical technology, can solve the problems of reducing the usage rate of formic acid, high requirements on the mechanical strength and corrosion strength of the reactor, environmental pollution, etc., and achieves low requirements on mechanical strength, good process economy, and purity. high effect

Inactive Publication Date: 2019-01-15
武汉中能恒信工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. In the actual production process, 88% formic acid solution is generally used, which has strong acidity and requires high mechanical strength and corrosion strength of the reactor;
[0004] 2. The condensation reaction in the pentaerythritol production process is an exothermic reaction, and the neutralization reaction of formic acid is also an exothermic reaction. A large amount of heat release causes formic acid in the formic acid solution to escape in the form of gas, which reduces the utilization rate of formic acid and easily causes environmental pollution;
[0005] 3. The traditional production of sodium formate requires a lot of heat energy for evaporation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation method for pentaerythritol co-production sodium oxalate, comprising the steps:

[0026] 1) Mix formaldehyde, acetaldehyde, and sodium hydroxide according to the mass ratio of 5:1:1.05 and carry out condensation reaction at 40°C. After 30 minutes of reaction, keep warm for 40 minutes;

[0027] 2), add saturated oxalic acid solution to the reaction solution after heat preservation in step 1), adjust its pH value to 6.5 (at this time, the material density is 1.29g / ml), cool and crystallize for 30min, filter, and filter to obtain the first filter material through Washing, drying to obtain a content of 98.6wt% sodium oxalate (99.2% conversion rate);

[0028] 3), the first mother liquor obtained by filtering in step 2) was removed from formaldehyde and methanol, concentrated to a density of 1.38g / ml, cooled and crystallized for 5.5h, and then centrifuged at 45°C to obtain the second filter material after washing, Pentaerythritol with a content of 95.8wt%, a pla...

Embodiment 2

[0032] A preparation method for pentaerythritol co-production sodium oxalate, comprising the steps:

[0033] 1) Mix formaldehyde, acetaldehyde, and sodium hydroxide according to the mass ratio of 8:1:1.1 and carry out condensation reaction at 20°C. After 60 minutes of reaction, keep warm for 45 minutes;

[0034] 2), add saturated oxalic acid solution to the reaction solution after heat preservation in step 1), adjust its pH value to 6 (at this time, the material density is 1.24g / ml), cool and crystallize for 45min, filter, and filter to obtain the first filter material through Washing and drying to obtain sodium oxalate (99.0% conversion rate) with a content of 99.0 wt%;

[0035] 3) Remove formaldehyde and methanol from the first mother liquor obtained by filtering in step 2), concentrate to a density of 1.40g / ml, cool and crystallize for 6h, and then centrifuge at 50°C to obtain the second filter material, which is washed and dried Pentaerythritol with a content of 95.2 wt%,...

Embodiment 3

[0039] A preparation method for pentaerythritol co-production sodium oxalate, comprising the steps:

[0040] 1) Formaldehyde, acetaldehyde, and sodium hydroxide are mixed according to the ratio of substances of 13:1.15:1.2, and condensation reaction is carried out at 68°C, and the reaction is 90 minutes and then kept for 50 minutes;

[0041] 2), add saturated oxalic acid solution to the reaction solution after heat preservation in step 1), adjust its pH value to 7 (at this time, the material density is 1.31g / ml), cool and crystallize for 45min, filter, and filter to obtain the first filter material through Washing and drying to obtain sodium oxalate (98.8% conversion rate) with a content of 99.0wt%;

[0042] 3) Remove formaldehyde and methanol from the first mother liquor obtained by filtering in step 2), concentrate to a density of 1.40g / ml, cool and crystallize for 7 hours, and then centrifuge at 45°C to obtain the second filter material, which is washed and dried Pentaeryt...

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PUM

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Abstract

The invention relates to a method for preparation of pentaerythritol and co-production of sodium oxalate. The method comprises the following steps: dissolving formaldehyde, acetaldehyde and sodium hydroxide, carrying out condensation reaction, adding an oxalic acid solution into a reaction liquid after heat preservation of the reaction, cooling, crystallizing, filtering to obtain a first filter material, washing the filtered first filter material, drying to obtain sodium oxalate, removing formaldehyde and methanol from filtered first mother liquor, concentrating, cooling, crystallizing, then centrifugally separating to obtain a second filter material, and washing and drying the second filter material to obtain the pentaerythritol; settling second mother liquor obtained by centrifugal separation, filtering, combining the filtered filter cake into the first mother liquor, adding an oxalic acid solution into the filtered filtrate to adjust the pH value, crystallizing, filtering to obtaina third filter material, and washing and drying the filtered third filter material to obtain the sodium oxalate. The yield of the pentaerythritol in the method provided by the invention is more than or equal to 90%, and the purity of the pentaerythritol in the product is greater than or equal to 95%, the ash content is less than or equal to 0.03%, and the chromaticity of the platinum-cobalt coloris less than or equal to 50; the yield of the sodium oxalate reaches more than 98%, and the purity of the sodium oxalate in the product is greater than 98.5%.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation method of pentaerythritol co-production sodium oxalate. Background technique [0002] At present, the production routes of pentaerythritol at home and abroad basically use formic acid as the neutralizing liquid after the condensation reaction. The following problems exist in this kind of production process: [0003] 1. In the actual production process, 88% formic acid solution is generally used, which has strong acidity and requires high mechanical strength and corrosion strength of the reactor; [0004] 2. The condensation reaction in the pentaerythritol production process is an exothermic reaction, and the neutralization reaction of formic acid is also an exothermic reaction. A large amount of heat release causes formic acid in the formic acid solution to escape in the form of gas, which reduces the utilization rate of formic acid and easily causes e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/38C07C29/78C07C31/24C07C51/41C07C53/06
CPCC07C29/38C07C29/78C07C51/412C07C31/245C07C53/06
Inventor 邓宏卫刘毅於佳龙秉文王声光刘祎
Owner 武汉中能恒信工程技术有限公司
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