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Synthesis method of glyoxal

A synthesis method and technology of glyoxal, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve problems such as difficulty in meeting quality requirements, pollution, and high cost of raw materials

Inactive Publication Date: 2020-07-07
徐州顺平生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the ethylene glycol air oxidation process is simple and the product yield is high, but the cost of raw materials is relatively high, and the product contains more formaldehyde, which is difficult to meet the quality requirements of the pharmaceutical and other industries; the cost of raw materials for the acetaldehyde nitric acid oxidation method is low, The reaction conditions are mild, the product does not contain formaldehyde, but the selectivity is poor, the yield is low, a large amount of acetic acid is produced by-product, the separation and treatment are more complicated, and there is NO x Pollution and other "three wastes" issues

Method used

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  • Synthesis method of glyoxal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1. A method for synthesizing glyoxal, characterized in that the method comprises the following steps:

[0016] Step 1. Weigh 0.1mol Na 2 SiO 3 ·9H 2 O was dissolved in 65ml of deionized water, then 0.01mol of ferric nitrate was added to the above solution, and the pH was adjusted to 11 with dilute sulfuric acid and then stirred for 30 min;

[0017] Step 2. Then weigh 0.02mol cetyltrimethylammonium bromide CTMAB and dissolve it in 15ml deionized water, add it to the above solution, and stir for 30 min until it is completely dissolved;

[0018] Step 3. Place the resulting solution in a reaction kettle to crystallize at 418 K for 48 h, cool to room temperature and then suction filter, wash with deionized water to neutrality, dry, and then transfer to a muffle furnace for forging at 823 K Burn for 6h to obtain Fe-MCM-41;

[0019] Step 4. Dissolve 6g of cellulose acetate powder, 12g of polyvinylpyrrolidone, and 8g of Fe-MCM-41 in the N,N-dimethylacetamide solution for 24 hours;

[00...

Embodiment 2

[0025] Step 7. After activation is completed, feed ethylene glycol into the preheater and heat it to 198°C. The gasified ethylene glycol is mixed with steam, preheated air and nitrogen. The liquid hourly space velocity of the glycol is 0.05 m / s. The molar ratio of ethylene glycol to oxygen is 1:5, the molar ratio of ethylene glycol to nitrogen is 1:21, and the molar ratio of ethylene glycol to water is 1:0.5; the remaining steps are the same as in Example 1.

Embodiment 3

[0027] Step 7. After activation is completed, feed ethylene glycol into the preheater and heat it to 198°C. The gasified ethylene glycol is mixed with steam, preheated air and nitrogen. The liquid hourly space velocity of the glycol is 0.05 m / s. The molar ratio of ethylene glycol to oxygen is 1:5, the molar ratio of ethylene glycol to nitrogen is 1:21, and the molar ratio of ethylene glycol to water is 1:0.5; other steps are the same as in Example 1.

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Abstract

The invention discloses a synthesis method of glyoxal, which comprises the following steps: taking Na2SiO3. 9H2O, ferric nitrate, hexadecyl trimethyl ammonium bromide, ethylene glycol and oxygen as main raw materials, wherein proportions of the used raw materials are set according to the following proportion: the molar ratio of ethylene glycol to oxygen is 1: 5; the molar ratio of Na2SiO3. 9H2O toferric nitrate is 10: 1; the molar ratio of ferric nitrate to hexadecyl trimethyl ammonium bromide is 1: 2. According to the synthesis process disclosed by the invention, ferrosilicon zeolite and cellulose acetate are used as raw materials to prepare the mesoporous blended solid catalyst by adopting a phase inversion method; the catalyst has good mesoporous distribution and mechanical properties,especially has a very good oxidation reaction effect on glyoxal; the production cost is greatly saved due to the recycling of the catalyst and residual gas, and the invention has a good industrial application value.

Description

Technical field [0001] The invention relates to a method for synthesizing glyoxal and belongs to the field of chemical synthesis. Background technique [0002] Glyoxal (CAS: 107-22-2) is the simplest aliphatic dibasic aldehyde with the simplest molecular structure. In addition to the generality of aliphatic aldehydes, it also has some special chemical properties. It is an important chemical raw material and intermediate Body, widely used in textile, medicine, metallurgy, environmental protection and other fields. The industry mainly uses ethylene glycol air oxidation method and acetaldehyde nitric acid oxidation method to produce glyoxal. Among them, the ethylene glycol air oxidation method has a simple process and high product yield, but the raw material cost is relatively high, and the product contains more formaldehyde, which is difficult to meet the quality requirements of the pharmaceutical and other industries; the acetaldehyde nitric acid oxidation method has low raw mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/127C07C45/38B01J29/03
CPCC07C45/38B01J29/0333B01J2229/18C07C47/127Y02P20/584
Inventor 赵可马刚
Owner 徐州顺平生物科技有限公司