Production process of high-purity aminoacetaldehyde dimethyl acetal

A technology of aminoacetaldehyde dimethyl acetal and chloroacetaldehyde dimethyl acetal, which is applied in the chemical industry, can solve environmental problems and energy consumption, increase the separation process, and difficult to separate finished products, etc., so as to reduce energy demand and improve reaction efficiency , The effect of increasing product output

Pending Publication Date: 2021-02-19
INNER MONGOLIA SAINTCHEM CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. This process produces more secondary amine and tertiary amine conjugate by-product impurities, and it is difficult to separate the secondary amine and tertiary amine conjugate by-product impurities from aminoacetaldehyde dimethyl acetal, which brings corresponding environmental problems and energy Consumption, and it is difficult to separate to obtain high-purity finished products
[0005] 2. When the process uses ammonia water as the reaction raw material, the product aminoacetaldehyde dimethyl acetal and water are co-dissolved and azeotroped, and the separation is difficult. It needs to be separated by a rectification tower, which increases the separation process, and the process generally uses a rectification tower to refine Distillation, resulting in a large amount of energy consumption, and can not simply obtain anhydrous high-purity products

Method used

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  • Production process of high-purity aminoacetaldehyde dimethyl acetal
  • Production process of high-purity aminoacetaldehyde dimethyl acetal
  • Production process of high-purity aminoacetaldehyde dimethyl acetal

Examples

Experimental program
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Effect test

Embodiment 1

[0028] In a 3000L high-pressure reactor, use a metering pump to add chloroacetaldehyde dimethyl acetal to the kettle. The mass of chloroacetaldehyde dimethyl acetal is 250kg (2kmol), and then add 4.2kg of iodine and potassium iodide mixed catalyst (1:1) (0.02 kmol). After sealing, replace with argon three times, then add 1632kg of anhydrous liquid ammonia (120kmol) through the liquid ammonia metering pump, then start to heat up to 120°C, the pressure in the kettle reaches 9.0MPa, keep this temperature, and continue the reaction for 30 hours. After the reaction, the temperature is lowered to 60-70°C, ammonia is removed and ammonia is recovered until the temperature drops below 30°C, and the ammonia is recovered and stopped. Then add 360 kg (2 kmol) of sodium methoxide methanol solution with a mass fraction of 30% measured from the dropping tank, stir for 1 hour, and filter to remove salt. The solvent methanol was evaporated from the filtrate under normal pressure, and the crud...

Embodiment 2

[0030] In a 3000L high-pressure reactor, use a metering pump to add chloroacetaldehyde dimethyl acetal to the kettle. The mass of chloroacetaldehyde dimethyl acetal is 250kg (2kmol), and then add iodine and ammonium iodide mixed catalyst (1:1) 4.04kg (0.02kmol). After sealing, replace with argon three times, then add 1768kg of anhydrous liquid ammonia (130kmol) through the liquid ammonia metering pump, then start to heat up to 122°C, the pressure in the kettle reaches 9.3MPa, keep this temperature, and continue the reaction for 35 hours. After the reaction, the temperature is lowered to 60-70°C, ammonia is removed and ammonia is recovered until the temperature drops below 30°C, and the ammonia is recovered and stopped. Then add 360 kg (2 kmol) of sodium methoxide methanol solution with a mass fraction of 30% measured from the dropping tank, stir for 1 hour, and filter to remove salt. The solvent methanol was evaporated from the filtrate under normal pressure, and the crude pr...

Embodiment 3

[0032] In a 3000L high-pressure reactor, use a metering pump to add chloroacetaldehyde dimethyl acetal to the kettle. The mass of chloroacetaldehyde dimethyl acetal is 250kg (2kmol), and then add iodine and silver iodide mixed catalyst (1:1) 4.88kg (0.015 kmol). After sealing, replace with argon three times, then add 1768kg of anhydrous liquid ammonia (130kmol) through the liquid ammonia metering pump, then start to heat up to 122°C, the pressure inside the kettle reaches 9.3MPa, keep this temperature, and continue the reaction for 38 hours. After the reaction, the temperature is lowered to 60-70°C, ammonia is removed and ammonia is recovered until the temperature drops below 30°C, and the ammonia is recovered and stopped. Then add 360 kg (2 kmol) of sodium methoxide methanol solution with a mass fraction of 30% measured from the dropping tank, stir for 1 hour, and filter to remove salt. The solvent methanol was evaporated from the filtrate under normal pressure, and the crud...

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Abstract

The invention discloses a production process of high-purity aminoacetaldehyde dimethyl acetal. The process comprises the following steps: proportionally mixing chloroacetaldehyde dimethyl acetal withanhydrous liquid ammonia to react, and carrying out ammoniation, deamination recovery, alkali neutralization desalination, distillation and rectification in the presence of an iodine-containing catalyst to obtain the high-purity aminoacetaldehyde dimethyl acetal. According to the method, chloroacetaldehyde dimethyl acetal is innovatively used as a main raw material, anhydrous liquid ammonia is used as a solvent and a reaction raw material, an iodine-containing catalyst is added, and the anhydrous high-purity aminoacetaldehyde dimethyl acetal is obtained through ammoniation, deamination, alkalineutralization desalination, distillation and rectification. In practice, the technical process can reduce the generation of by-product conjugates, can realize higher conversion rate than the traditional process under the condition of higher catalytic effect, and simultaneously reduces the requirements on organic solvents and energy sources; and under the condition of the same proportion, the single-batch feeding amount and the product yield of the novel process are improved by 50% or above, the yield is about 20% higher than that of a traditional process, and the effects of saving energy, improving quality, reducing cost and reducing consumption can be achieved.

Description

Technical field: [0001] The invention relates to a high-purity aminoacetaldehyde dimethyl acetal production process, which belongs to the field of chemical industry. Background technique: [0002] Aminoacetaldehyde dimethyl acetal, Aminoacetaldehyde dimethyl acetal, also known as aminoacetaldehyde dimethyl acetal, molecular formula is C4H12NO2, molecular weight is 105.14, CAS registration number is 22483-09-6, colorless liquid, used as a pharmaceutical intermediate . Used in efficient 3-step synthesis of proline analogs from ascorbic acid; 4 Catalyzed, 3-step reaction to prepare phosphoramidates. [0003] The traditional process route of aminoacetaldehyde dimethyl acetal is to react directly with chloroacetaldehyde dimethyl acetal and ammonia water. The temperature required for the reaction is relatively high, reaching about 135°C. Continue deamination and dehydration at 110-125°C, then lower the temperature to 60-70°C and add liquid caustic soda to neutralize and remove ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C213/10C07C217/40
CPCC07C213/02C07C213/10C07C217/40
Inventor 杨丰乐孙晟中白深科
Owner INNER MONGOLIA SAINTCHEM CHEM
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