Green synthesis method for one-pot process preparation of AMP-95

An AMP-95, green synthesis technology, which is applied in the preparation of nitro compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of unsuitability for industrial production, difficult purification of products, and high cost of raw materials, and achieves low cost, The effect of high yield and easy product

Inactive Publication Date: 2018-06-19
GUANGZHOU YINTIAN NEW MATERIAL CO LTD +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a green synthesis method for preparing AMP-95 by a one-pot method, which solves the problem that the traditional method has high cost of raw materials, cumbersome steps, great environmental pollution, low yield, and the product is not easy Purification, not suitable for industrial production

Method used

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Examples

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preparation example Construction

[0024] A green synthetic method for preparing AMP-95 by a one-pot method, comprising the following steps:

[0025] S1, in the alcohol solution, acetone, hydrogen peroxide and ammonia generate 2-nitropropane under the catalysis of the catalyst;

[0026] Among them, the conditions required for the preparation of 2-nitropropane in step S1 are: the reaction temperature range is 20-120°C, and the reaction time range is 0.5-5h, the catalyst is a porous framework metal hybrid catalyst, a porous framework metal hybrid catalyst Its skeleton is mainly silicon, oxygen and hybrid metal, wherein the hybrid metal is one or two combinations of titanium, zirconium, vanadium and molybdenum, the ratio of silicon to hybrid metal atoms is 20-100:1, and the hybrid The bimetallic molar ratio is 1:20~1:100; the configuration of the catalyst is one of ZSM-5, MCM-41, SBA-15, and its microporous-mesoporous composite structure and mesopore-macroporous composite structure , wherein the amount of catalys...

Embodiment 1

[0033] Add 10g of catalyst (Ti-V-ZSM-5), 58.08g of acetone, and 20g of ammonia water into 400ml of methanol, raise the temperature to 70°C, slowly add 226.7g of hydrogen peroxide (35%) dropwise, and maintain the temperature at 65- React at 75°C for 1 hour to obtain 2-nitropropane reaction solution; filter, add 5g of sodium hydroxide to the reaction solution, heat up to 35°C, add formaldehyde (40% aqueous solution) dropwise, and continue to react for 3 hours after the dropwise addition to obtain 2-nitropropane -Methyl-2-nitro-propanol reaction solution; put the reaction solution into the autoclave, add 14g of Raney nickel, the reaction temperature is 75°C, the reaction pressure is 3MPa, and the reaction is 4h to obtain 2-methyl-2-amino- The crude product of 1-propanol was rectified to obtain 44.6g of product (AMP-95).

Embodiment 2

[0035]Add 10g of catalyst (Zr-V-SBA-15), 58.08g of acetone, and 20g of ammonia water into 400ml of methanol, raise the temperature to 70°C, slowly add 226.7g of hydrogen peroxide (35%) dropwise, and maintain the temperature at 65- React at 75°C for 2 hours to obtain a 2-nitropropane reaction solution; filter, add 5g of sodium hydroxide to the reaction solution, heat up to 35°C, add formaldehyde (40% aqueous solution) dropwise, and continue the reaction for 3 hours after the dropwise addition to obtain 2-nitropropane -Methyl-2-nitro-propanol reaction solution; put the reaction solution into the autoclave, add 14g of Raney nickel, the reaction temperature is 75°C, the reaction pressure is 3MPa, and the reaction is 4h to obtain 2-methyl-2-amino- The crude product of 1-propanol was rectified to obtain 53.4g of product (AMP-95).

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Abstract

The invention discloses a green synthesis method for the one-pot process preparation of AMP-95. The method comprises the following steps: S1, preparing 2-nitropropane from acetone, hydrogen peroxide and ammonia in an alcohol solution under the catalysis of a catalyst; S2, directly reacting a reaction solution obtained in step S1 with formaldehyde or paraformaldehyde under an alkaline condition without purifying in order to generate 2-nitro-2-methyl-1-propanol; and S3, directly hydrogenating the reaction product obtained in step S2 without purifying to obtain the product 2-amino-2-methy-1-propanol (AMP-95), and rectifying the product to make the purity reach 99.5% or more. The method has the advantages of cheap and easily available raw materials, simple reaction steps, small pollution to the environment, low cost, high yield, easiness in purification of the product, and suitableness for industrial production.

Description

technical field [0001] The invention relates to the technical field of synthesis and preparation of fine chemical products, in particular to a green synthesis method for preparing AMP-95 by a one-pot method. Background technique [0002] 2-Amino-2-methyl-1-propanol is called AMP-95 for short. It is white crystal or colorless viscous liquid, miscible with water and soluble in ethanol. AMP-95 is a well-known multifunctional additive widely used in industries such as coating ink, metalworking fluid, personal care and pharmaceutical intermediates. As a primary amine, AMP-95 has a higher pH value due to its high pKa value. At the same time, because it is an organic base, it is relatively soft and has good compatibility with various emulsions. The performance impact is minor. Compared with other organic bases such as ammonia, trimethylamine, and triethylamine, AMP-95 has good stability, is not easy to yellow, and has low toxicity and is not volatile. It can reduce the odor of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C215/08
CPCC07C201/06C07C201/12C07C213/02C07C215/08C07C205/02C07C205/15
Inventor 杨海玉黄春龙朱红军
Owner GUANGZHOU YINTIAN NEW MATERIAL CO LTD
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