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A kind of preparation method of 2-nitro-2-methyl-1-propanol crystal

A technology of nitropropane and methyl, which is applied in the field of synthesis of 2-nitro-2-methyl-1-propanol, can solve problems such as undisclosed salt and formaldehyde treatment methods, affecting product quality, and formaldehyde residues. Achieve the effect of good industrial applicability, low cost and simple operation

Active Publication Date: 2021-03-02
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yet, the problem that exists is, in the synthetic process of NMP, yield is low (<97%), and there will be a small amount of salt and a large amount of incompletely reacted formaldehyde residues in NMP, influence product quality
However, the patent does not disclose the treatment method of residual salt and formaldehyde in the product

Method used

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  • A kind of preparation method of 2-nitro-2-methyl-1-propanol crystal
  • A kind of preparation method of 2-nitro-2-methyl-1-propanol crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Add 4000g of 2-nitropropane, 40g of methanol and 50g of 5mol / L NaOH aqueous solution into the reaction kettle, stir and heat to 55°C, and then add formaldehyde content of 95% to the reaction kettle within 2 hours 1516g of paraformaldehyde was added, and after the addition, the temperature was raised to 65° C. and kept for 0.5 hours, thereby reacting to generate a reaction liquid containing 2-nitro-2-methyl-1-propanol. The reaction conversion based on 2-nitropropane was 99.7%, and the selectivity of 2-nitro-2-methyl-1-propanol was 99.7%.

[0044] Add the methyl alcohol of 5300g in the reaction liquid and be made into methanol solution, then by acid purification resin alkali is removed, then pass through the reaction rectification tower (reaction condition is tower bottom temperature 70 ℃, tower top temperature) that strong acid ion exchange resin is housed 50°C, the reflux ratio is 6:1, and the pressure is normal pressure) to remove formaldehyde. The above-mentioned ald...

Embodiment 2

[0046] Add 4000g of 2-nitropropane, 10g of methanol and 50g of 5mol / L KOH aqueous solution into the reactor, stir and heat to 60°C, and then add formaldehyde content of 95% to the reactor within 2 hours. After the addition of 1488g of paraformaldehyde, the temperature was raised to 70°C and kept for 0.5 hours to react to generate a reaction solution containing 2-nitro-2-methyl-1-propanol. The reaction conversion based on 2-nitropropane was 99.5%, and the selectivity of 2-nitro-2-methyl-1-propanol was 99.6%.

[0047] Add the methyl alcohol of 5823g in the reaction liquid and be made into methanol solution, then by acid purification resin alkali is removed, then pass through the reaction rectification tower (reaction condition is tower bottom temperature 69 ℃, tower top temperature) that strong acid ion exchange resin is housed 52°C, the reflux ratio is 5:1, and the pressure is normal pressure) to remove formaldehyde. The above-mentioned aldehyde-removing solution was transferr...

Embodiment 3

[0049] Add 4000g of 2-nitropropane, 30g of methanol and 40g of triethylamine into the reactor, stir and heat to 55°C, then add 1487g of paraformaldehyde with a formaldehyde content of 95% to the reactor within 1.5 hours After the addition, the temperature was raised to 63° C. and kept for 1 hour, so that the reaction solution containing 2-nitro-2-methyl-1-propanol was generated. The reaction conversion based on 2-nitropropane was 99.1%, and the selectivity of 2-nitro-2-methyl-1-propanol was 99.9%.

[0050] Add 6100g of methanol to the reaction solution to form a methanol solution, then triethylamine is removed by an acidic purification resin, and then passed through a reactive distillation tower equipped with a strong acidic ion exchange resin (reaction conditions are 68 ° C at the bottom of the tower, and The top temperature is 54°C, the reflux ratio is 4:1, and the pressure is normal pressure) to remove formaldehyde. The above-mentioned aldehyde-removing solution is transfe...

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Abstract

The invention provides a preparation method of a 2-nitro-2-methyl-1-propanol crystal. According to the method, 2-nitro-2-methyl-1-propanol is prepared through a reaction between 2-nitropropane and paraformaldehyde, the residual formaldehyde is removed with an acidic solid catalyst, and the product is subjected to secondary purification with cyclohexane so as to obtain the 2-nitro-2-methyl-1-propanol crystal, wherein the purity is up to 99.8-99.99%, and the residual formaldehyde is 5-200 ppm; and the conversion rate of the reaction based on 2-nitropropane can be 98-99.7%, and the final yield after the secondary purification is 90-97%.

Description

technical field [0001] The present invention relates to the synthesis of 2-nitro-2-methyl-1-propanol, in particular to a preparation method of 2-nitro-2-methyl-1-propanol crystals, the method can be higher Final yield to prepare high purity product. Background technique [0002] 2-nitro-2-methyl-1-propanol (NMP) is an important raw material for organic synthesis. The multifunctional additive AMP-95 (95% aqueous solution of 2-amino-2-methyl-1-propanol) of American Angus company is exactly to be raw material with 2-nitro-2-methyl-1-propanol, Prepared by catalytic hydrogenation reduction. According to the existing method, NMP is prepared by condensation reaction of 2-nitropropane (2-NP) and formaldehyde under the action of a basic catalyst. Yet, the problem that exists is, in the synthetic process of NMP, yield is low (<97%), and there will be a small amount of salt and a large amount of incompletely reacted formaldehyde residues in NMP, influence product quality. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/12C07C205/15C07C201/16
CPCC07C201/12C07C201/16C07C205/15
Inventor 张英伟张绍岩王耀红王朋陈玉坤
Owner BEIJING RISUN TECH CO LTD
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