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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 good industrial applicability, low cost and simple operation

Active Publication Date: 2018-12-11
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Preparation method of 2-nitro-2-methyl-1-propanol crystal
  • Preparation method of 2-nitro-2-methyl-1-propanol crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 4000g of 2-nitropropane, 40g of methanol and 50g of 5mol / L NaOH aqueous solution into the reactor, stir and heat to 55℃, then add 95% formaldehyde to the reactor within 2 hours After adding 1516 g of paraformaldehyde, the temperature was raised to 65° C. and kept for 0.5 hour, so as to react to produce a reaction liquid containing 2-nitro-2-methyl-1-propanol. The reaction conversion rate based on 2-nitropropane was 99.7%, and the selectivity of 2-nitro-2-methyl-1-propanol was 99.7%.

[0044] 5300g of methanol was added to the reaction solution to prepare a methanol solution, after which the alkali was removed by the acid purification resin, and then passed through a reactive distillation column equipped with a strong acid ion exchange resin (reaction conditions were the temperature at the bottom of the tower and the temperature at the top 50℃, reflux ratio is 6:1, pressure is normal pressure) to remove formaldehyde. The above-mentioned aldehyde-removing solution was t...

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℃, and then add 95% formaldehyde to the reactor within 2 hours 1488 g of paraformaldehyde, after the addition, the temperature was raised to 70° C. and kept for 0.5 hours, thereby reacting to produce a reaction liquid containing 2-nitro-2-methyl-1-propanol. The reaction conversion rate based on 2-nitropropane is 99.5%, and the selectivity of 2-nitro-2-methyl-1-propanol is 99.6%.

[0047] 5823g of methanol was added to the reaction solution to prepare a methanol solution, after which the alkali was removed by the acid purification resin, and then passed through a reactive distillation tower equipped with a strong acid ion exchange resin (reaction conditions were 69°C at the bottom of the tower and temperature at the top 52℃, reflux ratio is 5:1, pressure is normal pressure) to remove formaldehyde. The above-mentioned aldehyde-removing solution was transf...

Embodiment 3

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

[0050] 6100g of methanol was added to the reaction solution to prepare a methanol solution, then the triethylamine was removed by the acid purifying resin, and then passed through a reactive distillation tower equipped with a strong acid ion exchange resin (reaction conditions were at the bottom of the tower at 68°C, the tower 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 removal s...

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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 method for preparing 2-nitro-2-methyl-1-propanol crystals. The final yield is used to prepare high-purity products. 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) from Angus Company in the United States is based on 2-nitro-2-methyl-1-propanol. It is 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. However, the problem is that the yield during the synthesis of NMP is low ( <97%), and there will be a small amount of salt and a large amount of incompletely reacted formaldehyde remaining in the NMP, which will affect the product quality. [0003] The US ...

Claims

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Application Information

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Patent Type & Authority Applications(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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