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Method for preparing isooctyl nitrate by recovering waste acid

A technology of isooctyl nitrate and nitric acid, applied in the field of waste acid recycling to prepare isooctyl nitrate, can solve the problems of low conversion rate, unsatisfactory catalytic effect and the like

Pending Publication Date: 2020-01-14
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing isooctyl nitrate by recycling waste acid. The method in the present invention solves the problem that the concentration of waste acid directly causes low conversion rate and unsatisfactory catalytic effect, and converts waste acid into isooctyl nitrate. The raw material of octyl ester reduces the cost of waste acid treatment, and at the same time reuses the nitric acid in the waste acid to reduce the unit consumption of nitric acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Take 1000g of waste acid, check the content of sulfuric acid to be 83%, and the content of nitric acid to be 5%, and use sulfuric acid with a concentration of 98% to mix evenly according to 1:1, and the content of sulfuric acid and nitric acid to be 2.5%.

[0043] Use this acid and nitric acid according to the ratio of 1:1 to adjust and form a mixed acid under the protection of nitrogen. The molar ratio of sulfuric acid and nitric acid in the mixed acid is 0.58:1. The nitric acid and isooctyl alcohol (content 99.5%) in the mixed acid enter the microchannel reactor according to the molar ratio of 2:1, and react at 50°C for 50s.

[0044] The reacted sample is layered, and the acid phase is separated, and the separated acid phase is reused in the raw material waste acid. Adding mass concentration in the organic phase obtained is 97% caustic soda 301g (caustic soda and product mass ratio are 0.12: 1) to carry out neutralization, after filtering, through 829g washing (water ...

Embodiment 2

[0046] Take 1000g of waste acid, check the sulfuric acid content of 83%, and the nitric acid content of 5%, and mix the sulfuric acid with a concentration of 98% at a ratio of 1.7:1. The sulfuric acid content is 92.4%, and the nitric acid content is 1.8%.

[0047] Use this acid and nitric acid in a ratio of 2.5:1 to adjust and mix under nitrogen protection to form a mixed acid. The molar ratio of sulfuric acid and nitric acid in the mixed acid is 1.5:1. Nitric acid and isooctyl alcohol (99.5% content) in the mixed acid enter the microchannel reactor at a molar ratio of 1.8:1, and react at 40° C. for 20 seconds.

[0048] The reacted sample is layered, and the acid phase is separated, and the separated acid phase is reused in the raw material waste acid. In the obtained organic phase, adding mass concentration is 190g of caustic soda (caustic soda and product mass ratio is not 0.15:1) of 97% to carry out neutralization, after filtering, through 385g washing (water and product ma...

Embodiment 3

[0050] Take 1000g of waste acid, check the sulfuric acid content of 83%, and the nitric acid content of 5%, and mix the sulfuric acid with a concentration of 98% according to 2.8:1, and the sulfuric acid content is 94%, and the nitric acid content is 0.8%.

[0051] Use this acid and nitric acid in a ratio of 2:1 to adjust and mix under nitrogen protection to form a mixed acid. The molar ratio of sulfuric acid and nitric acid in the mixed acid is 1.23:1. Nitric acid and isooctyl alcohol (99.5% content) in the mixed acid enter the microchannel reactor at a molar ratio of 1.5:1, and react at 20° C. for 40 seconds.

[0052] The reacted sample is layered, and the acid phase is separated, and the separated acid phase is reused in the raw material waste acid. Add mass concentration in the organic phase that is obtained and be 97% caustic soda 620g (caustic soda and product mass ratio are not 0.17: 1) carry out neutralization, after filtering, through 1500g washing (water and product ...

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Abstract

The invention provides a method for preparing isooctyl nitrate by recovering waste acid. The method comprises: A) adding 98% sulfuric acid into waste acid to obtain waste acid with a sulfuric acid concentration of 90-95%, wherein the mass concentration of the sulfuric acid in the waste acid is 80-85%, and the mass concentration of the nitric acid in the waste acid is 2-6%; B) adding nitric acid into the waste acid with the sulfuric acid concentration of 90-95% to obtain a mixed acid raw material, wherein a mass ratio of the nitric acid in the mixed acid raw material to the waste acid obtainedin the step A) is 1:(1.5-4); and C) pumping the mixed acid raw material and isooctyl alcohol into a micro-channel reactor, and carrying out a reaction to obtain isooctyl nitrate. According to the invention, the product isooctyl nitrate can be prepared by using the waste acid, and no other impurities are introduced, so that the product quality is good; the problem of nitrogen oxide emission pollution caused by post-treatment of nitric acid-containing waste acid is solved; and the nitric acid in the waste acid can be reused so as to reduce the unit consumption of nitric acid.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for preparing isooctyl nitrate by recycling waste acid. Background technique [0002] As an important basic chemical raw material, sulfuric acid is known as the "Mother of Chemical Industry" and is widely used in various fields of industry and agriculture. By the end of 2014, the national sulfuric acid production capacity reached 124 million tons. The consumption of sulfuric acid is mainly divided into two parts: fertilizer acid and industrial acid. In 2015, the apparent consumption of sulfuric acid in my country was 97.7 million tons, a year-on-year increase of 4.1%, of which the acid used in fertilizers accounted for more than 60%. Sulfuric acid is mainly used in nitrification industry, battery industry, chlor-alkali industry, hydrogen fluoride industry, alkylation industry, ion exchange resin industry and pesticide industry. At the same time, the output o...

Claims

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Application Information

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IPC IPC(8): C07C201/02C07C203/04
CPCC07C201/02C07C203/04
Inventor 张超梁万根杨聪马雪菲崔卫华宋吻吻
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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