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Method for recycling sulfuric acid and pivalic acid from byproduct waste acid in pivalic acid synthetic process

A synthesis process, pivalic acid technology, applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, sulfur trioxide/sulfuric acid, etc., can solve the problems of resource waste, non-recycling, environmental pollution, etc., and achieve the goal of eliminating pollution Effect

Inactive Publication Date: 2014-09-24
HEBEI HUAXU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used synthetic method of pivalic acid is the isobutylene carbonyl synthesis method, which uses sulfuric acid as a catalyst, so pivalic acid will produce a waste acid solution containing sulfuric acid and pivalic acid during the synthesis process (the concentration of sulfuric acid in the waste acid is generally ≤65 %), but there is no recycling method at present, which causes waste of resources and pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 5 kg of ethyl acetate to 100 kg of waste acid produced in the pivalic acid synthesis process, stir at room temperature for 4 hours, then leave to separate the layers for 2 hours, and separate the organic phase and the aqueous phase;

[0030] The organic phase is subjected to normal-pressure rectification, ethyl acetate is recovered, and the rest of the rectification liquid is used for subsequent use;

[0031] The water phase is filtered to remove solid impurities to obtain 90L of filtrate, and the obtained filtrate is passed through a macroporous adsorption resin column (the amount of resin is 9L, and the resin skeleton is a styrene system) for adsorption, and the effluent at the bottom of the resin column, i.e. sulfuric acid, is collected. Concentration 60%;

[0032] Add methanol twice the volume of the resin to the macroporous adsorption resin column after the adsorption filtrate to elute, collect the eluate, carry out rectification at atmospheric pressure, recove...

Embodiment 2

[0035] Add 10 kg of ethyl acetate to 100 kg of waste acid produced during pivalic acid synthesis, stir at room temperature for 5 hours, then leave to separate the layers for 3 hours, and separate the organic phase and the aqueous phase;

[0036] The organic phase is subjected to normal-pressure rectification, ethyl acetate is recovered, and the rest of the rectification liquid is used for subsequent use;

[0037] The water phase is filtered to remove solid impurities to obtain 86L of filtrate, which is passed through a macroporous adsorption resin column (the amount of resin is 17.2L, and the resin skeleton is polyvinylidene fluoride) for adsorption, and the effluent at the bottom of the resin column is collected. Namely sulfuric acid, concentration 65%;

[0038] Add ethanol of 2 times the volume of the resin to the macroporous adsorption resin column after the adsorption filtrate to elute, collect the eluate, carry out atmospheric rectification, recover ethanol, and rectify t...

Embodiment 3

[0041] Add 7.5 kg of ethyl acetate to 100 kg of waste acid produced during pivalic acid synthesis, stir at room temperature for 4.5 hours, then leave to separate the layers for 2.5 hours, and separate the organic phase and the aqueous phase;

[0042] The organic phase is subjected to normal-pressure rectification, ethyl acetate is recovered, and the rest of the rectification liquid is used for subsequent use;

[0043] The aqueous phase is filtered to remove solid impurities to obtain 92L of filtrate, and the obtained filtrate is passed through a macroporous adsorption resin column (the amount of resin is 18.4L, and the resin skeleton is an acrylic acid series) for adsorption, and the effluent at the bottom of the resin column, i.e. sulfuric acid, is collected. Concentration 62%;

[0044] Add isopropanol of 2 times the volume of the resin to the macroporous adsorption resin column after the adsorption filtrate to elute, collect the eluent, carry out rectification at atmospheric...

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PUM

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Abstract

The invention provides a method for recycling sulfuric acid and pivalic acid from byproduct waste acid in the pivalic acid synthetic process. The method includes the steps that organic solvents are added into the waste acid for extraction, an organic phase and a water phase are separated, filter liquor obtained after the water phase is filtered passes through large-hole adsorbent resin, obtained flowing-out liquor is the sulfuric acid which is colorless and transparent, organic solvents are added into the large-hole adsorbent resin obtained after the filter liquor passes through the large-hole adsorbent resin for elution, elution liquor is rectified to recycle the organic solvents, and left liquor is rectified for standby application; the organic phase is firstly rectified to recycle the organic solvents, and left liquor is rectified for standby application; the liquor left after the two times of rectification is mixed, then decompression rectification is carried out on the mixed liquid, and the pivalic acid is accordingly obtained. By means of the method, the aim of environment-friendly processing of the waste acid in the pivalic acid production technology is effectively achieved.

Description

technical field [0001] The invention belongs to the technical field of recovery of waste acid, and in particular relates to a method for recovering sulfuric acid and pivalic acid from the by-product waste acid in the synthesis process of pivalic acid. Background technique [0002] Pivalic acid is an important chemical raw material, which can be used to produce pivaloyl chloride as a pharmaceutical intermediate, and further produce ampicillin, amoxicillin, cephalexin, cefazolin, cefradine, cefaclor, etc.; it can also be used to produce important Pesticide intermediate pinazone and herbicide clomazone, etc.; in the perfume industry for the production of soap, shampoo, hair gel additives; in the plastics industry for the production of initiators; in the coatings industry for the production of tertiary carbon paint. [0003] The wide range of applications of pivalic acid requires extensive synthesis. The commonly used synthetic method of pivalic acid is the isobutylene carbony...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C53/128C01B17/90
CPCC01B17/905C07C51/42C07C53/128
Inventor 齐翠国王铁招吴素珍康志军刘玉生陈中强于娜梅
Owner HEBEI HUAXU CHEM
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