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Method for preparing purified acid from waste-acid after benzene refinery

A technology of refined benzene and sulfuric acid, applied in sulfur trioxide/sulfuric acid, liquid solution solvent extraction, etc., can solve the problems of difficult industrial application, complex process, high cost, and achieve the effect of solving environmental protection problems, simple process and easy separation

Inactive Publication Date: 2007-04-11
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the above studies have all made progress to varying degrees, the cost of purifying waste acid from benzene increases due to the use of admixtures or ANPA; or the use of NaOH to neutralize and generate sodium phenolate, and then use 30% sulfuric acid to decompose the phenate to obtain crude phenol , the process is complicated, the cost is high, and the recovery rate of sulfuric acid is low;

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 Weigh a certain amount of refined benzene spent acid, add ammonium sulfate mother liquor, heat to 70-80°C, and then add crude phenol. The weight ratio of the above added substances is: spent refined benzene acid / ammonium sulfate mother liquor / crude phenol is 100 / 10-20 / 20-30. Then heat to 90-110°C, stir for 10-12 minutes, and let stand for 1-3 hours to separate layers. The upper layer is the mixed solution of the extraction phase, and the lower layer is the purified sulfuric acid. Purified sulfuric acid is transparent and light in color, and can be used in the production of ammonium sulfate. The recovery rate of purified sulfuric acid is over 98%.

[0016] Then neutralize the upper extract phase mixture with ammonia water, add 2% washing oil, and recover the extractant by distillation. The extractant can be reused, and the distillation residue is used for coal blending and coking.

Embodiment 2

[0017] Example 2 Weigh a certain amount of refined benzene waste acid, add ammonium sulfate, heat to 70-80°C, and then add crude phenol. The weight ratio of the above additions is: waste refined benzene acid / ammonium sulfate / crude phenol is 100 / 5-15 / 20-40. Then heat to 100-110°C, stir for 12-15 minutes, and let stand for 1-3 hours to separate layers. The upper layer is the mixed solution of the extraction phase, and the lower layer is the purified sulfuric acid. Purified sulfuric acid is transparent and light in color, and can be used in the production of ammonium sulfate. The recovery rate of purified sulfuric acid is over 98%.

[0018] Then neutralize the upper extract phase mixture with ammonia water, add 2-3% washing oil, and distill and recover the extractant. The extractant can be reused, and the distillation residue is used for coal blending and coking.

Embodiment 3

[0019] Example 3 Weigh a certain amount of refined benzene waste acid, add ammonium sulfate mother liquor, heat to 70-80°C, and then add dephenolized phenol oil. The weight ratio of the above added substances is: waste refined benzene acid / ammonium sulfate mother liquor / dephenolized phenol oil is 100 / 20-40 / 20-40. Then heat to 100-110°C, stir for 12-15 minutes, and let stand for 1-3 hours to separate layers. The upper layer is the mixed solution of the extraction phase, and the lower layer is the purified sulfuric acid. Purified sulfuric acid is transparent and light in color, and can be used in the production of ammonium sulfate. The recovery rate of purified sulfuric acid is over 98%.

[0020] Then neutralize the upper extract phase mixture with sodium carbonate, add 3% anthracene oil, and recover the extractant by distillation. The extractant can be reused, and the distillation residue is used for coal blending and coking.

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Abstract

A process for preparing high-purity acid from the used acid generated by preparing refined benzene includes such steps as adding the salting-out agent to said used acid, heating while adding extractant, stirring at constant temp, laying aside for layering, taking the lower layer (high-purity acid), neutralizing upper layer by alkali, and distilling while adding organic solvent to obtain regenerated extractant.

Description

1. Technical field [0001] The invention belongs to the technology of refining and recovering crude benzene washed with sulfuric acid in a coking plant. In particular, it relates to a method for preparing purified acid from coking refined benzene waste acid. 2. Background technology [0002] In the process of producing refined benzene by pickling method, a large amount of waste acid will be produced, which contains tar-like sulfonic acid, glycolic acid, acetoformaldehyde resin, naphthalene, anthracene, phenol, styrene, indene, thiophene, etc. The substance is a black liquid containing 40-60% sulfuric acid. There is no effective recovery and utilization method at present. It often directly enters the external drainage system, which not only causes serious water pollution, but also wastes precious sulfuric acid resources, which has become an environmental protection problem for many coking plants. [0003] In recent years, coking plants at home and abroad have done a lot of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/90C01B17/92B01D11/04
Inventor 李其祥史世庄刘智平童仕唐
Owner WUHAN UNIV OF SCI & TECH
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