Method for preparing carbon-based acid material by means of alkylated waste acid

A technology for alkylating waste acids and acidic materials, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of long preparation time, many preparation procedures, and low oxidation efficiency, and achieve Reduced energy consumption, reduced reaction steps, and wide-ranging effects

Active Publication Date: 2018-03-06
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common problem of this method is that the oxidation efficiency is not high and the cost is high;
When p-toluenesulfonic acid and sulfamic acid catalyze organic reactions, they are easy to dissolve in water and become liquid acid catalysts, which have the disadvantages of difficult separation, strong corrosion, and serious pollution.
Sulfonic acid resin has low temperature resistance, and the silicon-based solid sulfonic acid obtained by silanization and oxidation on silicon-based materials takes a long time to prepare and is cumbersome to operate
Biomass charcoal uses biomass carbonized by sulfuric acid, and then sulfonated by sulfonating agent to produce solid sulfonic acid, which has the disadvantages of many preparation procedures and high cost.

Method used

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  • Method for preparing carbon-based acid material by means of alkylated waste acid
  • Method for preparing carbon-based acid material by means of alkylated waste acid
  • Method for preparing carbon-based acid material by means of alkylated waste acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0026] Weigh a certain amount of waste acid in a round bottom flask (250ml), raise it from room temperature to 160°C, then maintain it for 5h, cool to room temperature, weigh 150% of the waste acid mass in water and add it to the round bottom flask. Stir overnight, filter with suction, obtain filtrate (dilute sulfuric acid solution) and filter cake (carbon-based acidic material), collect filtrate in the beaker, add ammoniacal liquor (25-28wt%) slowly under the condition of stirring, until the solution is neutral properties, and then the solution was evaporated, and crystals were precipitated. The filter cake was washed with deionized water until neutral, dried, and the sulfur content was detected by elemental analysis. Test the COD value of filtrate, the results are as shown in table 1:

[0027] Table 1

[0028]

Embodiment example 2

[0030] Weigh a certain amount of spent acid in a round-bottomed flask (250ml), raise it from room temperature to 180°C, then maintain it for 5h, cool to room temperature, weigh 200% of the spent acid mass in water and add it to the round-bottomed flask. Stir overnight, and filter with suction to obtain filtrate (dilute sulfuric acid solution) and filter cake (carbon-based acidic material), collect the filtrate into a beaker, rotate to obtain concentrated sulfuric acid, and titrate to measure the concentration of sulfuric acid. The filter cake was washed with deionized water until neutral, dried, and the sulfur content was detected by elemental analysis. Test the COD value of filtrate, the results are as shown in table 2:

[0031] Table 2

[0032]

Embodiment example 3

[0034] Take a certain amount of waste acid and carbon-based acidic material in a round bottom flask (250ml), raise it from room temperature to 160°C, then maintain it for 4h, cool to room temperature, weigh 100% water of the waste acid mass and add it to the round bottom flask Bottom flask, stirred overnight at room temperature, filtered with suction to obtain filtrate (dilute sulfuric acid solution) and filter cake (carbon-based acidic material). Collect the filtrate into a beaker, slowly add ammonia water (25-28wt%) under the condition of stirring until the solution is neutral, then evaporate the solution, and crystals are precipitated. The filter cake was washed with deionized water until neutral, dried, and the sulfur content was detected by elemental analysis. Test the COD value of filtrate, the results are as shown in table 3:

[0035] table 3

[0036]

[0037]

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Abstract

The invention relates to a method for preparing a carbon-based acid material by means of alkylated waste acid. The method comprises the following steps that the alkylated waste acid is heated to reachthe temperature of 100-500 DEG C, the temperature is kept for 1-10 h, products are washed to be neutral with a solvent, drying is conducted at 60-200 DEG C, and the carbon-based acid material is obtained, wherein the solvent obtained after washing basically does not contain organic matter, and the solvent is at least one of water, dilute sulfuric acid, ammonium hydroxide and ammonium sulfate. Themethod for preparing the carbon-based acid material is short in process route, small in investment, easy to operate, low in running cost and wide in application range, resource recycling of acid soluble oil and sulfuric acid in waste sulfuric acid can be achieved, and carbon emission is reduced.

Description

technical field [0001] The invention relates to a method for preparing carbon-based acidic material by using alkylation waste acid, in particular, using acid-soluble oil in waste sulfuric acid which is produced by reacting isobutane and olefin to generate alkylated oil to prepare carbon-based acidic material. technical background: [0002] Waste sulfuric acid is produced in the production process of fine chemical products such as nitration, sulfonation, alkylation and esterification of organic matter, as well as in mineral processing, petroleum refining, national defense industry, etc. According to estimates, the amount of waste sulfuric acid produced every year is More than 100 million tons. Waste sulfuric acid has always been a major problem for production enterprises. If the country's environmental protection policies and precursor chemicals management regulations are strictly followed, most domestic enterprises that produce waste sulfuric acid will be shut down. Since ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J31/02
CPCB01J27/02B01J31/0225
Inventor 周志茂杨飞飞张锁江戴力
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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