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A resource utilization method of waste adsorption resin in resorcinol production

A technology of adsorption resin and resorcinol, which is applied in the field of resource utilization of waste adsorption resin in resorcinol production, can solve the problems of large water treatment volume, no treatment plan, limited number of resin regeneration, etc., and achieve material saving Cost, reasonable pore structure, and excellent adsorption effect

Active Publication Date: 2021-03-09
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The macroporous adsorption resin saturated by organic impurities can be regenerated by solvent elution, and the regenerated macroporous adsorption resin can recover a certain degree of adsorption capacity; however, the regeneration times of the resin are limited. When the resin cannot pass the regeneration treatment When the effective adsorption performance is restored, the service life will be reached, and it will become a chemical solid waste. There is still no good treatment plan.
However, due to the large amount of water treatment in the production of resorcinol, the amount of waste resin recycled and eliminated every year is huge

Method used

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  • A resource utilization method of waste adsorption resin in resorcinol production
  • A resource utilization method of waste adsorption resin in resorcinol production
  • A resource utilization method of waste adsorption resin in resorcinol production

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Take 200g of the macroporous adsorption resin microspheres discarded in the post-treatment process of the resorcinol hydrolyzate, add 500mL of 20% NaOH aqueous solution for ultrasonic washing, remove soluble impurities, and then wash and dry; add 30 % magnesium acetate solution, the mass ratio of resin to magnesium acetate is 1:1, impregnated under reduced pressure and ultrasonic conditions, and dried in the shade after impregnation to obtain a uniformly mixed material of resin / template precursor; transfer the above material to the tube type In the atmosphere furnace, in the high-purity nitrogen atmosphere, the temperature was raised according to the following program for carbonization: the heating rate was 3°C / min, the maximum carbonization temperature was 800°C; the maximum carbonization temperature was maintained for 1 hr; Wash with deionized water until neutral, filter, and dry to obtain about 110 g of mesoporous carbonized resin microspheres, which are designated as...

Embodiment 2

[0037] Take 200g of the macroporous adsorption resin microspheres discarded in the post-treatment process of resorcinol hydrolyzate, add 500mL20% NaOH aqueous solution for ultrasonic washing, remove soluble impurities, and then wash and dry; the above-mentioned dried resin is directly transferred to In a tubular atmosphere furnace, carbonization was carried out in a high-purity nitrogen atmosphere according to the following temperature program: heating rate 3°C / min, maximum carbonization temperature 800°C; maximum carbonization temperature maintenance time 1hr; about 104g of carbonized resin microspheres were obtained, denoted as CR -1.

[0038] The above-mentioned carbonized resin microspheres were used to fill the adsorption column, and the volume of the packed bed was 100mL. The dynamic adsorption method was used to adsorb and decolorize the raffinate aqueous phase of the m-phenylenediamine hydrolyzate. The flow rate of the upper column liquid was 500mL / hr, and the original ...

Embodiment 3

[0040] Using the same preparation method as CR-1 in Example 2, the only difference is that after the carbonization process is completed, water vapor is introduced into the product for high-temperature activation, the steam flow rate is 10mL / min, the activation temperature is 800°C, and the activation time is 4hr. The obtained carbonized product is designated as ACR-1.

[0041] The above-mentioned carbonized resin microspheres were used to fill the adsorption column, and the volume of the packed bed was 100mL. The dynamic adsorption method was used to adsorb and decolorize the raffinate aqueous phase of the m-phenylenediamine hydrolyzate. The flow rate of the upper column liquid was 500mL / hr, and the original COD of the aqueous phase It was 8000mg / L, and after continuous treatment of 2L of water phase, the COD of the effluent was measured to be 160mg / L.

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Abstract

The invention relates to the field of resource utilization of waste adsorption resins, and particularly discloses a method for resource utilization of waste adsorption resins in resorcinol production. The resource utilization method takes the discarded macroporous adsorption resin microspheres in the post-treatment process of resorcinol hydrolyzate as the processing object, and is characterized in that: it is subjected to ultrasonic cleaning treatment, washed with water and dried, and then added with a solution of template agent precursor Impregnate, then dry in the shade to obtain a uniform mixture of resin / template precursor; then heat up and carbonize, and then add an acid solution to remove the template agent to obtain a mesoporous carbonized resin as an adsorbent, and the raffinate of m-phenylenediamine hydrolyzate phase for adsorption and decolorization, and the saturated mesoporous carbonized resin is regenerated and recycled. The invention is green and environmentally friendly, has no additional pollutant discharge, and the required raw materials can be recycled without causing waste of resources; the prepared mesoporous carbonized resin has a reasonable pore structure, and the adsorption effect on macromolecular aromatic ring organic substances is better than that of traditional activated carbon .

Description

[0001] (1) Technical field [0002] The invention relates to the field of resource utilization of waste adsorption resins, in particular to a method for resource utilization of waste adsorption resins in resorcinol production. [0003] (2) Background technology [0004] Resorcinol is an important chemical intermediate widely used in the dye industry, plastic industry, medicine and rubber industry. The hydrolysis method of m-phenylenediamine is one of the main production methods of resorcinol at present. ℃) to generate resorcinol through hydrolysis reaction, and the hydrolyzed solution is strongly acidic after the reaction; use organic extractants (esters, ketones, ethers, alcohols, etc.) to extract the resorcinol in the hydrolyzed solution, The resorcinol product is obtained through desolventization and rectification and refining, and the raffinate water phase needs to undergo decolorization and impurity removal after adjusting the pH to neutral to obtain a relatively pure aqu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/20B01D15/20B01J20/30
CPCB01D15/203B01J20/041B01J20/06B01J20/20
Inventor 于文龙丁军委刘福胜于世涛
Owner QINGDAO UNIV OF SCI & TECH