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Resource utilization method of residual kettle tar in phenylenediamine production

A phenylenediamine and resource-based technology, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of non-reuse of aromatic amine structural substances, environmental pollution by toxic and harmful gases, and waste of resources. Achieve the effects of rich acidic oxygen-containing groups, efficient resource utilization and reasonable pore structure

Active Publication Date: 2019-01-11
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of tar has a high nitrogen content and is viscous. There is no good treatment method at present, and most of them are still treated by direct incineration. The disadvantage of this treatment method is that the incineration process produces a large amount of toxic and harmful gases to pollute the environment, which does not meet the current environmental protection and environmental protection requirements. The general trend of cleaner production; in addition, a large number of aromatic amine structure substances in the waste residue have not been reused, resulting in a great waste of resources

Method used

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  • Resource utilization method of residual kettle tar in phenylenediamine production
  • Resource utilization method of residual kettle tar in phenylenediamine production
  • Resource utilization method of residual kettle tar in phenylenediamine production

Examples

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Embodiment 1

[0027] A method for resource utilization of residual tar in the production of phenylenediamine, using the residual tar in the distillation still in the production process of phenylenediamine as a carbon source and a nitrogen source, wherein the nitrogen content of the residual tar in the still is 15%, and its characteristics for, including the following steps:

[0028] (1) Add 300g of kettle residual tar, 0.3g of acetic acid, and 150g of magnesium acetate into a reaction kettle equipped with a microwave device and a capacity of 1000mL, pass in compressed air, heat up and stir under 500W microwave irradiation conditions for stabilization pretreatment, The stirring speed is 1000rpm to obtain a compound in which the carbon precursor / template precursor is mixed uniformly;

[0029] (2) Transfer the above compound to a tubular atmosphere furnace, and carry out carbonization in the presence of high-purity nitrogen according to the following temperature program: the heating rate is 1°...

Embodiment 2

[0033] Using the same phenylenediamine rectification still residual tar as the carbon source and nitrogen source in Example 1, and using the same pretreatment method as in Example 1 to carry out the stabilization pretreatment to the residual tar in the still, the only difference is No template precursor is added; the stabilized pretreated residual tar is directly transferred to the tubular atmosphere furnace, and is carbonized according to the temperature program in the presence of high-purity nitrogen. The flow rate of the protective atmosphere, the heating rate, the maximum carbonization temperature and The carbonization temperature maintenance time is completely consistent with that in Example 1, and the carbonized product is treated with the same method as in Example 1 for template removal, and the obtained carbide is marked as N-C-1.

[0034] Using N-C-1 as the adsorbent, use the same method as step (3) in Example 1 to remove the aniline in the water produced by the hydrog...

Embodiment 3

[0036] Using the same preparation method as C-1 in Example 2, after the carbonization process was completed, water vapor was introduced for high-temperature activation, the steam flow rate was 20mL / min, the activation temperature was 850°C, and the activation time was 5hr. The resulting finished catalyst is designated N-AC-1.

[0037] Using N-AC-1 as the adsorbent, use the same method as step (3) in Example 1 to remove the aniline in the water generated by the hydrogenation reaction of mixed dinitrobenzene, and after a single adsorption, the aniline in the water phase The concentration of aniline decreased from 2000ppm to about 410ppm, and the removal rate of aniline was 79.5%.

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Abstract

The invention relates to the technical field of phenylenediamine production, and particularly discloses a resource utilization method of residual kettle tar in phenylenediamine production. The resource utilization method uses the residual tar in the rectification kettle in phenylenediamine production as a carbon source and a nitrogen source, and is characterized in that the residual tar in the kettle, an auxiliary agent and a templating agent precursor are added to an autoclave, a stabilization pre-treatment is performed under a microwave condition in a heating manner to obtain a carbon precursor / templating agent precursor mixture, the obtained mixture is transferred to a tubular atmosphere furnace, carbonization is performed, the obtained product is added to an acid solution to remove thetemplate, washing is performed to achieve a neutral pH value, drying is performed to obtain mesoporous carbon, the aniline in the water generated by a mixed dinitrobenzene hydrogenation reaction is subjected to adsorption removal by using the mesoporous carbon as an adsorbent, and the mesoporous carbon achieving the saturated adsorption is treated so as to recycled. According to the present invention, the prepared mesoporous carbon has characteristics of reasonable pore channel structure, high mesoporosity, rich acidic oxygen-containing groups on the carbon surface, and excellent adsorption effect on aniline-based weakly-basic aromatic ring organic substances; and the treatment method is environmentally friendly, and no additional pollutants are discharged.

Description

(1) Technical field [0001] The invention relates to the technical field of phenylenediamine production, in particular to a method for resource utilization of residual tar in the production of phenylenediamine. (2) Background technology [0002] Phenylenediamine is an important class of dye intermediates, widely used in the synthesis of various basic dyes, mordants, color developers, aromatic amine curing agents, and the preparation of high-performance new materials such as aramid 1313 and 1414 . [0003] The catalytic hydrogenation method of dinitrobenzene is the main production method of phenylenediamine at present. The technical process can be briefly described as follows: using benzene as the initial raw material, the mixed dinitrobenzene is prepared by nitration reaction in the presence of mixed acid (nitric acid / sulfuric acid) Dinitrobenzene (m-dinitrobenzene, o-dinitrobenzene, p-dinitrobenzene); mixed dinitrobenzene is prepared by catalytic hydrogenation reaction in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18B01J35/02B01J35/10B01J37/08C07C209/86C07C211/46B01J35/00
CPCC07C209/86B01J21/18B01J37/082B01J35/40B01J35/618B01J35/617B01J35/643B01J35/638B01J35/613B01J35/615B01J35/635B01J35/633B01J35/647C07C211/46
Inventor 丁军委于文龙于世涛刘福胜
Owner QINGDAO UNIV OF SCI & TECH
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