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Treatment method of O-xylene liquid phase oxidation residues

A treatment method and xylene liquid technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of waste of non-renewable resources, complex components, environmental pollution, etc., and achieve obvious industrial advantages and reaction conditions Mild, utilization-enhancing effect

Active Publication Date: 2016-12-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And these solid residues are highly acidic, and direct disposal methods such as landfills will cause serious environmental pollution. In the industry, the incineration method is usually used for disposal. Although this method solves environmental problems, it also wastes a large amount of non-renewable resources. Necessary to improve
The composition of these solid residues is complex, and the content of various components varies greatly with the fluctuation of oxidation conditions, so it is not meaningful to recover a certain component alone

Method used

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  • Treatment method of O-xylene liquid phase oxidation residues
  • Treatment method of O-xylene liquid phase oxidation residues

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Effect test

Embodiment 1

[0020] Such as figure 1 As shown, weigh 100g o-xylene oxidation solid residue, add 200g dimethyl phthalate, 100g methanol, 5g 98% concentrated sulfuric acid, react in an autoclave at 150°C for esterification and dissolution process, the pressure is 1.5Mpa , the reaction time is 5h. After the process is over, the liquid is mixed crude ester after solid-liquid separation, and the mass of the remaining oxidized solid residue after drying is 43.8g. It can be calculated that the removal rate of oxidized residue is 56.2%. The mixed crude esters enter the neutralization step, add 40mL of 5% NaOH solution to stir and neutralize, and then divide the water. The mixed crude esters after water division are neutral, and then enter the rectification process, and the low boiling The low boilers obtained are mainly unreacted methanol, which can be mixed with phthalates and recycled as reactants of the esterification reaction. The bottom of the tower is the obtained mixed ester, which can ent...

Embodiment 2-7

[0022] The reaction process of Example 1 was repeated, except that different solvents, catalysts and reaction conditions were used. The specific raw material reaction conditions and results of each embodiment are listed in Table 1.

[0023] Table 1

[0024]

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Abstract

The invention discloses a treatment method of O-xylene liquid phase oxidation residues. The method comprises the following steps of adding phthalate, or O-methyl benzoate or a mixture of the phthalate and the O-methyl benzoate to oxidation residues, and performing catalysing, dissolving and esterifying on a catalyst with low carbon and alcohol and low catalysis quantity so as to obtain mixed crude ester; and recovering most of solid residues, so that 50% or above of discharged solid waste can be reduced. After refining, the crude ester can be used as an o-xylene liquid phase oxidation solvent to return to an oxidation tower for use. According to the method, the o-xylene liquid phase oxidation residues are comprehensively used, so that the discharged solid waste is greatly reduced, and recycling of industrial waste residue is realized.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a treatment method for liquid-phase oxidation residue of o-xylene. Background technique [0002] Phthalate esters are important plasticizers, currently mainly obtained by esterification of o-xylene oxidation products (phthalic acid, phthalic anhydride). Among them, the esterification of phthalic anhydride through gas-phase oxidation of o-xylene is currently the main process route, but this route has disadvantages such as high reaction temperature and low yield, and has been gradually replaced by liquid-phase oxidative esterification technology of o-xylene in recent years. However, the liquid-phase oxidation of o-xylene to prepare phthalic acid will produce a large amount of aromatic acid residues, the main components of which include phthalic acid, terephthalic acid, phthalic acid, benzoic acid, methylbenzoic acid, O-carboxybenzaldehyde, etc. And these solid re...

Claims

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Application Information

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IPC IPC(8): C07C67/56C07C67/60C07C67/48C07C69/76
Inventor 徐杰孙颖高进石松苗虹徐永明
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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