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A kind of method of recycling iso-terephthaloyl dichloride still residue

A technology of terephthaloyl chloride residue and resource utilization, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of waste of resources, environmental impact, low product purity and yield, etc. The process is simple, the effect of reducing the residual amount of the kettle and improving the product quality

Active Publication Date: 2022-06-07
NINGXIA RUITAI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This application provides a method for resourceful utilization of m-terephthaloyl chloride still residues, which solves the problem that the traditional m-terephthaloyl chloride production cannot process the still residues, resulting in waste of resources, and the impact of transshipment treatment on the environment , and the problem of low product purity and yield

Method used

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  • A kind of method of recycling iso-terephthaloyl dichloride still residue
  • A kind of method of recycling iso-terephthaloyl dichloride still residue
  • A kind of method of recycling iso-terephthaloyl dichloride still residue

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Put 500g terephthaloyl chloride rectification still residue (containing 75% terephthaloyl chloride, 10% terephthalic acid monochloride, 10% tar, 5% terephthalic acid) into a 1000mL four-neck flask, under negative pressure Decoking is carried out at 1KPa; when the temperature / kettle temperature is 102°C / 104°C, the material is discharged until the kettle temperature is 160°C, and the decoking is completed; Add 152g of chlorobenzene and stir at 50°C, stir for 2 hours and then slightly cool down to 30°C and perform suction filtration to obtain 30g of wet-base filter cake (26g after drying), 198g of filtrate to remove the solvent chlorobenzene under negative pressure, and the residue of the precipitation kettle 52g, and 144g of recovered solvent; the residual amount of the distillation still is reduced by 89.6% after the treatment.

[0052] The decoking discharge and filter cake in the previous step are reused in the acid chloride synthesis process, and the product is obtain...

Embodiment 2

[0054] Put 500g isophthaloyl chloride rectifying still residue (containing 72% isophthaloyl chloride, 10% isophthalic acid monochloride, 12% tar, 6% isophthalic acid) into a 1000mL four-necked flask, under negative pressure Decoking is carried out at 2KPa; when the temperature / kettle temperature is 104°C / 106°C, the material is discharged until the kettle temperature is 170°C, and the coking is completed; 136.5g of chlorobenzene was added and stirred at 60°C. After stirring for 3 hours, the temperature was slightly lowered to 30°C and suction filtration was performed to obtain 35g of wet-base filter cake (30.5g after drying). The residue in the still is 61 g, and 130 g of the solvent is recovered; the residue in the distillation still is treated and the residue in the still is reduced by 87.8%.

[0055] The decoking discharge material and the filter cake in the previous step are reused in the acid chloride synthesis process, and the product is obtained after desolubilization an...

Embodiment 3

[0057] Put 500g terephthaloyl chloride rectification still residue (containing 60% terephthaloyl chloride, 13% terephthalic acid monochloride, 20% tar, 7% terephthalic acid) into a 1000mL four-neck flask, under negative pressure Decoking is carried out at 2KPa; when the temperature / kettle temperature is 110°C / 113°C, the material is discharged until the kettle temperature is 170°C, and the decoking is completed; Add 408g of thionyl chloride and stir at 30°C, and after stirring for 1 hour, perform suction filtration to obtain 42g of wet-based filter cake (35.5g after drying), 501g of filtrate to remove the solvent at normal pressure, and 100.5g of the remaining 100.5g of the precipitation tank to be recovered. Solvent 400g; after the rectification still residue is treated, the still residue is reduced by 79.9%.

[0058] The decoking discharge material and the filter cake in the previous step are reused in the acid chloride synthesis process, and the product is obtained after des...

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Abstract

This application discloses a method for resource utilization of m- and terephthaloyl dichloride still residues, comprising the following steps: S1, obtaining rectification still residues through acyl chloride synthesis process, and decoking the rectification still residues at 1-10KPa , the decoking discharge material contains 90% diacid chloride, 8‑10% monoacyl chloride, which is reused in the acid chloride synthesis process; After dissolving in a solvent for 1-6 hours, the solvent dissolving temperature is at least 10°C to obtain a solution, and then filter the solution to obtain a filtrate and a filter cake. The filter cake is mainly raw material phthalic acid recycled to the acyl chloride synthesis process. The process of the invention is easy to operate, and the effective components in the hazardous solid waste are fully utilized, and the refractory solid waste is used as a raw material for the synthesis of acyl chlorides to prepare products, and at the same time, the monoacyl chlorides enriched in the solid wastes are acyl chlorinated to synthesize phthalidine Acyl chlorides reduce the amount of monoacyl chlorides in the rectification system from the source and greatly improve product quality. The method realizes the dual purposes of emission reduction and income increase, and is economical and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of chemical production waste treatment, in particular to a method for resource utilization of m-terephthaloyl chloride residues. Background technique [0002] Meta and terephthaloyl chloride is an important organic synthesis intermediate, mainly used for the preparation of poly-p-phenylene isophthalamide (referred to as Aramid 1313) and poly-p-phenylene terephthalamide (referred to as poly-p-phenylene terephthalamide). Aramid 1414); in addition, it is also widely used in the synthesis of materials and pesticides; among them, aramid is a high-tech synthetic fiber with excellent properties such as ultra-high strength, high modulus, acid resistance, alkali resistance, and light weight, and is widely used. In composite materials, building materials, special protective clothing and military fields. As one of the important raw materials for the synthesis of aramid fiber, the quality of m-terephthaloyl chloride is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/60C07C51/64C07C63/30
CPCC07C51/60C07C51/64C07C63/30
Inventor 朱斌严绘石苏洋亢玉荣刘勇王明晨
Owner NINGXIA RUITAI TECH
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