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A method for purifying pgmea from pgmea waste liquid

A technology for waste liquid and solid waste, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid esters, etc., can solve the problems of large steam consumption, high treatment cost, and narrow application

Active Publication Date: 2016-01-06
惠州TCL环境科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, some enterprises have done a lot of research on the recycling of PGMEA waste liquid. At present, in the process of PGMEA recycling, the main problems are: 1. Due to the wide source of PGMEA waste liquid, the composition and content are complex and changeable , for PGMEA waste liquid with complex composition and content, the scope of application of a certain set of equipment is narrow; 2. The cost of treatment is high, especially the steam consumption is large

Method used

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  • A method for purifying pgmea from pgmea waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: PGMEA waste liquid, components: PGMEA: 72.66%, PGME: 14%, cyclohexanone 5.27%, moisture 1.52%, and other impurities 6.55%, etc.

[0015] Steps:

[0016] (1) After the waste PGMEA solution is filtered through filter A to remove large solid waste, it enters the raw material settling tank B to remove settleable solid impurities.

[0017] (2) PGMEA waste liquid through filtration and sedimentation enters distillation tower C, adopts 7~

[0018] The 9-meter-high orifice corrugated packing with strong anti-fouling ability, after the distillation kettle is heated by 0.6MPa saturated steam, the vacuum degree is controlled at -0.092MPa~-0.080MPa, the rising steam in the kettle enters the distillation tower C, and is adjusted by adjusting the reflux The ratio is 2 to 4:1, and the rising steam temperature of the distillation tower is controlled at 45°C to 50°C to distill out cyclohexanone and water. The temperature at the top of the distillation tower rises to 110°C...

Embodiment 2

[0021] Example 2: PGMEA waste liquid, components: PGMEA: 65.72%, PGME: 8.6%, 3-ethoxy ethyl propionate 14%, 3-methoxy-1-butanol acetate 2.5%, moisture 1.52%, and Other impurities 7.66%, etc.

[0022] Steps:

[0023] (1) After the waste PGMEA solution is filtered through filter A to remove large solid waste, it enters the raw material settling tank B to remove settleable solid impurities;

[0024] (2) After filtering and settling, the PGMEA waste liquid enters the distillation tower C. In this embodiment, a 7-10 meter high orifice corrugated packing with strong anti-fouling ability is used in the tower. After the distillation kettle is heated by 0.6MPa saturated steam , the rising steam in the kettle enters the distillation tower C, and the vacuum degree is controlled at -0.090MPa~-0.085MPa. By adjusting the reflux ratio of 3~5:1, the temperature of the distillation tower top is controlled to 90°C~120°C, and the crude product PGMEA is distilled;

[0025] (3) The crude produ...

Embodiment 3

[0027] Example 3: PGMEA waste liquid, components: PGMEA: 70.57%, xylene 10.85%, water 8.01%, 2-butoxyethanol 2.65%, and other impurities 7.92%.

[0028] Steps:

[0029] (1) After the waste PGMEA solution is filtered through filter A to remove large solid waste, it enters the raw material settling tank B to remove settleable solid impurities;

[0030] (2) The filtered and settled PGMEA waste liquid enters the distillation tower C. In this embodiment, a 7-9 meter high orifice corrugated packing with strong anti-fouling ability is used in the tower. After the distillation kettle is heated by 0.6MPa saturated steam , the vacuum degree is controlled at -0.095MPa~-0.090MPa, the rising steam in the kettle enters the distillation tower C, by adjusting the reflux ratio of 3 to 5:1, the temperature of the rising steam in the distillation tower is controlled at 50~55°C, and xylene and water are evaporated . The temperature at the top of the distillation tower rises to 110°C, and the ...

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Abstract

The present invention disclosed a method of purifying PGMEA from PGMEA waste liquid. PGMEA waste liquid mainly contains PGME (propylene glycol methar ether), ketone compounds, benzene compounds, ethyl ester compounds, methoxycodes, and compounds, and methamphetamine.Water, solid resistance, electronic component and other impurities, the scope and content of waste liquids and content changes are widely changed. The PGMEA waste liquid generated by the invention for the electronic industry is initially filtered for the collected waste solvents.Impurities, after the settlement, the upper liquid enters the distilled tower with vacuum pumps to remove the low -boiling point and high boiling point impurities that are difficult to handle. The target products generated by the distilled tower enter the psychiatric tower to further distille, obtaining target products with a purity of more than 95%The maximum purity can reach 99%.The processing equipment mainly includes filter, sinking kettle, distillation tower, and distillation tower.

Description

technical field [0001] The invention relates to a method for purifying PGMEA from the PGMEA waste liquid produced in the electronics industry, in particular to regenerate a PGMEA solvent with a purity >95% from the PGMEA waste liquid produced in the LCD industry. Background technique [0002] PGMEA (Propylene Glycol Methyl Ether Acetate) solvent, as a low-toxic high-grade industrial solvent with excellent performance, has a strong ability to dissolve polar and non-polar substances. In the electronics industry, especially in the production process of LCD panels, PGMEA solvent is needed as a cleaning agent for cleaning photoresist spray nozzles and coating containers, etc. The waste solvent generated usually contains solid impurities such as heavy metals, waste components, particulate impurities, high-boiling glue and oil. However, there are many useful components in PGMEA waste liquid, and the solvent is expensive. Considering the economy and environmental protection, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/16C07C67/48C07C67/54
CPCC07C67/48C07C67/54C07C69/16
Inventor 王治军李红玲
Owner 惠州TCL环境科技有限公司
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