阅读说明：本技术 一种从废剥离液中提纯二乙二醇丁醚试剂的方法 (Method for purifying diethylene glycol monobutyl ether reagent from waste stripping liquid ) 是由 李向峰 黄安宁 高豹 李星星 桂园芬 余何建 张晟煜 郭志祥 陈结文 于 2019-11-05 设计创作，主要内容包括：本发明属于废液回收领域,具体涉及一种从废剥离液中提纯二乙二醇丁醚试剂的方法,包括如下步骤：S1、除去废剥离液中的颗粒杂志、树脂、金属缓蚀剂和表面活性剂；S2、向经过S1处理后的母液中加入二氯甲烷进行萃取,收集有机相；S3、对有机相进行减压蒸馏,从35℃开始收集二氯甲烷,从140℃开始收集二乙二醇丁醚；S4、对收集的二乙二醇丁醚进行干燥处理。本发明的有益效果是：二乙二醇丁醚可以与水、乙醇、油类等溶剂完全混合,挥发度低,高沸点,毒性弱,被广泛用作油漆、油墨、树脂等的溶剂,可溶解油脂,染料,树脂,硝化纤维素；本发明提供一种从废剥离液中提纯二乙二醇丁醚试剂的方法,工艺简单、操作便捷,回收的二乙二醇丁醚含量高达99.8％。(The invention belongs to the field of waste liquid recovery, and particularly relates to a method for purifying a diethylene glycol monobutyl ether reagent from waste stripping liquid, which comprises the following steps: s1, removing particle impurities, resin, metal corrosion inhibitor and surfactant in the waste stripping liquid; s2, adding dichloromethane into the mother liquor treated by the S1 for extraction, and collecting an organic phase; s3, carrying out reduced pressure distillation on the organic phase, collecting dichloromethane from 35 ℃, and collecting diethylene glycol butyl ether from 140 ℃; and S4, drying the collected diethylene glycol butyl ether. The invention has the beneficial effects that: diethylene glycol monobutyl ether can be completely mixed with solvents such as water, ethanol, oil and the like, has low volatility, high boiling point and weak toxicity, is widely used as the solvent of paint, printing ink, resin and the like, and can dissolve grease, dye, resin and nitrocellulose; the invention provides a method for purifying a diethylene glycol monobutyl ether reagent from waste stripping liquid, which has the advantages of simple process and convenient operation, and the content of the recovered diethylene glycol monobutyl ether is as high as 99.8%.)

1. A method for purifying diethylene glycol monobutyl ether reagent from waste stripping liquid is characterized by comprising the following steps:

s1, removing particle impurities, resin, metal corrosion inhibitor and surfactant in the waste stripping liquid;

s2, adding dichloromethane into the mother liquor treated by the S1 for extraction, and collecting an organic phase;

s3, carrying out reduced pressure distillation on the organic phase, collecting dichloromethane from 35 ℃, and collecting diethylene glycol butyl ether from 140 ℃;

and S4, drying the collected diethylene glycol butyl ether.

2. The method for purifying diethylene glycol monobutyl ether reagent from waste stripping solution as claimed in claim 1, wherein the specific step of S1 is to make the waste stripping solution pass through a first separation layer for removing particulate impurities and resin and a second separation layer for removing metal corrosion inhibitor and surfactant in turn.

3. The method for purifying the diethylene glycol monobutyl ether reagent from the waste stripping solution as claimed in claim 2, wherein the first separation layer is provided with acidified activated carbon.

4. The method for purifying the diethylene glycol monobutyl ether reagent from the waste stripping liquid as claimed in claim 3, wherein an adsorbing material is arranged in the second separation layer, and the adsorbing material is polyanionic cellulose with chitosan microspheres adsorbed on the surface.

5. The method for purifying the diethylene glycol monobutyl ether reagent from the waste stripping liquid as claimed in claim 1, wherein the acidified activated carbon comprises, by weight, 90-98 parts of activated carbon, 1-5 parts of sodium silicate, 1-3 parts of polyvinyl alcohol, 3-5 parts of boron oxide and 3-5 parts of phosphotungstic acid.

6. The method for purifying diethylene glycol monobutyl ether reagent from waste stripping solution according to claim 5, wherein the acidified activated carbon is prepared by the following steps: adding activated carbon, sodium silicate, polyvinyl alcohol, boron oxide and phosphotungstic acid into water according to a ratio, uniformly stirring, extruding into a sheet-shaped object with the thickness of less than 5 mm, drying at the temperature of 110-130 ℃ until the water content in the sheet-shaped object is less than 5%, and then grinding until the particle size is less than 0.1 mm to obtain the acidified activated carbon.

7. The method for purifying diethylene glycol monobutyl ether reagent from waste stripping solution according to claim 4, wherein the preparation method of the adsorption material is as follows: dispersing chitosan microspheres in water, and separating out the chitosan microspheres on the surface of polyanionic cellulose to obtain the adsorbing material, wherein the mass percent of chitosan in the adsorbing material is 2% -4%.

Technical Field

The invention belongs to the field of waste liquid recovery, and particularly relates to a method for purifying a diethylene glycol monobutyl ether reagent from waste stripping liquid.

Background

With the rapid development of the domestic electronic manufacturing industry, the usage amount of the electronic chemicals such as the photoresist stripper is also increased. A large amount of photoresist stripper is used and a large amount of waste photoresist stripper is also generated. The waste stripping solution contains not only stripping solvent (diethylene glycol monobutyl ether), but also photoresist resin, water, metal corrosion inhibitor and surfactant.

Heretofore, these waste stripping solutions cannot meet the standard of recycling after simple treatment, and generally can only be degraded for use, for example, they are burned as organic fuel or simply recycled to become low-quality solvents for chemical industry, and in the process, secondary pollution is often generated.

Disclosure of Invention

In order to solve the problems, the invention provides a method for purifying a diethylene glycol butyl ether reagent from waste stripping liquid, which has the advantages of simple process and convenient operation, and the content of the recovered diethylene glycol butyl ether is as high as 99.8%.

The invention provides the following technical scheme:

a method for purifying diethylene glycol monobutyl ether reagent from waste stripping liquid comprises the following steps:

s1, removing particle impurities, resin, metal corrosion inhibitor and surfactant in the waste stripping liquid;

s2, adding dichloromethane into the mother liquor treated by the S1 for extraction, and collecting an organic phase;

s3, carrying out reduced pressure distillation on the organic phase, collecting dichloromethane from 35 ℃, and collecting diethylene glycol butyl ether from 140 ℃;

and S4, drying the collected diethylene glycol butyl ether.

Preferably, the specific step of S1 is to sequentially pass the waste stripping solution through a first separation layer for removing particulate impurities, resin and a second separation layer for removing metal corrosion inhibitor and surfactant.

Preferably, acidified activated carbon is arranged in the first separation layer.

Preferably, an adsorption material is arranged in the second separation layer, and the adsorption material is polyanionic cellulose with the surface adsorbing the chitosan microspheres.

Preferably, the acidified activated carbon comprises, by weight, 90-98 parts of activated carbon, 1-5 parts of sodium silicate, 1-3 parts of polyvinyl alcohol, 3-5 parts of boron oxide and 3-5 parts of phosphotungstic acid.

Preferably, the preparation method of the acidified activated carbon comprises the following steps: adding activated carbon, sodium silicate, polyvinyl alcohol, boron oxide and phosphotungstic acid into water according to a ratio, uniformly stirring, extruding into a sheet-shaped object with the thickness of less than 5 mm, drying at the temperature of 110-130 ℃ until the water content in the sheet-shaped object is less than 5%, and then grinding until the particle size is less than 0.1 mm to obtain the acidified activated carbon.

Preferably, the preparation method of the adsorbing material is as follows: dispersing chitosan microspheres in water, and separating out the chitosan microspheres on the surface of polyanionic cellulose to obtain the adsorbing material, wherein the mass percent of chitosan in the adsorbing material is 2% -4%.

The invention has the beneficial effects that:

diethylene glycol monobutyl ether can be completely mixed with solvents such as water, ethanol, oil and the like, has low volatility, high boiling point and weak toxicity, is widely used as the solvent of paint, printing ink, resin and the like, and can dissolve grease, dye, resin and nitrocellulose;

the invention provides a method for purifying a diethylene glycol monobutyl ether reagent from waste stripping liquid, which has the advantages of simple process and convenient operation, and the content of the recovered diethylene glycol monobutyl ether is as high as 99.8%.

Detailed Description

The present invention will be described in detail with reference to the following examples.

The waste stripping liquid mainly comprises diethylene glycol monobutyl ether, ethanolamine, water, a small amount of resin, a metal corrosion inhibitor and a surfactant, and the composition ratio is 0.55-0.65:0.2-0.3: 0.1-0.15: 0.01-0.05: 0.01-1: 0.01-1.