CN111018219A - Regeneration treatment process and device for waste stripping liquid - Google Patents
Regeneration treatment process and device for waste stripping liquid Download PDFInfo
- Publication number
- CN111018219A CN111018219A CN201911339818.5A CN201911339818A CN111018219A CN 111018219 A CN111018219 A CN 111018219A CN 201911339818 A CN201911339818 A CN 201911339818A CN 111018219 A CN111018219 A CN 111018219A
- Authority
- CN
- China
- Prior art keywords
- liquid
- waste
- distillation
- separation tank
- kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 120
- 239000002699 waste material Substances 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 58
- 230000008929 regeneration Effects 0.000 title claims abstract description 31
- 238000011069 regeneration method Methods 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 72
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000004821 distillation Methods 0.000 claims abstract description 48
- 238000000926 separation method Methods 0.000 claims abstract description 35
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000004062 sedimentation Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 6
- 229920002120 photoresistant polymer Polymers 0.000 claims description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 23
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 20
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 20
- 229910021645 metal ion Inorganic materials 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 12
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 7
- 239000008096 xylene Substances 0.000 claims description 6
- 230000001172 regenerating effect Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 239000011347 resin Substances 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 238000001179 sorption measurement Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000002920 hazardous waste Substances 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- -1 alcohol amine Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/10—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a regeneration treatment process and a device for waste stripping liquid, wherein the treatment process comprises the following steps: (1) settling and filtering the waste stripping liquid to remove solid impurities in the waste stripping liquid; (2) adding an extracting agent into the waste glass liquid after sedimentation and filtration, and stirring and mixing; (3) feeding the mixed material of the waste glass liquid and the extracting agent into a kettle body of a distillation kettle, heating to 120-220 ℃ to evaporate part of the material, cooling the evaporated material by a condenser at the top of the distillation kettle, feeding the cooled material into a liquid-liquid separation tank of the distillation kettle, and dividing the liquid-liquid separation tank into an upper layer and a lower layer; (4) refluxing the upper material of the liquid-liquid separation tank into the distillation still, and discharging the lower material to a collection tank; (5) when the liquid level of the lower-layer material of the liquid-liquid separation tank is not increased any more, the extractant in the kettle body is distilled, and the residual material at the bottom of the kettle body is further rectified to obtain the components of the stripping liquid. The method has low process cost and high recovery rate of the effective components of the ethanolamine and the stripping agent.
Description
Technical Field
The invention belongs to the field of waste liquid treatment, and particularly relates to a regeneration treatment process of waste stripping liquid.
Background
The main components of the waste stripping solution obtained by processing photoresist cleaning and the like in the electronic manufacturing industry and the photoelectric industry at present comprise moisture, light components (mainly ethanolamine and diethylene glycol monobutyl ether) and heavy components (mainly photoresist and metal ions). The harmless treatment process of the waste stripping liquid mainly adopts the methods of incineration, distillation and rectification, resin adsorption and filtration and the like to separate the water, light components and heavy components in the waste stripping liquid from the photoresist, metal ions and ethanolamine so as to achieve pollution-free regeneration treatment.
Although incineration, distillation and rectification, resin adsorption and filtration and the like can treat the waste stripping liquid, each method has its own defects, for example, the incineration method used in the treatment process has high cost and serious waste of resources; although the common distillation and rectification method can remove ethanolamine and moisture, the ethanolamine and the moisture are difficult to meet the quality requirement. The resin absorbs and filters water and ethanolamine, but cannot remove the components, and only can remove metal ions and heavy component photoresist.
Therefore, a high-performance material with good biological safety, good heavy metal adsorption effect, short treatment period of heavy metal pollution and low treatment cost is urgently needed for solving the problem of heavy metal pollution.
Disclosure of Invention
The invention aims to provide a regeneration treatment process of waste stripping liquid, aiming at solving the problems in the prior art in the treatment method of waste stripping liquid obtained by treating photoresist cleaning and the like in the electronic manufacturing industry and the photoelectric industry, wherein the recovery rate of ethanolamine and diethylene glycol monobutyl ether in a stripping agent in the waste stripping liquid can reach more than 99%, light components, heavy components of photoresist, ethanolamine and metal ions in the waste stripping liquid can be removed to the utmost extent, and the purity of the recovered components is high, for example, the purity of the recovered ethanolamine and diethylene glycol monobutyl ether can reach 99.9%.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a regeneration treatment process of waste stripping liquid comprises the following steps:
(1) settling and filtering the waste stripping liquid to remove solid impurities in the waste stripping liquid;
(2) adding an extracting agent into the waste glass liquid after sedimentation and filtration, and stirring and mixing;
(3) feeding the mixed material of the waste glass liquid and the extracting agent into a kettle body of a distillation kettle, heating to 120-220 ℃ to evaporate part of the material (mainly low-boiling-point components), cooling the evaporated material by a condenser at the top of the distillation kettle, feeding the cooled material into a liquid-liquid separation tank of the distillation kettle, and dividing the liquid-liquid separation tank into an upper layer and a lower layer;
(4) refluxing the upper material of the liquid-liquid separation tank into the distillation still, and discharging the lower material to a collection tank;
(5) when the liquid level of the lower-layer material of the liquid-liquid separation tank is not increased any more, the extractant in the kettle body is distilled, and the residual material (mainly low-boiling-point components) at the bottom of the kettle body is further rectified to obtain the components of the stripping liquid.
In the regeneration treatment process of the waste stripping liquid, the waste stripping liquid is obtained by cleaning photoresist in the electronic manufacturing industry and the photoelectric industry and comprises water, light components (mainly ethanolamine and diethylene glycol monobutyl ether) and heavy components (mainly photoresist and metal ions).
In a preferred embodiment, the regeneration treatment process of the waste stripping solution further comprises the step of further distilling the lower layer material to obtain ethanolamine.
In a preferred embodiment, the regeneration treatment process of the waste stripping solution of the present invention further comprises further treating the residue material at the bottom of the rectified still to remove metal ions and photoresist.
In a preferred embodiment, in the regeneration treatment process of the waste stripping solution, the weight ratio of the waste stripping solution to the extracting agent is 1: 0.5-2.
In a preferred embodiment, in the process for regenerating a spent stripping solution according to the present invention, the extractant is a low-boiling aromatic hydrocarbon or naphthenic hydrocarbon solvent.
In a preferred embodiment, in the regeneration treatment process of the waste stripping solution of the present invention, the above-mentioned extracting agent is selected from one or more of cyclohexane, toluene and xylene. In a more preferred embodiment, the extractant is cyclohexane and the heating temperature in step (3) is 120 ℃. In a more preferred embodiment, the extractant is toluene and the heating temperature in step (3) is 200 ℃. In a more preferred embodiment, the extractant is xylene and the heating temperature in step (3) is 150 ℃.
In a preferred embodiment, in the regeneration treatment process of the waste stripping solution of the present invention, the component of the stripping solution obtained by the further rectification in the step (5) is diethylene glycol monobutyl ether.
The invention also provides equipment for the regeneration treatment process of the waste stripping liquid, which comprises a distillation kettle, wherein the distillation kettle comprises a kettle body, a condenser, a liquid-liquid separation tank and a collection tank,
wherein the condenser is positioned at the top of the distillation kettle,
the liquid-liquid separation tank is respectively communicated with the condenser and the collection tank.
In a preferred embodiment, the apparatus for the regeneration treatment process of waste stripping liquid of the present invention further comprises a rectification device connected to the still body for rectifying residual materials at the bottom of the still body.
In a preferred embodiment, the apparatus for the regeneration treatment process of spent stripper according to the present invention further comprises a distillation means connected to the collection tank for distilling the lower layer material.
The working principle of the regeneration treatment process of the waste stripping liquid is as follows: the waste stripping liquid is separated by utilizing the different properties of different components in the waste stripping liquid. For example, solid impurities in the stripping liquid are removed through sedimentation and filtration, other high-boiling-point components and metal ions are not evaporated when heated at 120-200 ℃ and are continuously remained in the kettle body, and low-boiling-point components in the waste stripping liquid, such as water and ethanolamine, are evaporated together with an extracting agent when heated and enter a collecting tank after being cooled, so that the high-boiling-point components and the low-boiling-point components in the waste stripping liquid can be separated. Then, the high boiling point component and the low boiling point component are respectively rectified and distilled to obtain diethylene glycol monobutyl ether and ethanolamine.
According to the regeneration treatment process of the waste stripping liquid, the high-boiling-point component and the low-boiling-point component in the waste stripping liquid are separated by using the extracting agent, and then rectification and distillation are respectively carried out to obtain diethylene glycol monobutyl ether and ethanolamine, wherein the used extracting agent can be repeatedly used. Compared with the methods of incineration, distillation and rectification, resin adsorption and filtration and the like adopted in the prior art, the method for treating the waste stripping liquid has the advantages of high cost, high equipment investment, complex operation, easy generation of a large amount of secondary hazardous waste and the like, and the regeneration treatment process of the waste stripping liquid has the following beneficial effects:
1. the treatment process has the advantages of low equipment investment, simple operation, low treatment cost and less generated secondary hazardous waste.
2. The recovery rate of the stripping liquid is high, the recovery rate of the effective component (diethylene glycol monobutyl ether) of the stripping liquid and the ethanolamine can reach 99%, and the purity of the recovered diethylene glycol monobutyl ether and ethanolamine can reach 99.9%.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain and explain part of the invention.
FIG. 1 is a process flow diagram of a waste stripping solution regeneration treatment process of the present invention.
Fig. 2 is an apparatus for the spent stripper regeneration treatment process of the present invention.
Detailed Description
Aiming at the defects of the method for treating the waste stripping liquid by adopting incineration, distillation and rectification, resin adsorption and filtration and the like in the prior art, the inventor of the application finds that the waste stripping liquid can be recycled to the utmost extent by adopting an extractant treatment method, so that the separation of the effective components of the waste stripping liquid, water, light components, heavy component photoresist and ethanolamine is realized; meanwhile, the treatment production efficiency and the effective component yield of the waste stripping liquid can be improved, and the production cost and the investment cost are reduced.
As shown in fig. 1, the regeneration treatment process of the waste stripping solution of the present invention comprises the following steps: (1) settling and filtering the waste stripping liquid to remove solid impurities in the waste stripping liquid; (2) adding an extracting agent into the waste stripping liquid after sedimentation and filtration, and stirring and mixing; (3) feeding a material obtained by mixing the waste stripping liquid and the extracting agent into a kettle body of a distillation kettle, heating to 120-220 ℃ to evaporate part of the material, cooling the evaporated material by a condenser at the top of the distillation kettle, feeding the cooled material into a liquid-liquid separation tank of the distillation kettle, and dividing the liquid-liquid separation tank into an upper layer and a lower layer; (4) refluxing the upper layer material (mainly an extracting agent) of the liquid-liquid separation tank to the distillation still, and discharging the lower layer material (mainly water and ethanolamine) to a collection tank; (5) when the liquid level of the lower-layer material of the liquid-liquid separation tank is not increased any more, the extractant in the kettle body is distilled, and the residual material (mainly high-boiling-point components) at the bottom of the kettle body is further rectified to obtain the components of the stripping liquid. The regeneration treatment process of the waste stripping solution of the present invention as shown in FIG. 1 further comprises the step of further treating the residue material at the bottom of the rectified still to remove metal ions and photoresist.
The metal ion removal and the removal of the photoresist can be performed by a method conventional in the art, for example, the photoresist is removed by burning, and then the metal ion is removed by resin adsorption.
In the description of the present invention, the extracting agent includes, but is not limited to, one or more of cyclohexane, benzene, xylene, toluene and aromatic hydrocarbon solvents.
The invention is further illustrated with reference to the following figures and specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Experimental procedures for conditions not specified in the examples below are generally carried out under conventional conditions, or as recommended by the manufacturer. Percentages are by weight unless otherwise indicated.
An apparatus for the regeneration treatment of a spent stripping solution used in the following examples is shown in FIG. 2 and comprises a still 1 including a still body 11, a condenser 12, a liquid-liquid separation tank 2 and a collection tank 3.
Wherein the condenser 12 is positioned at the top of the kettle body 11,
the liquid-liquid separation tank 2 is in fluid communication with a condenser 12 and a collection tank 3, respectively.
The apparatus may further comprise a rectification means (not shown) in fluid communication with the still body for rectifying residual material at the bottom of the still body.
Example 1
The waste stripping solution treated in this example is a waste stripping solution obtained by cleaning a photoresist in the electronics manufacturing industry and the photovoltaic industry, and the main components of the waste stripping solution include moisture, light components (mainly ethanolamine and diethylene glycol monobutyl ether), and heavy components (mainly photoresist and metal ions).
The regeneration treatment process of the waste stripping liquid comprises the following steps:
(1) settling and filtering the waste stripping liquid to remove solid impurities in the waste stripping liquid;
(2) adding cyclohexane into the waste stripping liquid after sedimentation and filtration, and stirring and mixing, wherein the weight ratio of the waste stripping liquid to the cyclohexane is 1: 0.5;
(3) feeding the mixed material of the waste stripping liquid and cyclohexane into a kettle body of a distillation kettle, heating the material to 120 ℃ to evaporate part of the material (mainly low-boiling-point components), cooling the evaporated material by a condenser at the top of the distillation kettle, feeding the cooled material into a liquid-liquid separation tank of the distillation kettle, and dividing the liquid-liquid separation tank into an upper layer and a lower layer;
(4) refluxing the upper material (mainly cyclohexane) in the liquid-liquid separation tank to the kettle body of the distillation kettle, and discharging the lower material (mainly water and ethanolamine) phase to a collection tank for further distillation;
(5) when the material at the lower layer is not increased any more, distilling cyclohexane out, and further rectifying the residual material (mainly high boiling point component) at the bottom of the kettle body to obtain diethylene glycol monobutyl ether in the waste stripping liquid;
(6) and (4) burning and resin adsorbing the residual materials at the bottom of the rectified kettle body in sequence to remove the photoresist and metal ions. Distilling the lower layer material at 120 deg.c to eliminate water to obtain alcohol amine;
the purity of the recovered ethanolamine is 99.0%, and the recovery rate is 90%.
And further rectifying the residue at the bottom of the kettle at the temperature of 220 ℃ and under the pressure of 3000pa to obtain the diethylene glycol monobutyl ether.
The purity of the recovered diethylene glycol monobutyl ether was 99.9%, and the recovery rate was 90%.
Example 2
The waste stripping solution treated in this example is a waste stripping solution obtained by cleaning a photoresist in the electronics manufacturing industry and the photovoltaic industry, and the like, and the main components of the waste stripping solution include moisture, light components (mainly ethanolamine and diethylene glycol monobutyl ether), and heavy components (mainly photoresist and metal ions).
The regeneration treatment process of the waste stripping liquid comprises the following steps:
(1) settling and filtering the waste stripping liquid to remove solid impurities in the waste stripping liquid;
(2) adding toluene into the waste stripping liquid after sedimentation and filtration, and stirring and mixing, wherein the weight ratio of the waste stripping liquid to cyclohexane is 1: 0.5;
(3) feeding the mixed material of the waste stripping liquid and the toluene into a kettle body of a distillation kettle, heating the material to 200 ℃ to evaporate part of the material (mainly low-boiling-point components), cooling the evaporated material by a condenser at the top of the distillation kettle, feeding the cooled material into a liquid-liquid separation tank of the distillation kettle, and dividing the liquid-liquid separation tank into an upper layer and a lower layer;
(4) refluxing the upper layer material (mainly toluene) of the liquid-liquid separation tank to the kettle body of the distillation kettle, and discharging the lower layer material (mainly water and ethanolamine) phase to a collection tank for further distillation;
(5) when the material at the lower layer of the liquid-liquid separation tank is not increased any more, toluene is distilled out, and the residual material (mainly high boiling point component) at the bottom of the kettle body is further refined to distill the diethylene glycol monobutyl ether in the waste stripping liquid;
(6) and (4) burning and resin adsorbing the residual materials at the bottom of the rectified kettle body in sequence to remove the photoresist and metal ions. .
The procedure for further distillation of the aqueous phase described above in this example was the same as in example 1. The purity of the recovered ethanolamine is 99.5%, and the recovery rate is 95%.
The process of further distilling the residue at the bottom of the still in this example was the same as in example 1. The purity of the recovered diethylene glycol monobutyl ether is 99.9%, and the recovery rate is 95%.
Example 3
The waste stripping solution treated in this example is a waste stripping solution obtained by cleaning a photoresist in the electronics manufacturing industry and the photovoltaic industry, and the like, and the main components of the waste stripping solution include moisture, light components (mainly ethanolamine and diethylene glycol monobutyl ether), and heavy components (mainly photoresist and metal ions).
The regeneration treatment process of the waste stripping liquid comprises the following steps:
(1) settling and filtering the waste stripping liquid to remove solid impurities in the waste stripping liquid;
(2) adding dimethylbenzene into the waste stripping liquid after sedimentation and filtration, and stirring and mixing, wherein the weight ratio of the waste stripping liquid to the dimethylbenzene is 1: 1;
(3) feeding the mixed material of the waste stripping liquid and xylene into a kettle body of a distillation kettle, heating the material to 150 ℃ to evaporate part of the material (mainly low-boiling-point components), cooling the evaporated material by a condenser at the top of the distillation kettle, feeding the cooled material into a liquid-liquid separation tank of the distillation kettle, and dividing the liquid-liquid separation tank into an upper layer and a lower layer;
(4) refluxing the upper layer material (mainly xylene) of the liquid-liquid separation tank to the kettle body of the distillation kettle, and discharging the lower layer material (mainly water and ethanolamine) phase to a collection tank for further distillation;
(5) when the material at the lower layer of the liquid-liquid separation tank is not increased any more, distilling out dimethylbenzene, and further rectifying the diethylene glycol monobutyl ether in the waste stripping liquid from the residual material (mainly high boiling point components) at the bottom of the kettle body;
(6) and (4) burning and resin adsorbing the residual materials at the bottom of the rectified kettle body in sequence to remove the photoresist and metal ions.
The procedure for further distillation of the aqueous phase described above in this example was the same as in example 1. The purity of the recovered ethanolamine is 99.9%, and the recovery rate is 99%.
The process of further distilling the residue at the bottom of the still in this example was the same as in example 1. The purity of the recovered diethylene glycol monobutyl ether was 99.9, and the recovery rate was 99%.
The regeneration treatment process of the waste stripping liquid can achieve the aim of harmless regeneration treatment of the waste stripping liquid, and overcomes the defects of high production operation difficulty, high secondary hazardous waste, high equipment investment and the like in the waste stripping liquid treatment processes such as incineration, distillation and rectification, resin adsorption and filtration and the like. By adopting the regeneration treatment process of the waste stripping liquid, the waste stripping liquid can be regenerated to the utmost extent, and the separation of the effective components of the stripping agent, water, light components, heavy components, photoresist and ethanolamine is achieved; meanwhile, the production efficiency and the yield of effective components of the waste stripping liquid can be improved, and the production cost and the investment cost are reduced.
The invention has been described above without limitation by way of examples according to its preferred production modality, but it is to be understood that variations and/or modifications can be made by a person skilled in the art within the scope defined by the appended claims without departing from the relevant protection scope.
Claims (10)
1. The regeneration treatment process of the waste stripping liquid is characterized by comprising the following steps:
(1) settling and filtering the waste stripping liquid to remove solid impurities in the waste stripping liquid;
(2) adding an extracting agent into the waste glass liquid after sedimentation and filtration, and stirring and mixing;
(3) feeding the mixed material of the waste glass liquid and the extracting agent into a kettle body of a distillation kettle, heating to 120-200 ℃ to evaporate part of the material, cooling the evaporated material by a condenser at the top of the distillation kettle, feeding the cooled material into a liquid-liquid separation tank of the distillation kettle, and dividing the liquid-liquid separation tank into an upper layer and a lower layer;
(4) refluxing the upper material of the liquid-liquid separation tank into the distillation still, and discharging the lower material to a collection tank;
(5) when the liquid level of the lower-layer material of the liquid-liquid separation tank is not increased any more, the extractant in the kettle body is distilled, and the residual material at the bottom of the kettle body is further rectified to obtain the components of the stripping liquid.
2. The process of claim 1, further comprising further distilling the lower material to obtain ethanolamine.
3. The process of claim 1, further comprising further treating the residue at the bottom of the kettle after rectification to remove metal ions and photoresist.
4. The process for regenerating the spent stripper according to any of claims 1 to 3, wherein the weight ratio of the spent stripper to the extractant is 1:0.5 to 2.
5. The process for regenerating spent stripper according to any of claims 1 to 3, wherein the extractant is a low boiling aromatic or naphthenic solvent.
6. The process of claim 5, wherein the extractant is selected from one or more of cyclohexane, toluene and xylene.
7. The process for regenerating and treating waste stripping liquid as claimed in any one of claims 1 to 3, wherein the stripping liquid component obtained by further rectifying in step (5) is diethylene glycol monobutyl ether.
8. The apparatus for the spent stripper reclamation processing technique according to any one of claims 1 to 7, wherein the apparatus comprises a distillation still, the distillation still comprising a still body, a condenser, a liquid-liquid separation tank and a collection tank,
wherein the condenser is positioned at the top of the distillation kettle,
the liquid-liquid separation tank is respectively communicated with the condenser and the collection tank.
9. The apparatus of claim 8, further comprising a rectification device connected to the vessel for rectifying residual material from the bottom of the vessel.
10. The apparatus of claim 8, further comprising a distillation device connected to said holding tank for distilling said lower layer of material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911339818.5A CN111018219A (en) | 2019-12-23 | 2019-12-23 | Regeneration treatment process and device for waste stripping liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911339818.5A CN111018219A (en) | 2019-12-23 | 2019-12-23 | Regeneration treatment process and device for waste stripping liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111018219A true CN111018219A (en) | 2020-04-17 |
Family
ID=70212656
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911339818.5A Pending CN111018219A (en) | 2019-12-23 | 2019-12-23 | Regeneration treatment process and device for waste stripping liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111018219A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112321044A (en) * | 2020-09-01 | 2021-02-05 | 福建钰融科技有限公司 | Purification liquid of waste stripping liquid and purification method and application thereof |
| CN116332775A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Recycling method of stripping liquid waste liquid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1656054A (en) * | 2002-05-07 | 2005-08-17 | 巴斯福股份公司 | Method for producing an aqueous alkali acrylate solution |
| JP2007241278A (en) * | 2006-03-03 | 2007-09-20 | Dongjin Semichem Co Ltd | Regeneration method and regeneration apparatus for resist stripping waste liquid |
| CN102219272A (en) * | 2011-03-09 | 2011-10-19 | 友达光电股份有限公司 | Photoresist stripper waste liquid recovery system and method thereof |
| CN102951761A (en) * | 2012-11-14 | 2013-03-06 | 杭州格林达化学有限公司 | Method for recovering waste photoresist stripper |
| CN109111011A (en) * | 2018-10-30 | 2019-01-01 | 上海天汉环境资源有限公司 | A kind of waste emulsified mixture innocuity disposal system and demulsifier |
| CN208340142U (en) * | 2018-02-15 | 2019-01-08 | 上海晶福机电科技有限公司 | A kind of regenerative system for glass substrate treated stripper |
-
2019
- 2019-12-23 CN CN201911339818.5A patent/CN111018219A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1656054A (en) * | 2002-05-07 | 2005-08-17 | 巴斯福股份公司 | Method for producing an aqueous alkali acrylate solution |
| JP2007241278A (en) * | 2006-03-03 | 2007-09-20 | Dongjin Semichem Co Ltd | Regeneration method and regeneration apparatus for resist stripping waste liquid |
| CN102219272A (en) * | 2011-03-09 | 2011-10-19 | 友达光电股份有限公司 | Photoresist stripper waste liquid recovery system and method thereof |
| CN102951761A (en) * | 2012-11-14 | 2013-03-06 | 杭州格林达化学有限公司 | Method for recovering waste photoresist stripper |
| CN208340142U (en) * | 2018-02-15 | 2019-01-08 | 上海晶福机电科技有限公司 | A kind of regenerative system for glass substrate treated stripper |
| CN109111011A (en) * | 2018-10-30 | 2019-01-01 | 上海天汉环境资源有限公司 | A kind of waste emulsified mixture innocuity disposal system and demulsifier |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112321044A (en) * | 2020-09-01 | 2021-02-05 | 福建钰融科技有限公司 | Purification liquid of waste stripping liquid and purification method and application thereof |
| CN116332775A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Recycling method of stripping liquid waste liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102604732A (en) | Static mixed rotational flow separation and extraction process of regenerative base oil N-methyl pyrrolidone | |
| CN106753742B (en) | Regeneration method of waste lubricating oil | |
| CN105016554B (en) | Semi-coke wastewater treatment process | |
| CN102659204B (en) | Method for treating waste water in coal chemical industry | |
| CN102674609A (en) | Separation treatment method for waste water in coal tar machining process | |
| CN106906365A (en) | Rare earth oxide production wastewater treatment and rare earth recycling technique | |
| KR970009646B1 (en) | Process for extracting and disposing of nitrophenolic by-products | |
| CN111018219A (en) | Regeneration treatment process and device for waste stripping liquid | |
| CN102267890A (en) | Method for extracting and recovering acrylic acid from acrylic ester production wastewater | |
| CN104099171A (en) | Continuous distillation technology used for regeneration of spent lubrication oil | |
| CN107098554B (en) | Oil field sludge recycling treatment method | |
| CN113698959A (en) | Waste mineral oil recovery treatment process | |
| CN110252269A (en) | A kind of resin regeneration method for handling containing high-boiling components waste water | |
| CN102757813A (en) | Crude oil processing unit containing electro-desalted sewage oil remover and method of crude oil processing unit | |
| KR101794623B1 (en) | Method and apparatus for eliminating tar emulsion in ammoina liquor | |
| CN103820200B (en) | A kind of technique by producing base oil by regenerating waste lubricating oil | |
| CN111943297A (en) | A kind of method for resourceful treatment of high-salt and high-organic wastewater | |
| JPH11347536A (en) | Method for treating wastewater containing phenols | |
| CN215208811U (en) | Paint spraying wastewater treatment recycling system | |
| CN105505551B (en) | A kind of electrochemical regeneration processing method of waste lubricating oil | |
| CN102295380A (en) | Processing and recovering method of aromatic nitro-compound wastewater | |
| CN107814720B (en) | A kind of method that nitrobenzene tar recycles | |
| CN117959760A (en) | Regeneration method of waste mineral oil extractant | |
| KR20110111946A (en) | Waste Sludge Recycling Method and Regeneration System Generated in Manufacturing Solar Cell Wafer | |
| CN109987768A (en) | A method for treating cutting fluid waste water and recovering its effective components by extraction method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Guo Benhui Inventor after: Zong Jie Inventor after: Yao Kang Inventor after: Shen Jun Inventor before: Yao Kang Inventor before: Guo Benhui Inventor before: Shen Jun |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200417 |