CN115159636A - Developing solution waste liquid recycling and regenerating device and method - Google Patents
Developing solution waste liquid recycling and regenerating device and method Download PDFInfo
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- CN115159636A CN115159636A CN202210479558.7A CN202210479558A CN115159636A CN 115159636 A CN115159636 A CN 115159636A CN 202210479558 A CN202210479558 A CN 202210479558A CN 115159636 A CN115159636 A CN 115159636A
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Abstract
The invention provides a device and a method for recycling and regenerating waste liquid of developing solution, aiming at solving the problems that the waste liquid of developing solution contains photoresist and tetraalkylammonium hydroxide (TAAH) which is not completely utilized, a factory needs to spend a large amount of cost to carry out biodegradation treatment on the waste liquid, the investment of the existing process equipment is large, and the content of recycled impurities is high. The invention is especially suitable for recycling and regenerating the developer solution waste liquid with low cost and high quality, and has higher social use value and application prospect.
Description
Technical Field
The invention relates to the technical field of developer solution regeneration, in particular to a developer solution waste liquid recycling device and a developer solution waste liquid recycling method.
Background
A method of forming a pattern on a wafer or glass substrate during semiconductor and flat panel display manufacturing: first, a photoresist is coated on a substrate or a metal or non-metal film layer formed on the substrate, and then the photoresist is exposed to ultraviolet light through a patterned mask. The difference in solubility between exposed and unexposed photoresists is exploited, developed with a developer solution and then etched to achieve the purpose of patterning.
The main component of the developer is tetraalkylammonium hydroxide (i.e., TAAH), and after development, the developer waste liquid contains photoresist and incompletely utilized TAAH, and the factory needs to perform biodegradation treatment on the waste liquid at a large cost.
Chinese patent publication No. CN 101111804A discloses a method for treating a developing waste liquid: firstly, neutralizing with acid, filtering to remove the precipitated photoresist, evaporating and concentrating the filtrate to obtain high-concentration tetramethylammonium salt, further electrolyzing the tetramethylammonium salt with an ionic membrane to obtain TAAH, and adjusting the concentration to obtain a new developing solution;
the Chinese patent publication No. CN 108623052A discloses a method for treating developing waste liquid, which comprises the following steps: firstly, neutralizing with acid, filtering to remove the precipitated photoresist, removing metal ions from the filtrate through cation exchange resin, then evaporating and concentrating to obtain high-concentration tetramethylammonium salt, further electrolyzing the tetramethylammonium salt with an ionic membrane to obtain TAAH, and adjusting the concentration to obtain a new developing solution;
the two methods both need to be regenerated by electrolysis, and the equipment investment is large.
Chinese patent publication No. CN 105314770A discloses a method for treating a developing waste liquid: the precipitated photoresist is first neutralized with an acid, removed by filtration, and the filtrate is further removed by adsorption. Obtaining purified tetramethylammonium salt, and finally exchanging tetramethylammonium salt anions by using hydroxide radical of anion exchange resin to obtain TMAH;
the TMAH anion obtained by the method has high impurity content, and a large amount of alkali wastewater can be generated during resin regeneration.
Therefore, a device and a method for recycling and regenerating the waste liquid of the developing solution are provided.
Disclosure of Invention
It is an object of the present invention to solve or at least alleviate problems in the prior art.
In order to achieve the purpose, the invention is realized by the following technical scheme: the utility model provides a developer solution waste liquid recovery regenerating unit, is including the bipolar membrane electrodialysis mechanism that is used for retrieving regeneration development waste liquid, and wherein, bipolar membrane electrodialysis mechanism contains first utmost point liquid room, electrodialysis compartment, the second utmost point liquid room that sets gradually including handling the cell body at least in handling the cell body to carry out developer solution cation migration recombination under the drive of applied electric field and obtain regeneration pure TAAH.
Optionally, the device further comprises a development waste liquid storage tank for receiving and containing development waste liquid, a product tank for containing pure TAAH, and a waste liquid tank for containing secondary waste liquid generated by the development waste liquid treatment.
Optionally, the number of the electrodialysis compartments is multiple, and the electrodialysis compartments at least comprise a first bipolar membrane, an anion exchange membrane, a cation exchange membrane and a second bipolar membrane which are arranged in sequence;
a middle compartment filled with electrolyte-containing aqueous solution is formed between the first bipolar membrane and the anion exchange membrane;
a raw material compartment filled with developing waste liquid is formed between the anion exchange membrane and the cation exchange membrane, and the developing waste liquid is added into the raw material compartment in a pump or gravity flowing mode;
a product compartment filled with deionized water/pure TAAH aqueous solution is formed between the cation exchange membrane and the second bipolar membrane;
under the drive of an external electric field, TAAH cations of the development waste liquid in the raw material compartment migrate into the product compartment through the cation exchange membrane and are combined with hydroxide radicals generated by the second bipolar membrane to obtain a pure TAAH product;
organic matters such as photoresist and the like in the development waste liquid are blocked by the cation exchange membrane and still remain in the raw material compartment, and anions such as hydroxyl carbonate and the like in the development waste liquid enter the middle compartment through the anion exchange membrane and are combined with hydrogen ions generated by the first bipolar membrane to obtain water or carbon dioxide.
Optionally, the tank space on the side of the first bipolar membrane away from the second bipolar membrane forms a first electrode liquid chamber, an anode is arranged in the first electrode liquid chamber, and an electrolyte-containing aqueous solution is injected into the first electrode liquid chamber.
Optionally, a tank space on a side of the second bipolar membrane, which is away from the first bipolar membrane, constitutes a second electrolyte chamber, a cathode is disposed in the second electrolyte chamber, and an electrolyte-containing aqueous solution is injected into the second electrolyte chamber.
Alternatively, the electrolyte-containing aqueous solution may be sulfuric acid, sodium sulfate, sodium chloride, sodium hydroxide, or pure TAAH.
Alternatively, the electrolyte-containing aqueous solutions in the first and second polar liquid chambers and the electrolyte-containing aqueous solution in the intermediate compartment may be the same or different.
Optionally, a plurality of anion exchange membranes or cation exchange membranes are arranged between the first bipolar membrane and the anion exchange membrane to form a plurality of intermediate compartments.
Optionally, a plurality of anion exchange membranes or cation exchange membranes are arranged between the cation exchange membrane and the second bipolar membrane to form a plurality of intermediate compartments.
The invention also provides a method for recycling the developer solution waste liquid, which comprises the following steps:
s1, sequentially dividing a first polar liquid chamber, an electrodialysis compartment and a second polar liquid chamber in a treatment tank body, and dividing a middle compartment, a raw material compartment and a product compartment in the electrodialysis compartment;
s2, injecting an electrolyte-containing aqueous solution into the middle compartment, the first polar liquid chamber and the second polar liquid chamber, injecting a developing waste liquid into the raw material compartment, and injecting deionized water or a pure TAAH-containing aqueous solution into the product compartment;
s3, simultaneously starting the anode and the cathode in the first polar liquid chamber and the second polar liquid chamber, and transferring the positive ions of the developing liquid in the developing waste liquid into the product compartment to be combined with the hydroxyl generated by the second bipolar membrane for regeneration to obtain pure TAAH;
and S4, transferring and outputting the pure TAAH in the product compartment to a product tank for storage or directly entering a developing process, and transferring and outputting the remaining secondary waste liquid to a waste liquid tank for subsequent waste water treatment.
Optionally, there is at least one electrodialysis compartment and at least one intermediate compartment within each electrodialysis compartment.
The embodiment of the invention provides a device and a method for recycling and regenerating waste liquid of developing solution, which have the following beneficial effects:
1. according to the invention, by utilizing the characteristic that the bipolar membrane dissociates water under direct current to generate hydrogen ions and hydroxyl ions and the characteristic that an anion-cation exchange membrane has selective permeability to anions and cations, impurities such as photoresist and the like in the developer solution waste liquid are separated from the alkyl ammonium hydroxide under the action of an external electric driving force to obtain a pure alkyl ammonium hydroxide solution, so that the regeneration of the developer solution is realized, the waste liquid treatment cost is reduced, the ammonia nitrogen discharge in the waste water is reduced, and the resource utilization of the tetraalkylammonium hydroxide is improved.
2. According to the invention, the bipolar membrane electrodialysis method is adopted, organic matters such as photoresist and the like do not need to be removed in advance through acid-base neutralization, electrolytic regeneration is also not needed, pure TAAH can be obtained through regeneration of the developing waste liquid in one step, the process is simple, no extra waste is generated, all recovery and regeneration processes are physical recovery operation under normal temperature and normal pressure, and the operation process is green and safe.
Drawings
The above-described characteristics, technical features, advantages and modes of realization of a developer waste liquid recovery and regeneration apparatus and method will be described in detail below with reference to the accompanying drawings.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of a bipolar membrane electrodialysis mechanism according to embodiment 1 of the present invention;
FIG. 3 is a schematic view of a bipolar membrane electrodialysis mechanism according to embodiment 2 of the present invention;
FIG. 4 is a schematic view of a bipolar membrane electrodialysis mechanism according to embodiment 3 of the present invention;
FIG. 5 is a schematic view of a bipolar membrane electrodialysis mechanism according to embodiment 4 of the present invention;
fig. 6 is a schematic view of a bipolar membrane electrodialysis mechanism in example 5 of the present invention.
In the figure: the device comprises a development waste liquid storage tank 10, a bipolar membrane electrodialysis mechanism 20, a first polar liquid chamber a, an electrodialysis compartment b, a second polar liquid chamber c, an anode 201, a cathode 202, a first bipolar membrane 203, an anion exchange membrane 204, a cation exchange membrane 205, a second bipolar membrane 206, a product tank 30 and a waste liquid tank 40.
Detailed Description
The invention will be further illustrated with reference to the following figures 1-6 and examples:
example 1
Referring to fig. 2, in the present embodiment, an anode 201 is a titanium material-coated ruthenium oxide, a cathode 202 is stainless steel, and an electrodialysis compartment b includes a first bipolar membrane 203, an anion exchange membrane 204, a cation exchange membrane 205, and a second bipolar membrane 206, which are arranged in sequence, and is divided into a raw material compartment b2, an intermediate compartment b1, and a product compartment b3;
s1, adding a developing waste liquid into the raw material compartment b2, wherein the waste liquid comprises the following components: 2.4% of tetramethylammonium hydroxide, 0.5% of photoresist and 2000ppm of carbonate;
s2, adding dilute sulfuric acid with the concentration of 2% into the middle partition chamber b1, the first extreme liquid chamber a and the second extreme liquid chamber c;
s3, adding deionized water into the product compartment b3;
s4, the anode 201 and the cathode 202 are connected with a direct current power supply, and the current density is 100A.m -1 Electrodialysis was performed, and after 10 hours the pure TAAH concentration in product compartment b3 was 2.01%, the photoresist content was less than 0.05%, and carbonate was not detected.
Example 2
Referring to fig. 2, in the present embodiment, an anode 201 is a titanium material-coated ruthenium oxide, a cathode 202 is stainless steel, and an electrodialysis compartment b includes a first bipolar membrane 203, an anion exchange membrane 204, a cation exchange membrane 205, and a second bipolar membrane 206, which are arranged in sequence, and is divided into a raw material compartment b2, an intermediate compartment b1, and a product compartment b3;
s1, adding a developing waste liquid into the raw material compartment b2, wherein the waste liquid comprises the following components: 2.4% of tetramethylammonium hydroxide, 0.5% of photoresist and 2000ppm of carbonate;
s2, adding dilute sulfuric acid with the concentration of 2% into the middle partition chamber b1, the first extreme liquid chamber a and the second extreme liquid chamber c;
s3, adding deionized water containing 1% of tetramethyl ammonium hydroxide into the product compartment b3;
s4, the anode 201 and the cathode 202 are connected with a direct current power supply, and the current density is 100A.m -1 Electrodialysis was performed, after 8 hours, with a pure TAAH concentration of 2.81% in the product compartment b3, a photoresist content of less than 0.05% and no carbonate detected.
Example 3
Referring to fig. 2, in the present embodiment, an anode 201 is a titanium material coated ruthenium oxide, a cathode 202 is stainless steel, and an electrodialysis compartment b includes a first bipolar membrane 203, an anion exchange membrane 204, a cation exchange membrane 205, and a second bipolar membrane 206 arranged in sequence, and the electrodialysis compartment b is partitioned into a raw material compartment b2, an intermediate compartment b1, and a product compartment b3;
s1, adding a developing waste liquid into the raw material compartment b2, wherein the waste liquid comprises the following components: 2.4% of tetramethylammonium hydroxide, 0.5% of photoresist and 2000ppm of carbonate;
s2, adding dilute sulfuric acid with the concentration of 2% into the first dipolar liquid chamber a and the second dipolar liquid chamber c;
s3, adding 2% of tetramethylammonium hydroxide into the middle compartment b 1;
s4, adding deionized water into the product compartment b3;
s5, connecting the anode 201 and the cathode 202 with a direct current power supply at a current density of 100A.m -1 Electrodialysis was performed, after 10 hours, with a pure TAAH concentration of 1.95% and a photoresist content of less than 0.05% in the product compartment b3, and no carbonate was detected.
Example 4
Referring to fig. 3, in the present embodiment, an anode 201 is a titanium material coated ruthenium oxide, a cathode 202 is stainless steel, and an electrodialysis compartment b includes a first bipolar membrane 203, an anion exchange membrane 204, a cation exchange membrane 205, and a second bipolar membrane 206, which are arranged in sequence, and is partitioned into a first intermediate compartment b1, a raw material compartment b2, a second intermediate compartment b3, and a product compartment b4;
s1, adding a developing waste liquid into the raw material compartment b2, wherein the waste liquid comprises the following components: 2.4% of tetramethylammonium hydroxide, 0.5% of photoresist and 2000ppm of carbonate;
s2, adding dilute sulfuric acid with the concentration of 2% into the first middle chamber b1, the first extreme liquid chamber a and the second extreme liquid chamber c;
s3, adding 2% tetramethyl ammonium hydroxide into the second middle chamber b3;
s4, adding deionized water into the product compartment b4;
s5, connecting the anode 201 and the cathode 202 with a direct current power supplyAt a current density of 100A.m -1 Electrodialysis was performed, and after 10 hours the pure TAAH concentration in product compartment b3 was 1.98%, no resist was detected and no carbonate was detected.
Example 5
Referring to fig. 4, in the present embodiment, an anode 201 is a titanium material-coated ruthenium oxide, a cathode 202 is stainless steel, and an electrodialysis compartment b includes a first bipolar membrane 203, an anion exchange membrane 204, a cation exchange membrane 205, and a second bipolar membrane 206, which are arranged in sequence, and is divided into a first intermediate chamber b1, a second intermediate chamber b2, a raw material chamber b3, and a product compartment b4;
s1, adding a developing waste liquid into the raw material compartment b3, wherein the waste liquid comprises the following components: 2.4% of tetramethylammonium hydroxide, 0.5% of photoresist and 2000ppm of carbonate;
2, adding dilute sulfuric acid with the concentration of 2% into the first intermediate chamber b1, the second intermediate chamber b2, the first polar liquid chamber a and the second polar liquid chamber c;
s3, adding deionized water into the product compartment b4;
s4, the anode 201 and the cathode 202 are connected with a direct current power supply, and the current density is 100A.m -1 Electrodialysis was performed, and after 10 hours the pure TAAH concentration in the product compartment b3 was 2.01%, no resist was detected and no carbonate was detected.
According to the device and the method for recycling and regenerating the waste developing solution, provided by the invention, by utilizing the characteristics that the bipolar membrane dissociates water under direct current to generate hydrogen ions and hydroxyl ions and the characteristics that the anion and cation exchange membranes have selective permeability to anions and cations, impurities such as photoresist and the like in the waste developing solution are separated from alkyl ammonium hydroxide under the action of external electric driving force, so that a pure alkyl ammonium hydroxide solution is obtained, the regeneration of the developing solution is realized, the waste solution treatment cost is reduced, the ammonia nitrogen discharge in the waste water is reduced, and the resource utilization of the tetraalkyl ammonium hydroxide is improved;
and the bipolar membrane electrodialysis method is adopted, organic matters such as photoresist and the like do not need to be removed in advance through acid-base neutralization, electrolytic regeneration is also not needed, the pure TAAH can be obtained through the regeneration of the developing waste liquid in one step, the process is simple, no extra waste is generated, all the recycling and regenerating processes are physical recycling operation under normal temperature and normal pressure, and the operation process is green and safe.
In the description of the present invention, it should be noted that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The utility model provides a developer solution waste liquid retrieves regenerating unit, which characterized in that, including bipolar membrane electrodialysis mechanism (20) that is used for retrieving regeneration development waste liquid, wherein, bipolar membrane electrodialysis mechanism (20) are including handling the cell body, contain first utmost point liquid chamber (a), electrodialysis compartment (b), second utmost point liquid chamber (c) that set gradually in handling the cell body at least to carry out developer solution cation migration recombination under the drive of applied electric field and obtain regeneration pure TAAH.
2. The developer waste liquid recovery and regeneration apparatus according to claim 1, wherein: the device also comprises a developing waste liquid storage tank (10) for receiving and containing the developing waste liquid, a product tank (30) for containing pure TAAH, and a waste liquid tank (40) for containing secondary waste liquid generated by treating the developing waste liquid.
3. The developer waste liquid recovery and regeneration apparatus according to claim 1, wherein: the number of the electrodialysis compartments (b) is multiple, and the electrodialysis compartments (b) at least comprise a first bipolar membrane (203), an anion exchange membrane (204), a cation exchange membrane (205) and a second bipolar membrane (206) which are sequentially arranged;
an intermediate compartment (b 1) into which an electrolyte-containing aqueous solution is injected is formed between the first bipolar membrane (203) and the anion exchange membrane (204);
a raw material compartment (b 2) injected with development waste liquid is formed between the anion exchange membrane (204) and the cation exchange membrane (205);
the cation exchange membrane (205) and the second bipolar membrane (206) form a product compartment (b 3) filled with deionized water/pure TAAH-containing aqueous solution.
4. The developer waste liquid recovery and regeneration apparatus according to claim 3, wherein: the groove body space of the first bipolar membrane (203) on the side departing from the second bipolar membrane (206) forms a first bipolar liquid chamber (a), an anode (201) is arranged in the first bipolar liquid chamber (a), and electrolyte-containing aqueous solution is injected.
5. The developer waste liquid recovery and regeneration apparatus according to claim 4, wherein: the tank space on the side of the second bipolar membrane (206) away from the first bipolar membrane (203) forms a second bipolar chamber (c), and a cathode (202) is arranged in the second bipolar chamber (c) and is filled with electrolyte-containing aqueous solution.
6. The developer waste liquid recovery and regeneration apparatus according to claim 5, wherein: the electrolyte-containing aqueous solution in the first polar liquid chamber (a) and the second polar liquid chamber (c) may be the same or different from the electrolyte-containing aqueous solution in the intermediate compartment, and the electrolyte-containing aqueous solution may be sulfuric acid, sodium sulfate, sodium chloride, sodium hydroxide or pure TAAH.
7. The developer waste liquid recovery and regeneration apparatus according to claim 3, wherein: a plurality of anion exchange membranes (204) or cation exchange membranes (205) are arranged between the first bipolar membrane (203) and the anion exchange membranes (204) to form a plurality of intermediate compartments (b 1).
8. The developer waste liquid recovery and regeneration apparatus according to claim 3, wherein: a plurality of anion exchange membranes (204) or cation exchange membranes (205) are arranged between the cation exchange membrane (205) and the second bipolar membrane (206) to form a plurality of intermediate compartments (b 1).
9. A method for recycling and regenerating the waste developer solution based on the device for recycling and regenerating the waste developer solution according to any one of claims 1 to 8, comprising the steps of:
s1, sequentially dividing a first polar liquid chamber (a), an electrodialysis compartment (b) and a second polar liquid chamber (c) in a treatment tank body, and dividing a middle compartment, a raw material compartment and a product compartment in the electrodialysis compartment (b);
s2, injecting an electrolyte-containing aqueous solution into the middle compartment, the first polar liquid compartment (a) and the second polar liquid compartment (c), injecting a development waste liquid into the raw material compartment, and injecting deionized water or a pure TAAH-containing aqueous solution into the product compartment;
s3, simultaneously starting the anode (201) and the cathode (202) in the first polar liquid chamber (a) and the second polar liquid chamber (c), and transferring the positive ions of the developing liquid in the developing waste liquid into the product compartment to be combined with the hydroxyl generated by the second bipolar membrane for regeneration to obtain pure TAAH;
and S4, transferring and outputting the pure TAAH in the product compartment to a product tank (30) for storage or directly entering a developing process, and transferring and outputting the rest secondary waste liquid to a waste liquid tank (40) for subsequent wastewater treatment.
10. The method for recovering and regenerating the waste developer solution of the device for recovering and regenerating the waste developer solution according to claim 9, wherein: at least one electrodialysis compartment (b) and at least one intermediate compartment in each electrodialysis compartment (b).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210479558.7A CN115159636A (en) | 2022-05-07 | 2022-05-07 | Developing solution waste liquid recycling and regenerating device and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210479558.7A CN115159636A (en) | 2022-05-07 | 2022-05-07 | Developing solution waste liquid recycling and regenerating device and method |
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| CN115159636A true CN115159636A (en) | 2022-10-11 |
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