CN102951761A - Method for recovering waste photoresist stripper - Google Patents
Method for recovering waste photoresist stripper Download PDFInfo
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- CN102951761A CN102951761A CN2012104559792A CN201210455979A CN102951761A CN 102951761 A CN102951761 A CN 102951761A CN 2012104559792 A CN2012104559792 A CN 2012104559792A CN 201210455979 A CN201210455979 A CN 201210455979A CN 102951761 A CN102951761 A CN 102951761A
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Abstract
The invention provides a method for recovering a waste photoresist stripper, in particular a method for recovering the waste photoresist stripper after photoresist remaining on a semiconductor substrate is removed. The method comprises the following steps of: precipitating a main ingredient phenolic novolac resin of the photoresist by two steps under an acidic condition by adopting a proper amount of water to obtain the phenolic novolac resin which can be reused as the photoresist; performing adsorption bleaching by using activated carbon, and removing metal ions; and performing distillation under reduced pressure by two steps to remove low-boiling substances such as moisture and recover a pure photoresist stripper. The method is simple, the use of an expensive organic solvent-resistant filtering membrane or filter is avoided, the industrial recovery of the waste photoresist stripper is facilitated, and the using cost of the photoresist stripper and the photoresist is lowered.
Description
Technical field
The present invention relates to a kind of recovery method of photoresist lift off liquid waste liquid, refer to especially the recovery method of photoresist lift off liquid waste liquid that the photoresist material after developing on the TFT-LCD substrate is removed.
Background technology
Along with developing rapidly of domestic electronics manufacturing industry, the usage quantity of the electronic chemical products such as photoresist lift off liquid also greatly increases.Usually at printed circuit board (PCB); display panels; in the technique manufacturing processedes such as semiconductor integrated circuit; need to pass through repeatedly the operations such as graphic mask irradiation exposure and etching form the multilayer precision at Silicon Wafer or glass substrate microcircuit; form after the microcircuit, further stripping liquid (stripper) will be coated on the microcircuit protection zone photoresist material as mask and remove with photoresist.The composition that industrial employed photoresist lift off liquid mainly is organic amine and polar organic solvent is peeled off by swelling and dissolution mechanism and to be removed photoresist material.Above-mentioned machine amine can comprise monoethanolamine (MEA), N,N-DIMETHYLACETAMIDE (DMAC), N-METHYLFORMAMIDE (NMF), N methyldiethanol amine (MDEA) etc.Above-mentioned polar organic solvent can comprise diethylene glycol dimethyl ether (DGME), diethylene glycol monobutyl ether (BDG), methyl-sulphoxide (DMSO), hydroxyethyl piperazine (NEP) etc.Also produce a large amount of photoresist lift off liquid waste liquids in the time of a large amount of use of photoresist lift off liquid.
Except containing a small amount of macromolecule resin and photosensitizers, major part is the photoresist lift off liquid that recycle value is arranged in the photoresist lift off liquid waste liquid.US Patent No. 7273560 has been announced and has been contained 19.3% monoethanolamine, 77% diethylene glycol monobutyl ether, 3% photoresist material and 0.7% water in the photoresist lift off liquid waste liquid that comprises the combination of monoethanolamine and diethylene glycol monobutyl ether.The photoresist lift off liquid method for recovering waste liquid that prior art extensively adopts normally reclaims most organic composition by thin-film evaporator, can again use as photoresist lift off liquid after reclaim the organic constituent that obtains or dewater through decolouring again etc. processed.Although this method simple flow, in using thin-film evaporator evaporating solvent process, its heat and mass efficient fast-descending after photoresist material concentration acquires a certain degree greatly reduces solvent recuperation efficient, processes energy consumption and significantly raises.And the material demands such as photoresist material residual after the desolventizing are regularly removed it totally, and then affect technological operation efficient.
Except above-mentioned photoresist lift off liquid method for recovering waste liquid, it is the polysulfones of 100-1500 and the method that the compound millimicro filtering membrane (NF film) of polyacrylonitrile is processed photoresist lift off liquid waste liquid with molecular weight cut-off that Chinese patent CN1421398A has also announced a kind of.US Patent No. 20070235132 has been announced at etching product line filtering recovering device has been set, and removes photoresist material by the two steps combination filtration method of gross porosity and pore filter, and photoresist lift off liquid is being produced line cocycle use.Although the recovery and treatment method energy consumption of above-mentioned photoresist lift off liquid waste liquid is lower, but the filtering membrane or the strainer that need expensive organic solvent-resistant type, cause cost to increase, and photoresist material is that polymkeric substance stops up the filter opening on filter membrane or the strainer easily, affects the recovering effect of photoresist lift off liquid waste liquid.
Summary of the invention
The objective of the invention is to provide in order to solve the problems of the technologies described above a kind of photoresist lift off liquid method for recovering waste liquid, the method is not only separated photoresist material component contained in the photoresist lift off liquid waste liquid and photoresist lift off fluid component, make its isolate be applied to again suitability for industrialized production, and have technique simply with separate efficient characteristics.
Technical solution of the present invention is:
A kind of recovery method of photoresist lift off liquid waste liquid comprises the steps:
Step 1 adds high purity water in photoresist lift off liquid waste liquid, mix, and the sedimentation and filtration that produces is separated, and obtains the linear phenolic resin of solid phase and the one-level filtrate of liquid phase.
Step 2 adds acidic substance in described one-level filtrate, its pH value is transferred to 1～7, and the sedimentation and filtration that produces is separated, and obtains the linear phenolic resin of solid phase and the secondary filtrate of liquid phase.
Step 3 is processed described secondary filtrate by sorbent material, and adsorption bleaching is also removed metal ion, obtains elementary regenerated liquid.
Step 4 is distilled processing to described elementary regenerated liquid, obtains photoresist lift off liquid.
Further, the photoresist lift off liquid waste liquid in the described step 1 and the mass ratio of high purity water are 0.1～10 ︰ 1, preferred 0.3～5 ︰ 1.
Further, the acidic substance that add in the described step 2 are mineral acid, organic acid or sour gas, and described mineral acid comprises sulfuric acid, hydrochloric acid, nitric acid, carbonic acid, phosphoric acid, or solid super-strong acid; Described organic acid comprises vinylformic acid, acetic acid, oxalic acid, trifluoroacetic acid, methylsulphonic acid, sulfonic acid, thionamic acid, citric acid or thionothiolic acid; Described sour gas comprises carbonic acid gas or sulfurous gas.
Further, in the described step 2, the pH value of regulating one-level filtrate is preferably 5～7.
Further, the sorbent material in the described step 3 comprises gac, polymeric adsorbent or ion chelating agent, and described polymeric adsorbent is preferably the ion exchange resin with benzene ring structure.
Again further, the distillation of described step 4 is treated to vacuum distillation method, comprises the steps: ⑴ temperature 60～100
oC, pressure 1.01 * 10
2Pa～1.01 * 10
4Under the Pa condition, distillation is collected and is obtained low-boiling-point substance impurity; ⑵ temperature 140～200
oC, pressure 1.01 * 10
2Pa～1.01 * 10
4Under the Pa condition, distillation is collected and is obtained described photoresist lift off liquid.
The present invention is through precipitating, adsorb and distill three kinds of separate modes; efficiently photoresist material component and photoresist lift off fluid component are separated from photoresist lift off liquid waste liquid; the method technique is simple; avoid using expensive organic solvent-resistant filtering membrane or strainer; be conducive to large-scale industrialization and reclaim photoresist lift off liquid waste liquid, reduce the use cost of photoresist lift off liquid and photoresist material.
Description of drawings
Fig. 1 is the schema of the recovery method of photoresist lift off liquid waste liquid of the present invention;
Fig. 2 is the effect contrast figure of the recovery method of photoresist lift off liquid waste liquid of the present invention.
Embodiment
Present most widely used photoresist material is ultraviolet positive photoresist, and its main component is linear phenolic resin and sensitizer.Azo effect after the exposure between sensitizer molecule and the linear phenolic resin is destroyed, the sensitizer molecule produces hydroxy-acid group, exposure region forms the alkali soluble part and can remove in developing process, the unexposed area then can't be dissolved in the alkaline-based developer, it need to after the metal pattern etching, adopt photoresist lift off liquid that it is peeled off.In the stripping process, the organic amine in the photoresist lift off liquid infiltrates through photoresist material, causes the photoresist material swelling, and under the effect of polar organic solvent, and it is peeled off and then dissolve from substrate the most at last.
The invention provides a kind of recovery method of photoresist lift off liquid waste liquid: at first adopt an amount of water and acidic conditions to divide two step precipitation photoresist material main component linear phenolic resins, obtain linear phenolic resin and can be used for other industrial circle; Then utilize the charcoal absorption decolouring and remove metal ion; Finally by the dual-step type underpressure distillation, remove the low boiling substances such as moisture, reclaim and obtain pure photoresist lift off liquid.
Fig. 1 is the schema of the recovery method of photoresist lift off liquid waste liquid of the present invention, and the discharge port of waste liquid tank a, tank b and acid tank c all is connected to the first opening for feed of tempering tank d, and the discharge port of tempering tank d is connected to the opening for feed of strainer e; The discharge port of strainer e is connected with the first pump f, and the power that produces by the first pump f will be sent to next device through the flowing material after the filter e filtration; The first pump f has two discharge ports, and its first discharge port connects back the second opening for feed of tempering tank d, and its second discharge port is connected to the opening for feed of adsorption tower g; The discharge port of adsorption tower g is connected to the opening for feed of the second pump h, and the discharge port of the second pump h is connected to the opening for feed of rectifying tower i; The first discharge port of rectifying tower i is connected with condenser j, and the other end of condenser j connects pan tank k.
Corresponding to Fig. 1, operating process of the present invention is:
(1) in tempering tank d, adds photoresist lift off liquid waste liquid by waste liquid tank a, in tank b, add high purity water, in the tempering tank d that photoresist lift off liquid waste liquid is housed, inject high purity water by it, wherein the mass ratio of photoresist lift off liquid waste liquid and high purity water is 0.2～5 ︰ 1, fully mix the turbid solution that obtains containing precipitation, this turbid solution enters into strainer e, e separates sedimentation and filtration via strainer, obtain the linear phenolic resin of solid phase and the one-level filtrate of liquid phase, linear phenolic resin can collect again and use as photoresist material.
(2) one-level filtrate comes back to tempering tank d through the first pump f, and the sulfuric acid strong solution enters into tempering tank d from acid tank c, and the pH value of one-level filtrate is transferred to 5～7, and one-level filtrate becomes the muddy precipitation that produces.The one-level filtrate that to contain precipitation enters into strainer e, and e separates sedimentation and filtration via strainer, obtains the linear phenolic resin of solid phase and the secondary filtrate of liquid phase, and linear phenolic resin can collect as other industrial circle.
(3) secondary filtrate enters adsorption tower g through the first pump f, and after processing through charcoal absorption in the tower, adsorption bleaching and the metal ion in the secondary filtrate of going out obtain elementary regenerated liquid.Can also select other sorbent material in the adsorption tower g, such as polymeric adsorbent or ion chelating agent.
(4) elementary regenerated liquid enters rectifying tower i via the power of the second pump h and carries out underpressure distillation, and pressure-controlling is 1.01 * 10
3Pa is in temperature 70～80
oIn the C scope, distillation duration 1～4h reclaims collection and obtains the low impurity l that boil such as moisture.Then further heat up, in temperature 160～180
oUnder the C condition, distillation duration 2～5h, cut enters pan tank k recovery through condenser j and obtains photoresist lift off liquid, can collect residue m such as obtaining photoresist material by rectifying tower i bottom, adopts the measurement of platinum cobalt colorimetry to reclaim the photoresist lift off liquid colourity that obtains to be＜20Hazen.
Fig. 2 is that the present invention reclaims the photoresist lift off liquid that obtains and the effect contrast figure of photoresist lift off liquid waste liquid, can find out obviously that reclaiming the photoresist lift off liquid purity that obtains is better than photoresist lift off liquid purity in the photoresist lift off liquid waste liquid.
Below in conjunction with specific examples technical solution of the present invention is described further, for embodiment only be typical case, help to understand better this case of the technology of the present invention, the interest field claimed to the present invention do not constitute any limitation.
Embodiment 1
Add the 100g high purity water in 200g photoresist lift off liquid waste liquid, fully mixed precipitation obtains one-level filtrate behind the sedimentation and filtration.Regulating one-level filtrate pH value with sulfuric acid strong solution (60wt%) is 7, and one-level filtrate produces precipitation, further its filtering separation is obtained secondary filtrate.Secondary filtrate obtains the about 290g of elementary regenerated liquid after charcoal absorption is processed.This elementary regenerated liquid is carried out underpressure distillation, and pressure-controlling is 1.01 * 10
3Pa is at first in temperature 80
oObtain the low-boiling-point substance impurity such as moisture under the C condition behind the distillation 2h, then adjusting temperature is 180
oC can obtain photoresist lift off liquid 160g behind the distillation 3h, and surveying its colourity is 15Hazen.
Embodiment 2
Add the 200g high purity water in 200g photoresist lift off liquid waste liquid, fully mixed precipitation obtains one-level filtrate behind the sedimentation and filtration.Regulating one-level filtrate pH value by adding sulfuric acid strong solution (60wt%) is 5, produces precipitation in the one-level filtrate, will get secondary filtrate after its filtering separation.Secondary filtrate adopts gac that it is carried out adsorption treatment, obtains the about 392g of elementary regenerated liquid.Elementary regenerated liquid is carried out underpressure distillation, and pressure-controlling is 1.01 * 10
3Pa at first controls temperature 70
oC obtains the low-boiling-point substance impurity such as moisture behind the distillation 3h, then be warming up to 160
oC obtains photoresist lift off liquid 170g behind the distillation 5h, and surveying its colourity is 10Hazen.
Claims (10)
1. the recovery method of a photoresist lift off liquid waste liquid is characterized in that comprising the steps:
Step 1 adds high purity water in photoresist lift off liquid waste liquid, mix, and the sedimentation and filtration that produces is separated, and obtains the linear phenolic resin of solid phase and the one-level filtrate of liquid phase;
Step 2 adds acidic substance in described one-level filtrate, its pH value is transferred to 1～7, and the sedimentation and filtration that produces is separated, and obtains the linear phenolic resin of solid phase and the secondary filtrate of liquid phase;
Step 3 is processed described secondary filtrate by sorbent material, and adsorption bleaching is also removed metal ion, obtains elementary regenerated liquid;
Step 4 is carried out underpressure distillation to described elementary regenerated liquid and is processed, and obtains photoresist lift off liquid.
2. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: the photoresist lift off liquid waste liquid in the described step 1 and the mass ratio of high purity water are 0.1～10 ︰ 1.
3. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: the photoresist lift off liquid waste liquid in the described step 1 and the mass ratio of high purity water are 0.3～5 ︰ 1.
4. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: the acidic substance that add in the described step 2 are mineral acid, and described mineral acid comprises sulfuric acid, hydrochloric acid, nitric acid, carbonic acid, phosphoric acid, or solid super-strong acid.
5. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: the acidic substance that add in the described step 2 are organic acid, and described organic acid comprises vinylformic acid, acetic acid, oxalic acid, trifluoroacetic acid, methylsulphonic acid, sulfonic acid, thionamic acid, citric acid or thionothiolic acid.
6. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: the acidic substance that add in the described step 2 are sour gas, and described sour gas comprises carbonic acid gas or sulfurous gas.
7. the recovery method of photoresist lift off liquid waste liquid according to claim 1 is characterized in that: in the described step 2, the pH value of regulating one-level filtrate is 5～7.
8. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: the sorbent material in the described step 3 is gac, polymeric adsorbent or ion chelating agent.
9. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: described polymeric adsorbent is the ion exchange resin with benzene ring structure.
10. the recovery method of photoresist lift off liquid waste liquid according to claim 1, it is characterized in that: the distillation of described step 4 is treated to vacuum distillation method, comprises the steps:
⑴ temperature 60～100
oC, pressure 1.01 * 10
2Pa～1.01 * 10
4Under the Pa condition, distillation is collected and is obtained low-boiling-point substance impurity;
⑵ temperature 140～200
oC, pressure 1.01 * 10
2Pa～1.01 * 10
4Under the Pa condition, distillation is collected and is obtained described photoresist lift off liquid.
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| CN2012104559792A CN102951761A (en) | 2012-11-14 | 2012-11-14 | Method for recovering waste photoresist stripper |
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| CN2012104559792A CN102951761A (en) | 2012-11-14 | 2012-11-14 | Method for recovering waste photoresist stripper |
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