CN105523598A - Method for recovering photoresist stripping liquid through periodic pressure change of rectification column - Google Patents
Method for recovering photoresist stripping liquid through periodic pressure change of rectification column Download PDFInfo
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- CN105523598A CN105523598A CN201610089438.0A CN201610089438A CN105523598A CN 105523598 A CN105523598 A CN 105523598A CN 201610089438 A CN201610089438 A CN 201610089438A CN 105523598 A CN105523598 A CN 105523598A
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- liquid
- pressure
- photoresist lift
- stripping liquid
- rectification
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- 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
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- 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
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/40—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture or use of photosensitive materials
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/002—Construction details of the apparatus
- C02F2201/007—Modular design
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for recovering a photoresist stripping liquid through periodic pressure change of a rectification column. The method comprises specific steps as follows: (1), activated carbon is added to the photoresist stripping liquid for decoloration and metal ion adsorption, and a primary regenerated liquid is obtained after separation; (2), the primary generated liquid is subjected to normal-pressure rectification, low-vacuum rectification, high-vacuum rectification and a positive-pressure rectification under the protection of nitrogen atmosphere and an antioxidant, and a qualified photoresist stripping liquid product is obtained. The method has the benefits as follows: the method adopts cooperative use of negative pressure, normal pressure and positive pressure, can cope with a solvent with a low boiling point, a solvent with a high boiling point and solvents with the approximate boiling point and can realize good separation effect; with the adoption of the method, a photoresist component and a photoresist stripping liquid component contained in the waste photoresist stripping liquid are separated, separation substances are applied to industrial production again, and the method has the characteristics of simple technology and high separation efficiency.
Description
Technical field
The present invention relates to a kind of method that rectifying tower reclaims, be specifically related to a kind of method that interim variable-pressure rectification tower reclaims photoresist lift off liquid.
Background technology
Along with developing rapidly of domestic electronic manufacture industry, the usage quantity of the electronic chemical products such as photoresist lift off liquid also greatly increases.Also a large amount of photoresist lift off liquid waste liquid is produced while photoresist lift off liquid uses in a large number.Except containing except a small amount of macromolecule resin and photosensitizers in photoresist lift off liquid waste liquid, major part is the photoresist lift off liquid having recycle value, therefore very urgent to the requirement of the recycling of photoresist lift off liquid.
In recent years, the requirement for distillation technology is more and more higher, is mainly being separated completely and the various consumption that bring of high tower rectifying of each component contained by solvent, and the consumption comprising the consumption of raw material and the energy is increasing.Under this overall situation, obtain large benefit in the urgent need to reducing to consume.Mainly the too high heating raw materials of tower height is uneven in the consumption of raw material, easily occurs that raw material becomes the residual result of still, studies the subject matter that raw material drops into immediately, the rapid output of product becomes current needs solution for this reason.
Existing solvent composition separation method is mainly for the atmospheric distillation method of low boiling point solvent and the negative pressure rectificating method for high boiling solvent.Non-pressure process is commonplace, but is not the very high limitation having it for the requirement of equipment, is mainly difficult to get a desired effect to high boiling separated from solvent; Negative pressure method serves very good effect in the separation of high boiling solvent, but very high for the requirement of equipment, need filtering membrane or the strainer of expensive organic solvent-resistant type, cause cost to increase, and it is higher to reclaim stripping liquid water content, affects the recycling effect of photoresist lift off liquid waste liquid.In addition, for the solvent that boiling point is close, aforesaid method is also not enough to be separated.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of interim variable-pressure rectification tower to reclaim the method for photoresist lift off liquid, the method effectively solves existing lower boiling solvent and the defect existing for high boiling solvent, and for the above-mentioned Problems existing such as separation of the close solvent of boiling point.
Technical problem to be solved by this invention realizes by the following technical solutions:
Interim variable-pressure rectification tower reclaims the method for photoresist lift off liquid, and its concrete steps are:
(1) in photoresist lift off liquid, add activated carbon decolorizing and adsorbing metal ions, after being separated, obtain elementary regenerated liquid;
(2) the elementary regenerated liquid of gained obtains photoresist lift off liquid salable product through four rectifying under nitrogen atmosphere and antioxidant protection.
The present invention improves further and is: in described step 2, four rectifying specifically comprises: (1) atmospheric distillation; (2) rough vacuum rectifying; (3) high vacuum rectification; (4) malleation rectifying.
The present invention improves further and is: described atmospheric distillation temperature range value is 79 ~ 86 DEG C.
The present invention improves further and is: described rough vacuum rectification temperature value is 100 DEG C, and low vacuum pressure value is-0.1MPa.
The present invention improves further and is: the atmospheric pressure value in described high vacuum rectification process is-0.06MPa.
The present invention improves further and is: the atmospheric pressure value in described malleation rectifying is 4MPa.
The invention has the beneficial effects as follows: interim transformation is in for some time and changes Rectification column pressure, be beneficial to still internal solvent Component seperation, normal employing normal pressure, negative pressure transform method, the present invention uses malleation, normal pressure, negative pressure three kinds of mapping modes on this basis instead, is well separated to reach each component.The conversion of normal pressure, negative pressure, malleation in tower, namely can Rapid Variable Design when needs, and the change of pressure always drives the change of material component content in still, adjusts pressure change on appropriate opportunity, is conducive to being separated of high content component and low levels component.
The cooperation of negative pressure, normal pressure, malleation three kinds of methods uses, and not only can tackle lower boiling solvent, also can for high boiling solvent, and the solvent close for boiling point also can be tackled, and reaches good separating effect.Photoresist material component contained in photoresist lift off liquid waste liquid and photoresist lift off fluid component are not only separated by the method, make its isolate be applied to suitability for industrialized production again, and have technique simply be separated efficient feature.
Accompanying drawing explanation
Fig. 1 is the inventive method schema.
Wherein: T1-normal pressure, negative pressure tower, T2-pressurizing tower, S01 ~ S12-logistics, E01-preheater, E02, E04-condenser, E03, E05-reboiler, P01, P02-pump.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
Interim variable-pressure rectification tower reclaims the method for photoresist lift off liquid, and its concrete steps are:
(1) in photoresist lift off liquid, add activated carbon decolorizing and adsorbing metal ions, after being separated, obtain elementary regenerated liquid;
(2) the elementary regenerated liquid of gained obtains photoresist lift off liquid salable product through four rectifying under nitrogen atmosphere and antioxidant protection.
In described step 2, four rectifying specifically comprises: (1) atmospheric distillation; (2) rough vacuum rectifying; (3) high vacuum rectification; (4) malleation rectifying.
Rectifying tower is the tower vapor-liquid contacting apparatus of one carrying out rectifying, steam enters by the bottom of tower, the gas phase evaporated and decline liquid carry out counter current contact, two contact, volatile (lower boiling) component in decline liquid constantly shifts in gas phase, difficulty volatilization (high boiling point) component in gas phase constantly shifts in decline liquid, gas phase is more close to tower top, its volatile components concentration is higher, and decline liquid more close at the bottom of tower, its difficult volatiles is more enrichment then, thus reaches the object of Component seperation.The gas phase risen by tower top enters condenser, and a part for the liquid of condensation returns tower top as phegma and enters in rectifying tower, and remaining part is then taken out as distillate.The liquid that tower bottom flow goes out, a part wherein sends into reboiler, and heating evaporation becomes gas phase to return in tower, and another part liquid takes out as still raffinate.
Embodiment one:
Under nitrogen protection, drop into through the stripping liquid solvent 1.8 tons of gac adsorption treatment, moisture content 5%, is slowly warming up to 85 DEG C, removes lower-boiling impurity 50KG under normal pressure; Be raised to (100 DEG C) after certain value until temperature, rough vacuum (-0.1MPa) removes moisture content 60KG; Rear high vacuum (-0.06Pa) remove a small amount of water obtain moisture content lower than 0.1% stripping liquid, after through malleation tower (4MPa) the removing impurity close with finished product boiling point, obtain the stripping liquid finished product that finished product content is more than 99%.
Embodiment two:
Under nitrogen protection, drop into through the stripping liquid solvent 1.9 tons of gac adsorption treatment, moisture content 4%, is slowly warming up to 80 DEG C, removes lower-boiling impurity 56KG under normal pressure; Be raised to (100 DEG C) after certain value until temperature, rough vacuum (-0.1MPa) is except the 70KG that anhydrates; Rear high vacuum (-0.06Pa) removes a small amount of water, obtain moisture content lower than 0.1% stripping liquid, after through malleation tower malleation (4MPa) the removing impurity close with finished product boiling point, obtain the stripping liquid finished product that finished product content is more than 99%.
Embodiment three:
Under nitrogen protection, drop into through the stripping liquid solvent 1.7 tons of gac adsorption treatment, moisture content 4.5%, slowly heat up 79 DEG C, under normal pressure, remove lower-boiling impurity 60KG; Be raised to (100 DEG C) after certain value until temperature, rough vacuum (-0.1MPa) removes moisture content 66KG; Rear high vacuum (-0.06Pa) remove a small amount of water obtain moisture content lower than 0.1% stripping liquid, after through malleation tower malleation (4MPa) the removing impurity close with finished product boiling point, obtain the stripping liquid finished product that finished product content is more than 99%.
Embodiment four:
Under nitrogen protection, drop into through the stripping liquid solvent 1.92 tons of gac adsorption treatment, moisture content 3.5%, is slowly warming up to 86 DEG C, removes lower-boiling impurity 48KG under normal pressure; Be raised to (100 DEG C) after certain value until temperature, rough vacuum (-0.1MPa) removes moisture content 78KG; Rear high vacuum (-0.06Pa) remove a small amount of water obtain moisture content lower than 0.1% stripping liquid, after through malleation tower malleation (4MPa) the removing impurity close with finished product boiling point, obtain the stripping liquid finished product that finished product content is more than 99%.
The invention has the beneficial effects as follows: the method for the invention comprises the cooperation use of negative pressure, normal pressure, malleation three kinds of methods, not only can tackle lower boiling solvent, also can for high boiling solvent, the solvent close for boiling point also can be tackled, and reaches good separating effect.Photoresist material component contained in photoresist lift off liquid waste liquid and photoresist lift off fluid component are not only separated by the method, make its isolate be applied to suitability for industrialized production again, and have technique simply be separated efficient feature.
Utilize the recovery method of the described solvent slop of this invention, save ample resources.Large quantity of moisture under nitrogen atmosphere protection in normal pressure removing stripping liquid, after use negative pressure rectifying instead and be with further and dewater, with obtain water content lower than 0.1% qualified stripping liquid finished product.The energy consumed is more much smaller than simple atmospheric distillation.In addition for the high boiling component that will obtain, malleation rectifying can remove the component close with required component, is like this conducive to the reaction that component carries out next step, has saved the time, also improve benefit than general purification means.
More than show and describe ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. interim variable-pressure rectification tower reclaims the method for photoresist lift off liquid, it is characterized in that: its concrete steps are:
(1) in photoresist lift off liquid, add activated carbon decolorizing and adsorbing metal ions, after being separated, obtain elementary regenerated liquid;
(2) the elementary regenerated liquid of gained obtains photoresist lift off liquid salable product through four rectifying under nitrogen atmosphere and antioxidant protection.
2. interim variable-pressure rectification tower according to claim 1 reclaims the method for photoresist lift off liquid, it is characterized in that: in described step 2, four rectifying specifically comprises: (1) atmospheric distillation; (2) rough vacuum rectifying; (3) high vacuum rectification; (4) malleation rectifying.
3. interim variable-pressure rectification tower according to claim 2 reclaims the method for photoresist lift off liquid, it is characterized in that: described atmospheric distillation temperature range value is 79 ~ 86 DEG C.
4. interim variable-pressure rectification tower according to claim 2 reclaims the method for photoresist lift off liquid, it is characterized in that: described rough vacuum rectification temperature value is 100 DEG C, and low vacuum pressure value is-0.1MPa.
5. interim variable-pressure rectification tower according to claim 2 reclaims the method for photoresist lift off liquid, it is characterized in that: the atmospheric pressure value in described high vacuum rectification process is-0.06MPa.
6. interim variable-pressure rectification tower according to claim 2 reclaims the method for photoresist lift off liquid, it is characterized in that: the atmospheric pressure value in described malleation rectifying is 4MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610089438.0A CN105523598B (en) | 2016-02-17 | 2016-02-17 | The method of interim variable-pressure rectification tower recycling photoresist lift off liquid |
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| CN201610089438.0A CN105523598B (en) | 2016-02-17 | 2016-02-17 | The method of interim variable-pressure rectification tower recycling photoresist lift off liquid |
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| CN105523598A true CN105523598A (en) | 2016-04-27 |
| CN105523598B CN105523598B (en) | 2019-03-05 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242149A (en) * | 2016-08-31 | 2016-12-21 | 惠州市惠阳区力行环保有限公司 | The processing method of useless stripper |
| CN108840495A (en) * | 2018-05-13 | 2018-11-20 | 四川久远化工技术有限公司 | A kind of stripping waste liquor method of purification |
| CN110387158A (en) * | 2019-07-16 | 2019-10-29 | 福建钰融科技有限公司 | With the iron oxide red anticorrosive paint and preparation method thereof of dilution vacuum distillation raffinate preparation |
| CN111170541A (en) * | 2020-01-08 | 2020-05-19 | 安庆市鑫祥瑞环保科技有限公司 | Photoresist stripping liquid waste liquid recovery system |
| CN111807974A (en) * | 2020-08-06 | 2020-10-23 | 江阴市大洋固废处置利用有限公司 | Stripping waste liquid component recovery system and recovery process |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242149A (en) * | 2016-08-31 | 2016-12-21 | 惠州市惠阳区力行环保有限公司 | The processing method of useless stripper |
| CN106242149B (en) * | 2016-08-31 | 2019-11-08 | 惠州市惠阳区力行环保有限公司 | The processing method of useless stripper |
| CN108840495A (en) * | 2018-05-13 | 2018-11-20 | 四川久远化工技术有限公司 | A kind of stripping waste liquor method of purification |
| CN108840495B (en) * | 2018-05-13 | 2020-12-22 | 四川久远化工技术有限公司 | Method for purifying stripping waste liquid |
| CN110387158A (en) * | 2019-07-16 | 2019-10-29 | 福建钰融科技有限公司 | With the iron oxide red anticorrosive paint and preparation method thereof of dilution vacuum distillation raffinate preparation |
| CN110387158B (en) * | 2019-07-16 | 2021-07-16 | 福建钰融科技有限公司 | Iron oxide red antirust paint prepared by using diluent to distill residual liquid under reduced pressure and preparation method thereof |
| CN111170541A (en) * | 2020-01-08 | 2020-05-19 | 安庆市鑫祥瑞环保科技有限公司 | Photoresist stripping liquid waste liquid recovery system |
| CN111807974A (en) * | 2020-08-06 | 2020-10-23 | 江阴市大洋固废处置利用有限公司 | Stripping waste liquid component recovery system and recovery process |
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| CN105523598B (en) | 2019-03-05 |
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