CN110314555B - Cleaning agent and cleaning method for developing solution filter - Google Patents
Cleaning agent and cleaning method for developing solution filter Download PDFInfo
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- CN110314555B CN110314555B CN201910684060.2A CN201910684060A CN110314555B CN 110314555 B CN110314555 B CN 110314555B CN 201910684060 A CN201910684060 A CN 201910684060A CN 110314555 B CN110314555 B CN 110314555B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/04—Backflushing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/162—Use of acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/164—Use of bases
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Abstract
The invention relates to the technical field of filter cleaning, in particular to a cleaning agent and a cleaning method for a developing solution filter. In the acid washing process, the micelle impurities can be contracted, so that the gap between the micelle impurities and the filter hole is enlarged, the permeation of the cleaning agent A and the subsequent cleaning agent B is facilitated, the micropores of the membrane are more sufficiently washed, and meanwhile, the oxidation effect of hydrogen peroxide can be improved by the heating and soaking of the cleaning agent A, and the micelle impurities are oxidized into smaller particles, so that the micelle impurities are prevented from being hardened and adhered to the wall of the filter hole. In the alkaline washing process, colloidal particles can be expanded under the condition that a small amount of small acid-washed particles still remain in the ceramic membrane, so that the contact area between the colloidal particles and water flow is increased, and the washing effect is improved; in addition, under the actions of NaClO, sodium dodecyl benzene sulfonate and disodium ethylene diamine tetraacetate and temperature rise soaking, the expanded colloidal particles can not be agglomerated, and the membrane flux can be easily recovered by back washing operation.
Description
Technical Field
The invention relates to the technical field of filter cleaning, in particular to a cleaning agent and a cleaning method for a developing solution filter.
Background
The PCB dry film developer generally comprises metol, hydroquinone, sodium carbonate, sodium hypochlorite, water and the like. The main purpose of using the developer is to remove ink that has been crosslinked by not being irradiated with ultraviolet light. The chemical structure reaction formula of the printing ink during developing and processing is as follows:
the chemical structure reaction formula shows that sodium bicarbonate and resin micelle impurities are generated after development. Therefore, when the ceramic membrane is used for filtration, the sodium bicarbonate is recycled, the resin micelle impurities and other inorganic dirt are intercepted, and the resin micelle impurities and other inorganic dirt gradually block the micropores of the membrane along with the use of the ceramic membrane.
In order to recover the flux of the ceramic membrane, the common methods include acid washing, such as dilute hydrochloric acid and dilute sulfuric acid, and alkali washing, such as sodium hydroxide, and proper chelating agent and surfactant are matched to improve the cleaning effect. However, the above method still has a poor cleaning effect.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a cleaning agent and a cleaning method for a developing solution filter, which can completely recover the membrane flux of a ceramic membrane.
The purpose of the invention is realized by the following technical scheme:
a cleaning agent for a developing solution filter comprises a cleaning agent A and a cleaning agent B;
the cleaning agent A comprises the following components: h2SO41-3wt％、H2O21-3 wt% per mill, and the balance of water;
the cleaning agent B comprises the following components: NaClO3-5 wt%, sodium dodecyl benzene sulfonate 1-3 wt%, disodium ethylene diamine tetraacetate 0.5-1.5 wt%, and water for the rest.
The applicant finds that the micelle shrinkage volume of the developer solution dirt blocking object blocking the ceramic membrane is reduced and hardened under an acidic condition, when the developer solution dirt blocking object is cleaned by acid by adopting the traditional chemical cleaning method, the artifact of membrane flux recovery is caused, in fact, the dirt blocking micelle impurities are not cleaned out, and the membrane flux is rapidly reduced when the developer solution dirt blocking object is reused; the developer solution dirt blocking the ceramic membrane is easy to expand and agglomerate into flocculent micelles under the alkaline condition, and the flocculent micelles can be flushed out by matching with proper flushing, but partial large micelles still remain, so that the membrane flux recovery effect after cleaning is poor.
The utility model provides a cleaner A can make micelle impurity shrink to the clearance grow of micelle impurity and filtration pore is favorable to cleaner A and follow-up cleaner B's infiltration, carries out more abundant washing to the membrane micropore, and the effect of hydrogen peroxide also can be with micelle impurity oxidation to littleer granule simultaneously, thereby avoids its sclerosis and adhesion on filtering the pore wall.
According to the cleaning agent B, colloidal particles can be expanded under the condition that a small amount of small acid-washed particles still remain in the ceramic membrane, so that the contact area between the colloidal particles and water flow is increased, and the washing effect is improved; in addition, under the action of NaClO, sodium dodecyl benzene sulfonate and disodium ethylene diamine tetraacetate, the expanded colloid particles can not be agglomerated, so that the colloid of the ceramic membrane can be completely removed, and the membrane flux of the ceramic membrane can be recovered.
More preferably, the cleaning agent A comprises the following components: h2SO42wt％、H2O22 per mill by weight, and the balance of water.
More preferably, the cleaning agent B comprises the following components: NaClO4 wt%, sodium dodecyl benzene sulfonate 2 wt%, disodium ethylene diamine tetraacetate 1 wt%, and water for the rest.
The method for cleaning the developing solution filter comprises the following steps:
(1) primary water washing: flushing the filter assembly with clean water and then emptying the water;
(2) acid washing: washing the filter assembly forward by using a cleaning agent A, then heating and soaking, and finally washing backward;
(3) and (3) secondary water washing: emptying the cleaning agent A in the step (2), then washing the filter assembly by using clear water, and then emptying water;
(4) alkali washing: washing the filter assembly forward by using a cleaning agent B, then heating and soaking, and finally washing backward;
(5) and (3) washing for the third time: and (4) emptying the cleaning agent B in the step (4), then washing the filter assembly by using clean water, and then emptying the water.
In the acid washing process, the micelle impurities can be contracted, so that the gap between the micelle impurities and the filter hole is enlarged, the permeation of the cleaning agent A and the subsequent cleaning agent B is facilitated, the membrane micropore is more sufficiently washed, meanwhile, the micelle can be softened by heating and soaking the cleaning agent A, the oxidation effect of hydrogen peroxide is improved, the micelle impurities are oxidized into smaller particles, the micelle impurities are prevented from being hardened and adhered to the wall of the filter hole, and most of the micelle subjected to contraction and oxidation is carried out of the membrane micropore by back flushing.
In the alkaline washing process, colloidal particles can be expanded under the condition that a small amount of small acid-washed particles still remain in the ceramic membrane, so that the contact area between the colloidal particles and water flow is increased, and the washing effect is improved; in addition, under the actions of NaClO, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid and temperature rise and immersion, the expanded colloid particles cannot be agglomerated, and by back flushing operation, the colloid after expansion and loosening can be easily brought out of the micropores of the membrane by back flushing, and the membrane flux is recovered.
The multiple washing is to reduce the influence of impurities and pH values on the cleaning effect of the cleaning agent A and the cleaning agent B.
Wherein the filter component is a ceramic membrane filter and a pipeline thereof, and the filtering precision of the ceramic membrane filter is 0.1-0.3 μm.
Wherein in the step (2), the water pressure of the forward flushing and the reverse flushing is 0.3-0.5MPa, and the flushing time is 20-40 min.
In the step (4), the water pressure of the forward flushing and the water pressure of the reverse flushing are both 0.3-0.5MPa, and the flushing time is both 20-40 min.
If the water pressure or time for flushing is too low, the flushing effect cannot be achieved, but if the water pressure exceeds 0.5MPa or the time exceeds 40min, the cleaning effect is not greatly benefited, and only the cost is improved.
Wherein, in the step (2), the temperature-raising soaking treatment comprises the following steps: heating the cleaning agent A to 40-60 ℃, and soaking for 3-5 h.
In the step (4), the temperature-raising soaking treatment comprises the following steps: heating the cleaning agent B to 40-60 ℃, and soaking for 7-9 h.
The ceramic membrane is purified by adopting a combined mode of soaking and washing, and compared with washing, the soaking treatment has the advantages of lower damage capability to the membrane, capability of improving the oxidation degree of micelle to enable the micelle to be small and granular, capability of improving the expansion and loosening degree of colloid particles, capability of improving the contact area of the colloid particles and water flow and better improvement on the purification effect.
The invention has the beneficial effects that:
in the acid washing process, the micelle impurities can be contracted, so that the gap between the micelle impurities and the filter hole is enlarged, the permeation of the cleaning agent A and the subsequent cleaning agent B is facilitated, the membrane micropore is more sufficiently washed, meanwhile, the micelle can be softened by heating and soaking the cleaning agent A, the oxidation effect of hydrogen peroxide is improved, the micelle impurities are oxidized into smaller particles, the micelle impurities are prevented from being hardened and adhered to the wall of the filter hole, and most of the micelle subjected to contraction and oxidation is carried out of the membrane micropore by back flushing.
In the alkaline washing process, colloidal particles can be expanded under the condition that a small amount of small acid-washed particles still remain in the ceramic membrane, so that the contact area between the colloidal particles and water flow is increased, and the washing effect is improved; in addition, under the actions of NaClO, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid and temperature rise and immersion, the expanded colloid particles cannot be agglomerated, and by back flushing operation, the colloid after expansion and loosening can be easily brought out of the micropores of the membrane by back flushing, and the membrane flux is recovered.
Drawings
FIG. 1 is a PCB developer recycling system of example 4;
the reference signs are: 1-developing cylinder, 2-collecting tank, 3-feeding pump, 4-first filter, 5-circulating pump, 6-second filter, 7-clear liquid tank, 8-regeneration liquid tank and 9-quantitative feeding box.
Detailed Description
For the understanding of those skilled in the art, the present invention will be further described with reference to the following examples and the accompanying fig. 1, and the description of the embodiments is not intended to limit the present invention.
Example 1
A cleaning agent for a developing solution filter comprises a cleaning agent A and a cleaning agent B;
the cleaning agent A comprises the following components: h2SO42wt％、H2O22 per mill by weight, and the balance of water;
the cleaning agent B comprises the following components: NaClO4 wt%, sodium dodecyl benzene sulfonate 2 wt%, disodium ethylene diamine tetraacetate 1 wt%, and water for the rest.
The method for cleaning the developing solution filter comprises the following steps:
(1) primary water washing: flushing the filter assembly with clean water and then emptying the water;
(2) acid washing: washing the filter assembly forward by using a cleaning agent A, then heating and soaking, and finally washing backward;
(3) and (3) secondary water washing: emptying the cleaning agent A in the step (2), then washing the filter assembly by using clear water, and then emptying water;
(4) alkali washing: washing the filter assembly forward by using a cleaning agent B, then heating and soaking, and finally washing backward;
(5) and (3) washing for the third time: and (4) emptying the cleaning agent B in the step (4), then washing the filter assembly by using clean water, and then emptying the water.
The filter component is a ceramic membrane filter and a pipeline thereof, and the filtering precision of the ceramic membrane filter is 0.2 mu m.
In the step (2), the water pressure of the forward flushing and the water pressure of the reverse flushing are both 0.4MPa, and the flushing time is both 30 min.
In the step (4), the water pressure of the forward flushing and the water pressure of the reverse flushing are both 0.4MPa, and the flushing time is both 30 min.
Wherein, in the step (2), the temperature-raising soaking treatment comprises the following steps: the temperature of the cleaning agent A is raised to 50 ℃, and the soaking time is 4 hours.
In the step (4), the temperature-raising soaking treatment comprises the following steps: and heating the cleaning agent B to 50 ℃, and soaking for 8 hours.
Example 2
A cleaning agent for a developing solution filter comprises a cleaning agent A and a cleaning agent B;
the cleaning agent A comprises the following components: h2SO41wt％、H2O23 per mill by weight, and the balance of water;
the cleaning agent B comprises the following components: NaClO3 wt%, sodium dodecyl benzene sulfonate 3 wt%, disodium ethylene diamine tetraacetate 1.5 wt%, and water for the rest.
The method for cleaning the developing solution filter comprises the following steps:
(1) primary water washing: flushing the filter assembly with clean water and then emptying the water;
(2) acid washing: washing the filter assembly forward by using a cleaning agent A, then heating and soaking, and finally washing backward;
(3) and (3) secondary water washing: emptying the cleaning agent A in the step (2), then washing the filter assembly by using clear water, and then emptying water;
(4) alkali washing: washing the filter assembly forward by using a cleaning agent B, then heating and soaking, and finally washing backward;
(5) and (3) washing for the third time: and (4) emptying the cleaning agent B in the step (4), then washing the filter assembly by using clean water, and then emptying the water.
Wherein the filter component is a ceramic membrane filter and a pipeline thereof, and the filtering precision of the ceramic membrane filter is 0.1-0.3 μm.
In the step (2), the water pressure of the forward flushing and the water pressure of the reverse flushing are both 0.3MPa, and the flushing time is both 40 min.
In the step (4), the water pressure of the forward flushing and the water pressure of the reverse flushing are both 0.3MPa, and the flushing time is both 40 min.
Wherein, in the step (2), the temperature-raising soaking treatment comprises the following steps: and heating the cleaning agent A to 40 ℃, and soaking for 5 hours.
In the step (4), the temperature-raising soaking treatment comprises the following steps: and heating the cleaning agent B to 40 ℃, and soaking for 9 h.
Example 3
A cleaning agent for a developing solution filter comprises a cleaning agent A and a cleaning agent B;
the cleaning agent A comprises the following components: h2SO43wt％、H2O21 wt% per mill, and the balance of water;
the cleaning agent B comprises the following components: NaClO5 wt%, sodium dodecyl benzene sulfonate 1 wt%, disodium ethylene diamine tetraacetate 0.5 wt%, and water for the rest.
The method for cleaning the developing solution filter comprises the following steps:
(1) primary water washing: flushing the filter assembly with clean water and then emptying the water;
(2) acid washing: washing the filter assembly forward by using a cleaning agent A, then heating and soaking, and finally washing backward;
(3) and (3) secondary water washing: emptying the cleaning agent A in the step (2), then washing the filter assembly by using clear water, and then emptying water;
(4) alkali washing: washing the filter assembly forward by using a cleaning agent B, then heating and soaking, and finally washing backward;
(5) and (3) washing for the third time: and (4) emptying the cleaning agent B in the step (4), then washing the filter assembly by using clean water, and then emptying the water.
The filter component is a ceramic membrane filter and a pipeline thereof, and the filtering precision of the ceramic membrane filter is 0.1 mu m.
In the step (2), the water pressure of the forward flushing and the water pressure of the reverse flushing are both 0.5MPa, and the flushing time is both 20 min.
In the step (4), the water pressure of the forward flushing and the water pressure of the reverse flushing are both 0.5MPa, and the flushing time is both 20 min.
Wherein, in the step (2), the temperature-raising soaking treatment comprises the following steps: the temperature of the cleaning agent A is raised to 60 ℃, and the soaking time is 3 hours.
In the step (4), the temperature-raising soaking treatment comprises the following steps: and heating the cleaning agent B to 60 ℃, and soaking for 7 h.
Comparative example 1 conventional acid cleaning
This comparative example differs from example 1 in that:
the cleaning agent A and the cleaning agent B of example 1 were replaced with 2 wt% diluted hydrochloric acid.
Comparative example 2 Mixed Pickling
This comparative example differs from example 1 in that:
cleaning agent A was used instead of cleaning agent B.
Comparative example 3 Mixed acid cleaning + conventional alkaline cleaning
This comparative example differs from example 1 in that:
the cleaning agent B of example 1 was replaced with a 1 wt% sodium hydroxide solution.
Comparative example 4 Mixed acid cleaning + sodium hydroxide Mixed alkali cleaning
The NaClO in cleaning agent B of example 1 was replaced with 0.5 wt% sodium hydroxide.
Comparative example 5 conventional acid cleaning + Mixed alkali cleaning
This comparative example differs from example 1 in that:
cleaning agent A of example 1 was replaced with 2 wt% dilute hydrochloric acid.
Example 4 Performance testing
As shown in fig. 1, the system for recycling the developer solution of the PCB sequentially comprises a collecting tank 2, a feeding pump 3, a first filter 4, a circulating pump 5, a second filter 6, a clear solution tank 7, a regeneration solution tank 8 and a quantitative feeding box 9 according to the flow direction of the developer solution, wherein the filtering precision of the first filter 4 is 0.8-1.2 μm, the filtering precision of the second filter 6 is 0.1-0.3 μm, and the clear solution tank 7 is provided with a sodium hydroxide feeding port.
Wherein, the first filter 4 is a wire-wound filter, and the filtering precision is 1 μm.
Wherein the second filter 6 is a ceramic membrane filter with the filtration precision of 0.2 μm and the clear water permeation flux per transmembrane pressure difference (MPa) of 10.52m3/(m2·h)。
After the PCB developing solution regeneration recovery system runs for 12 hours, the second filter 6 is cleaned by the cleaning methods of the embodiment 1 and the comparative examples 1-4 respectively, and the clean water permeation flux of the cleaned clean water under the unit transmembrane pressure difference (MPa) is calculated to obtain the clean water permeation flux retention rate, wherein the test results are as follows:
| cleaning type | Retention rate of clear water permeation flux | |
| Example 1 | Mixed acid washing and mixed alkali washing | 99.13％ |
| Comparative example 1 | Conventional acid pickling | 42.21％ |
| Comparative example 2 | Mixed pickling | 55.63％ |
| Comparative example 3 | Mixed acid washing and conventional alkali washing | 58.74％ |
| Comparative example 4 | Mixed acid washing and sodium hydroxide mixed alkaline washing | 62.31％ |
| Comparative example 5 | Conventional acid washing and mixed alkali washing | 53.38％ |
As can be seen from the comparison of the above table, the first acid washing plays a critical role, because the colloid after the conventional acid washing is adopted is hardened, even if the colloid is subsequently washed by the mixed alkali, the colloid still adheres to the inside of the filter pores stubborn, and the membrane flux recovery effect is poorer than that of the mixed acid washing firstly; the recovery of the membrane flux is still not obvious by adopting the conventional sodium hydroxide solution or the sodium hydroxide mixed alkaline washing after the mixed acid washing, because the sodium hydroxide is adopted, the contracted colloid can expand again and agglomerate, and cannot be well washed clean.
In addition, in order to verify that the conventional acid washing can falsely recover the membrane flux, the clean water permeation flux of the ceramic membrane filter cleaned in the comparative example 1 and the comparative example 2 is calculated according to the clean water permeation flux per transmembrane pressure difference (MPa) before the cleaning step (5) is carried out for three times, so that the clean water permeation flux retention rate is obtained, and the test results are as follows:
| cleaning type | Retention rate of clear water permeation flux | |
| Comparative example 1 | Conventional acid pickling | 47.62％ |
| Comparative example 2 | Mixed pickling | 52.85％ |
As can be seen from the above table, the conventional acid-washed ceramic membrane filter suffers from a decrease in the flux of permeate of clean water after being washed again, while the mixed acid wash does not, which demonstrates that the conventional acid wash can falsely restore the flux of the membrane.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (8)
1. A cleaning method of a developing solution filter is characterized in that: cleaning by using a cleaning agent of the developing solution filter:
the cleaning agent comprises a cleaning agent A and a cleaning agent B;
the cleaning agent A comprises the following components: h2SO4 1-3wt％、H2O21-3 wt% per mill, and the balance of water;
the cleaning agent B comprises the following components: 3-5 wt% of NaClO, 1-3 wt% of sodium dodecyl benzene sulfonate, 0.5-1.5 wt% of disodium ethylene diamine tetraacetate and the balance of water;
the cleaning method of the developing solution filter comprises the following steps:
(1) primary water washing: flushing the filter assembly with clean water and then emptying the water;
(2) acid washing: washing the filter assembly forward by using a cleaning agent A, then heating and soaking, and finally washing backward;
(3) and (3) secondary water washing: emptying the cleaning agent A in the step (2), then washing the filter assembly by using clear water, and then emptying water;
(4) alkali washing: washing the filter assembly forward by using a cleaning agent B, then heating and soaking, and finally washing backward;
(5) and (3) washing for the third time: and (4) emptying the cleaning agent B in the step (4), then washing the filter assembly by using clean water, and then emptying the water.
2. The method according to claim 1, wherein the cleaning step comprises: the cleaning agent A comprises the following components: h2SO4 2wt％、H2O22 per mill by weight, and the balance of water.
3. The method according to claim 1, wherein the cleaning step comprises: the cleaning agent B comprises the following components: 4 wt% of NaClO, 2 wt% of sodium dodecyl benzene sulfonate, 1 wt% of disodium ethylene diamine tetraacetate and the balance of water.
4. The method according to claim 1, wherein the cleaning step comprises: the filter component is a ceramic membrane filter and a pipeline thereof, and the filtering precision of the ceramic membrane filter is 0.1-0.3 mu m.
5. The method according to claim 1, wherein the cleaning step comprises: in the step (2), the water pressure of the forward flushing and the water pressure of the backward flushing are both 0.3-0.5MPa, and the flushing time is both 20-40 min.
6. The method according to claim 1, wherein the cleaning step comprises: in the step (4), the water pressure of the forward flushing and the water pressure of the backward flushing are both 0.3-0.5MPa, and the flushing time is both 20-40 min.
7. The method according to claim 1, wherein the cleaning step comprises: in the step (2), the temperature-raising soaking treatment comprises the following steps: heating the cleaning agent A to 40-60 ℃, and soaking for 3-5 h.
8. The method according to claim 1, wherein the cleaning step comprises: in the step (4), the temperature-raising soaking treatment comprises the following steps: heating the cleaning agent B to 40-60 ℃, and soaking for 7-9 h.
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