CN106276814A - The recovery and treatment method of useless persulfate solution - Google Patents
The recovery and treatment method of useless persulfate solution Download PDFInfo
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Abstract
The present invention is to give up persulfate solution recovery and treatment method about one, and it carries out reclaiming and regeneration sulphuric acid and the method for hydrogenperoxide steam generator for the useless persulfate solution (sulphuric acid and mixed solution of hydrogen peroxide) that semiconductor crystal wafer is cleaned.More particularly, it is to remove about a kind of useless photoresistance that waste liquid is remained or metal ion such as aluminium ion, and makes spent solution regeneration become to meet the sulphuric acid of technical grade and the method for hydrogenperoxide steam generator.
Description
Technical field
The present invention is to carry out reclaiming and regeneration sulphuric acid and the method for hydrogenperoxide steam generator by being used for the clean useless persulfate solution (sulphuric acid and mixed solution of hydrogen peroxide) of semiconductor crystal wafer about a kind of.More particularly, it is to remove about a kind of useless photoresistance that waste liquid is remained or metal ion such as aluminium ion, and makes spent solution regeneration become to meet the sulphuric acid of technical grade and the method for hydrogenperoxide steam generator.
Background technology
Printed circuit board (PCB) is complicated due to technique, and uses the treatment agent of multiple different components, can discharge waste water of different nature in each technique.Owing to semiconductor crystal wafer is very sensitive to the existence of micropollutants, in order to reach the target of crystal column surface contamination-free, it is necessary to remove the pollutant on surface and avoid allowing pollutant again remain in crystal column surface before technique.Therefore semiconductor crystal wafer is in the fabrication process, need through surface cleaning step repeatedly, to remove the pollutant of surface attachment, such as impurity such as micronic dust particle (Particle), Organic substance (Organic), inorganic matter metal ions (Metal-Ions).
Wafer current cleaning technique is broadly divided into wet type and the big class of dry type two, still with wet-cleaned method as main flow.Wherein the photoresistance in order to be coated on wafer is peeled off, or it is attached to the organic matter removal of crystal column surface, or it is attached to the removal of the metal etch residue such as aluminum of crystal column surface, SPM [sulphuric acid (Sulfuric Acid) and hydrogen peroxide (Hydrogen Peroxide) mixed solution (Mixing Solutions) claim persulfate solution] wafer ablution need to be used in a large number. its cleaning principle is by producing permonosulphuric acid, and is carbon dioxide (CO by the most useless for Organic substance photoresistance oxidation Decomposition2) and water (H2O), its reaction equation is as follows:
H2SO4+H2O2--->H2SO5+H2O
The useless over cure acid solution that wafer after using is cleaned, making sulphuric acid originally and concentration of hydrogen peroxide reduce, so that being difficult to recycle, the most directly processing with waste chemicals Wei Wai manufacturer.Due to useless persulfuric acid strong acid medicament own, therefore can not discard and need to be neutralized process with substantial amounts of alkali by footpath row, and begin to discard after coagulation Shen Dian processes.
The at present process of useless persulfate solution, most outer manufacturer that processes that all entrust makees the raw material of aluminum sulfate, but the persulfuric acid that gives up be re-used as aluminum sulfate raw material, its process needs to use other a large amount of chemical principle materials, such as aluminium hydroxide [Al (OH)3] react, therefore in the process of useless persulfuric acid, there is the problem needing a large amount of medicaments.
Therefore need badly and to develop, it is possible to useless persulfate solution is changed into the reuse method of technical grade sulphuric acid and hydrogenperoxide steam generator.
Summary of the invention
The present invention is based on the above object, there is provided one useless persulfate solution recovery and treatment method, the waste liquid that persulfuric acid (sulphuric acid and mixed solution of hydrogen peroxide) is cleaned for semiconductor crystal wafer is reclaimed by it, and regeneration meets the sulphuric acid of technical grade and the method for hydrogenperoxide steam generator.
For solving above-mentioned technical problem, the present invention provides a kind of useless persulfate solution recovery and treatment method, it is characterised in that the method is to carry out the useless persulfate solution containing sulphuric acid and hydrogen peroxide reclaiming and regeneration sulphuric acid and the method for hydrogenperoxide steam generator, comprises:
One infrared heating concentrating method, useless persulfuric acid is injected in the reactor being provided with infrared lamp pipe heater, it is not necessary to add any solvent, under conditions of temperature range is-50 DEG C to 330 DEG C and pressure limit 0.1 to 20 atmospheric pressure, reclaims and regenerate and obtain high-concentration sulfuric acid solution；
By the hydrogen peroxide vapor of heated generation and steam through a condenser, cooling is congealed into aqueous hydrogen peroxide solution；And
Collect produced aqueous hydrogen peroxide solution and and black sulfuric acid solution.
In one embodiment of the present of invention, wherein the wavelength of this infrared lamp is 760nm to 1mm.
In one embodiment of the present of invention, wherein this infrared lamp pipe heater is a carbon fiber heaters.
In one embodiment of the present of invention, wherein this infrared lamp pipe heater is an Aludirome (FeCrAl) heater.
In one embodiment of the present of invention, wherein this infrared heating reactor is for being heated to 234 DEG C by this useless persulfate solution from room temperature 14 DEG C.
In one embodiment of the present of invention, it comprises a nanometer scale ceramics film filter purification process further, comprise and the high-concentration sulfuric acid solution of gained is inputted a nanometer scale ceramics film filter via pumping, the impurity such as useless photoresistance of over cure acid solution of giving up with further filtration, or metal ion.
In one embodiment of the present of invention, described method is collectively constituted by described infrared heating concentrating method and described nanometer scale ceramics film filter purification process.
In one embodiment of the present of invention, it comprises the strong acidic ion resin/film ion-exchange purification method of a perfluorinated sulfonic acid polymer further.
In one embodiment of the present of invention, it wraps a regeneration sulfuric acid concentration control method further.
In one embodiment of the present of invention, wherein this impurity includes Organic substance and the multivalent ion of molecular weight ranges more than 450g/ mole.
In one embodiment of the present of invention, wherein the core component of this nanometer scale ceramics film filter is the inorganic ceramic film having excellent heat stability with hole stability, has chemically-resistant strong acid corrosivity.
In one embodiment of the present of invention, it comprises the strong acidic ion resin/film ion-exchange purification method of a perfluorinated sulfonic acid polymer further, by the high-concentration sulfuric acid solution of gained strong acidic ion resin/film by a perfluorinated sulfonic acid polymer, make negative electricity group contained in this resin can adsorb the cation combining in sulfuric acid solution, and make the hydrion (H in resin/film+) intercourse with the cation in sulfuric acid solution, reach to remove aluminium ion or the effect of metal ion.
In one embodiment of the present of invention, it comprises a regeneration sulfuric acid concentration control method, the black sulfuric acid solution that will produce through infrared lamp heating further, mixes with 25% oleum, makes the concentration of black sulfuric acid solution adjust to 98%.
In one embodiment of the present of invention, wherein the sulfuric acid solution of this high concentration is 25% oleum solution.
In one embodiment of the present of invention, described method is collectively constituted by infrared heating concentrating method and black sulfuric acid concentration regulating method.
In one embodiment of the present of invention, it comprises a concentration of hydrogen peroxide control method further, the recovery hydrogenperoxide steam generator that will produce through infrared lamp heating, mixes with the hydrogenperoxide steam generator of high concentration, makes the concentration of recovery hydrogenperoxide steam generator adjust to 30%.
In one embodiment of the present of invention, wherein the hydrogenperoxide steam generator of this high concentration is 50% hydrogenperoxide steam generator.
In one embodiment of the present of invention, described method is collectively constituted by infrared heating concentrating method and concentration of hydrogen peroxide control method.
In one embodiment of the present of invention, described method is by by this infrared heating concentrating method and this black sulfuric acid solution concentration control method, and the strong acidic ion resin/film ion-exchange purification method with a nanometer scale ceramics film filter purification process and/or a perfluorinated sulfonic acid polymer collectively constitutes further.
Accompanying drawing explanation
Fig. 1 is that a preferred embodiments of the present invention utilizes infrared ray (wavelength: 760nm to 1mm) fluorescent tube heater to carry out useless persulfuric acid heating concentration, the flow chart of the method for regeneration high-concentration sulfuric acid and aqueous hydrogen peroxide solution.
Fig. 2 is that a preferred embodiments of the present invention utilizes nanometer scale ceramics film filter to carry out useless persulfuric acid purification, filters the Organic substance and impurity metal ion removed in useless over cure acid solution and obtains the flow chart of the method for the sulfuric acid solution of purification.
Fig. 3 is that a preferred embodiments of the present invention utilizes the strong acidic ion resin/film of perfluorinated sulfonic acid polymer to carry out useless persulfuric acid ion-exchange purification, filters the impurity metal ion removed in useless over cure acid solution and obtains the flow chart of the method for the sulfuric acid solution of purification.
Fig. 4 is the recovery and black sulfuric acid solution produced through infrared lamp heating by useless persulfuric acid and the mixing of 25% oleum, carries out the flow chart of the method for black sulfuric acid concentration regulation.This 25% oleum method can make produced black sulfuric acid concentration regulate to 98%.
Fig. 5 is the recovery produced through infrared lamp heating by useless persulfuric acid and black sulfuric acid solution mixes with the hydrogenperoxide steam generator of high concentration, carries out regenerating the flow chart of the method for concentration of hydrogen peroxide regulation.The method can make to bring back to life concentration of hydrogenperoxide steam generator adjusts to 30%.
Fig. 6 is that infrared heating concentrating method (method (1)) interlinks into one and gives up persulfuric acid concentration and purification system schematic diagram with nanometer scale ceramics film filter purification process (method (2)).
Fig. 7 is infrared heating concentrating method (method (1)) with black sulfuric acid concentration regulating method (method (4)) to interlink into one and gives up persulfuric acid concentration and purification system schematic diagram with concentration of hydrogen peroxide control method (method (5)).
Fig. 8 is infrared heating concentrating method (method (1)) with nanometer scale ceramics film filter purification process (method (2)) and black sulfuric acid concentration regulating method (method (4)) to interlink into one and gives up persulfuric acid concentration and purification system schematic diagram with concentration of hydrogen peroxide control method (method (5)).
Fig. 9 is infrared heating concentrating method (method (1)) with the strong acidic ion resin/film ion-exchange purification method (method (3)) of perfluorinated sulfonic acid polymer and black sulfuric acid concentration regulating method (method (4)) to interlink into one and gives up persulfuric acid concentration and purification system schematic diagram with concentration of hydrogen peroxide control method (method (5)).
Figure 10 is that infrared heating concentrating method (method (1)) sequentially interlinks into one and gives up persulfuric acid concentration and purification system schematic diagram with nanometer scale ceramics film filter purification process (method (2)) with the strong acidic ion resin/film ion-exchange purification method (method (3)) of perfluorinated sulfonic acid polymer.
Figure 11 is that infrared heating concentrating method (method (1)) sequentially interlinks into one and gives up persulfuric acid concentration and purification system schematic diagram with the strong acidic ion resin/film ion-exchange purification method (method (3)) of perfluorinated sulfonic acid polymer with nanometer scale ceramics film filter purification process (method (2)).
Detailed description of the invention
Other characteristics of the present invention and advantage will be illustrated and explanation in following enforcement example further, and this enforcement example is only used as aiding in illustrating, and is not intended to limit the scope of the present invention.
Infrared ray (wavelength: 760nm to 1mm) fluorescent tube is used to carry out the method (method (1)) of useless persulfuric acid heating concentration
Method flow diagram refers to Fig. 1, is injected by useless persulfuric acid in the reactor being equiped with the heaters such as infrared lamp pipe heater, such as carbon fiber or Aludirome (FeCrAl), is not necessary to add any solvent；Aquae hydrogenii dioxidi (150 DEG C) and the water (100 DEG C) of different boiling are heated into hydrogen peroxide vapor and steam；Again via condenser, hydrogen peroxide vapor and water vapor condensation are become aqueous hydrogen peroxide solution；Finally produce and reclaim aqueous hydrogen peroxide solution and recovery and black sulfuric acid solution.This useless persulfate solution inserts infrared heating reactor can be-50 DEG C to 330 DEG C in temperature range, and pressure limit 0.1 to 20 atmospheric pressure is carried out.
A preferred embodiment in the present invention, the useless persulfate solution of acquirement detects its composition through titration method and contains: 70% sulphuric acid, with other 30% containing permonosulphuric acid, hydrogen peroxide and water and the mixed solution of impurity (give up photoresistance on a small quantity, aluminium ion or other a small amount of metal ions).This useless persulfate solution 3200ml is injected the reactor of infrared heating, uses infrared heater that from room temperature 14 DEG C, this useless persulfate solution is heated to 234 DEG C.The hydrogen peroxide vapor and the steam that produce cool down through condenser, obtain 1040ml aqueous hydrogen peroxide solution.Taking this aqueous hydrogen peroxide solution of part and detecting its concentration through titration is 1.61%.In heating process, this permonosulphuric acid temperature raises, and is decomposed by the useless photoresistance of residual spent acid and be oxidized to carbon dioxide (CO2) and water.It addition, after the heating of this useless persulfate solution infrared heater, the recovery of generation and black sulfuric acid solution, detecting its concentration through titration is 96.91%.
Nanometer scale ceramics film filter purification process (method (2))
Method flow diagram refers to Fig. 2, impurity in useless persulfate solution such as useless photoresistance or metal ion such as aluminium ion, filtering useless persulfuric acid impurity via pumping input nanometer scale ceramics film filter, its impurity screening molecular weight ranges is more than 450g/ mole and the multivalent ion of part.The core component inorganic ceramic film of this filter, has excellent heat stability and hole stability, and not only intensity is high and chemically-resistant strong acid corrodes such as useless persulfate solution, and cleaning and regeneration performance is good, has both the two-fold advantage having high efficiency filter with secondary filter.
A preferred embodiment in the present invention, obtain useless persulfate solution to detect its composition through titration method and contain: 70% sulphuric acid and other 30% containing permonosulphuric acid, hydrogen peroxide and water and impurity, (give up photoresistance on a small quantity, aluminium ion or other a small amount of metal ions) mixed solution, detecting its metal ion through ICP-MS instrument, the most most compositions is aluminium ion (content is 280ppm).The useless persulfuric acid of 55 liters are filtered via glandlesspump Pu, suction nanometer scale ceramics film.Through repeatedly ceramic membrane filter, former containing the 280ppm aluminum ions spent acid filtration the most only aluminum ions acid pickle Han 137ppm, aluminium ion clearance is 51%.
The strong acidic ion resin of perfluorinated sulfonic acid polymer/film ion-exchange purification method (method (3))
Method flow diagram refers to Fig. 3, and in useless persulfuric acid, metal ion (aluminium ion or other metal ions) is via the strong acidic ion resin/film of perfluorinated sulfonic acid polymer, and it contains substantial amounts of strong acid group such as sulfonic group (-SO3H), in useless persulfate solution, hydrion (H is easily dissociateed+).Negative electricity group (-SO after resin/film dissociates, contained by body3 -) the useless persulfate solution cationic (such as aluminium ion and other metal ions) of combination can be adsorbed.Its reaction makes the hydrion (H in resin/film+) intercourse with the metal cation in waste acid liquor, reach to remove aluminium ion and the effect of gold Pterostyrax ion.The dissociation capability of highly acidic resin/film is very strong, therefore all can dissociate at acid solution and produce ion exchange.
In a preferred embodiment of the present invention, obtain useless persulfate solution through titration method detect its composition containing 70% sulphuric acid and other 30% containing permonosulphuric acid, hydrogen peroxide and water and impurity, (give up photoresistance on a small quantity；Aluminium ion or other a small amount of metal ions) mixed solution, detect its metal ion through ICP-MS instrument, contained most composition is aluminium ion (207ppm).Suction pipe is used to be injected by the useless persulfuric acid of 50ml, the test tube of the strong acidic ion resin/film containing perfluorinated sulfonic acid polymer, through rocking concussion, make storng-acid cation exchange resin/film contain certain ion exchange capacity IEC [Ion Exchange Capacity (meq/g)], reach saturated after the most no longer absorption spent acid in metal ion exchange.Exchange with the such as aluminium ion of the metal ion in spent acid through repeatedly strong acidic ion resin/film, make former containing the aluminum ions spent acid of 207ppm, exchange after purification through repeatedly strong acidic ion resin/film, the metal ion in this acid pickle, reduced to 25ppm such as aluminium ion.Aluminium ion clearance in spent acid is 87.92%.
25% oleum concentration regulating method (method (4)) to black sulfuric acid
Method flow diagram refers to Fig. 4, and recovery and black sulfuric acid solution that useless persulfuric acid produces through infrared lamp heating mix with 25% oleum, so as to adjustment gained bring back to life and the concentration of black sulfuric acid is to 98%.
In a preferred embodiment of the present invention, recovery that useless persulfuric acid produces through infrared lamp heating and black sulfuric acid solution, its concentration is 96.9%, it is mixed with 25% oleum, makes the concentration of this recovery and black sulfuric acid adjust to 98%.It is computed, reclaims and its concentration of black sulfuric acid solution is 96.9%, be about 25:1 with 25% oleum mixed proportion.
Also can be to black sulfuric acid after above-mentioned ceramic membrane filter, and/or after the strong acidic ion resin/film ion-exchange purification of above-mentioned perfluorinated sulfonic acid polymer, obtained recovery and the regulation of black sulfuric acid solution concentration.
The hydrogenperoxide steam generator of the high concentration concentration regulating method (method (5)) to regeneration hydrogen peroxide
Method flow diagram refers to Fig. 5, the recovery hydrogenperoxide steam generator produced through infrared lamp heating by useless persulfuric acid, mixes with the hydrogenperoxide steam generator of high concentration, makes recovery adjust to 30% with the concentration of regeneration hydrogenperoxide steam generator.
In a preferred embodiment of the present invention, the recovery hydrogenperoxide steam generator that useless persulfuric acid produces through infrared lamp heating, its concentration is 2.97%, it is mixed with 50% hydrogenperoxide steam generator, and the concentration making this recovery aqueous hydrogen peroxide solution is adjusted to 30%.Being computed, the concentration reclaiming hydrogenperoxide steam generator is 2.97%, is about 1:1.36 with 50% hydrogenperoxide steam generator mixed proportion.
Combination two exemplified below or multiple above-mentioned recovery and renovation process, the useless persulfuric acid concentration interlinked and purification system.
Above-mentioned infrared heating concentrating method (method (1)) interlinks into one and gives up persulfuric acid concentration and purification system with above-mentioned nanometer scale ceramics film filter purification process (method (2)), as shown in Figure 6.
Above-mentioned infrared heating concentrating method (method (1)) and above-mentioned black sulfuric acid concentration regulating method (method (4)) interlink into one and give up persulfuric acid concentration and purification system with concentration of hydrogen peroxide control method (method (5)), as shown in Figure 7.
Above-mentioned infrared heating concentrating method (method (1)) and above-mentioned nanometer scale ceramics film filter purification process (method (2)) and above-mentioned black sulfuric acid concentration regulating method (method (4)) interlink into one and give up persulfuric acid concentration and purification system with concentration of hydrogen peroxide control method (method (5)), as shown in Figure 8.
Above-mentioned infrared heating concentrating method (method (1)) and the strong acidic ion resin of above-mentioned perfluorinated sulfonic acid polymer/film ion-exchange purification method (method (3)) and above-mentioned black sulfuric acid concentration regulating method (method (4)) interlink into one and give up persulfuric acid concentration and purification system with concentration of hydrogen peroxide control method (method (5)), as shown in Figure 9.
Above-mentioned infrared heating concentrating method (method (1)) sequentially interlinks into one and gives up persulfuric acid concentration and purification system with above-mentioned nanometer scale ceramics film filter purification process (method (2)) with the strong acidic ion resin/film ion-exchange purification method (method (3)) of above-mentioned perfluorinated sulfonic acid polymer, as shown in Figure 10.
Above-mentioned infrared heating concentrating method (method (1)) sequentially interlinks into one and gives up persulfuric acid concentration and purification system with the strong acidic ion resin of above-mentioned perfluorinated sulfonic acid polymer/film ion-exchange purification method (method (3)) with above-mentioned nanometer scale ceramics film filter purification process (method (2)), as shown in figure 11.
Other concrete aspects
Whole features disclosed in this specification can be combined in any combination.Then, the individual features disclosed in this specification can be replaced by the alternative features according to identical, equal or similar purpose.Therefore, unless explicitly indicated that separately, disclosed each feature is only the example of a series of coordinate or similar characteristics.
The useless persulfate solution recovery and treatment method of the present invention, is collectively constituted by the nanometer scale ceramics film filter purification process of infrared heating concentrating method sum.
The useless persulfate solution recovery and treatment method of the present invention, it comprises the strong acidic ion resin/film ion-exchange purification method of a perfluorinated sulfonic acid polymer further.
The useless persulfate solution recovery and treatment method of the present invention, it wraps a regeneration sulfuric acid concentration control method further.
The useless persulfate solution recovery and treatment method of the present invention, wherein this impurity includes Organic substance and the multivalent ion of molecular weight ranges more than 450g/ mole.
The useless persulfate solution recovery and treatment method of the present invention, wherein the core component of this nanometer scale ceramics film filter is the inorganic ceramic film having excellent heat stability with hole stability, has chemically-resistant strong acid corrosivity.
The useless persulfate solution recovery and treatment method of the present invention, it comprises the strong acidic ion resin/film ion-exchange purification method of a perfluorinated sulfonic acid polymer further, by the high-concentration sulfuric acid solution of gained strong acidic ion resin/film by a perfluorinated sulfonic acid polymer, make negative electricity group contained in this resin can adsorb the cation combining in sulfuric acid solution, and make the hydrion (H in resin/film+) intercourse with the cation in sulfuric acid solution, reach to remove aluminium ion or the effect of metal ion.
The useless persulfate solution recovery and treatment method of the present invention, it comprises a regeneration sulfuric acid concentration control method, the black sulfuric acid solution that will produce through infrared lamp heating further, mixes with 25% oleum, makes the concentration of black sulfuric acid solution adjust to 98%.
The useless persulfate solution recovery and treatment method of the present invention, wherein the sulfuric acid solution of this high concentration is 25% oleum solution.
The useless persulfate solution recovery and treatment method of the present invention, is collectively constituted by infrared heating concentrating method and black sulfuric acid concentration regulating method.
The useless persulfate solution recovery and treatment method of the present invention, it comprises a concentration of hydrogen peroxide control method further, the recovery hydrogenperoxide steam generator that will produce through infrared lamp heating, mixes with the hydrogenperoxide steam generator of high concentration, makes the concentration of recovery hydrogenperoxide steam generator adjust to 30%.
The useless persulfate solution recovery and treatment method of the present invention, wherein the hydrogenperoxide steam generator of this high concentration is 50% hydrogenperoxide steam generator.
The useless persulfate solution recovery and treatment method of the present invention, is collectively constituted by infrared heating concentrating method and concentration of hydrogen peroxide control method.
The useless persulfate solution recovery and treatment method of the present invention, it comprises a regeneration sulfuric acid concentration control method further.
The useless persulfate solution recovery and treatment method of the present invention, method is by by this infrared heating concentrating method and this black sulfuric acid solution concentration control method, and the strong acidic ion resin/film ion-exchange purification method with a nanometer scale ceramics film filter purification process and/or a perfluorinated sulfonic acid polymer collectively constitutes further.
From aforesaid explanation, practise the basic feature being readily determined the present invention in these those skilled in the art, and without departing under its scope, various changes and the modification of the present invention can be carried out, to be adapted to various different purposes and situation.Therefore, in applying for a patent right and requiring, other concrete aspects are also comprised.
These are only presently preferred embodiments of the present invention, be not able to this and limit the protection domain that the present invention implements that simply equivalence change and the modification that the description of the most all reference present invention is made still belongs to protection scope of the present invention.
Claims (19)
1. a useless persulfate solution recovery and treatment method, it is characterised in that the method is to carry out the useless persulfate solution containing sulphuric acid and hydrogen peroxide reclaiming and regeneration sulphuric acid and the method for hydrogenperoxide steam generator, comprises:
One infrared heating concentrating method, useless persulfuric acid is injected in the reactor being provided with infrared lamp pipe heater, it is not necessary to add any solvent, under conditions of temperature range is-50 DEG C to 330 DEG C and pressure limit 0.1 to 20 atmospheric pressure, reclaims and regenerate and obtain high-concentration sulfuric acid solution；
By the hydrogen peroxide vapor of heated generation and steam through a condenser, cooling is congealed into aqueous hydrogen peroxide solution；And
Collect produced aqueous hydrogen peroxide solution and and black sulfuric acid solution.
Method the most according to claim 1, it is characterised in that wherein the wavelength of this infrared lamp is 760nm to 1mm.
Method the most according to claim 1, it is characterised in that wherein this infrared lamp pipe heater is a carbon fiber heaters.
Method the most according to claim 1, it is characterised in that wherein this infrared lamp pipe heater is an Aludirome (FeCrAl) heater.
Method the most according to claim 1, it is characterised in that wherein this infrared heating reactor is for being heated to 234 DEG C by this useless persulfate solution from room temperature 14 DEG C.
Method the most according to claim 1, it is characterized in that, it comprises a nanometer scale ceramics film filter purification process further, comprise and the high-concentration sulfuric acid solution of gained is inputted a nanometer scale ceramics film filter via pumping, the impurity such as useless photoresistance of over cure acid solution of giving up with further filtration, or metal ion.
Method the most according to claim 6, it is characterised in that described method is collectively constituted by described infrared heating concentrating method and described nanometer scale ceramics film filter purification process.
Method the most according to claim 7, it is characterised in that it comprises the strong acidic ion resin/film ion-exchange purification method of a perfluorinated sulfonic acid polymer further.
9. according to the method described in claim 7 or 8, it is characterised in that it comprises a regeneration sulfuric acid concentration control method further.
Method the most according to claim 6, it is characterised in that wherein this impurity includes Organic substance and the multivalent ion of molecular weight ranges more than 450g/ mole.
11. methods according to claim 6, it is characterised in that wherein the core component of this nanometer scale ceramics film filter is the inorganic ceramic film having excellent heat stability with hole stability, has chemically-resistant strong acid corrosivity.
12. according to the method described in claim 1 or 6, it is characterized in that, it comprises the strong acidic ion resin/film ion-exchange purification method of a perfluorinated sulfonic acid polymer further, by the high-concentration sulfuric acid solution of gained strong acidic ion resin/film by a perfluorinated sulfonic acid polymer, make negative electricity group contained in this resin can adsorb the cation combining in sulfuric acid solution, and make the hydrion (H in resin/film+) intercourse with the cation in sulfuric acid solution, reach to remove aluminium ion or the effect of metal ion.
13. methods according to claim 1, it is characterised in that it comprises a regeneration sulfuric acid concentration control method, the black sulfuric acid solution that will produce through infrared lamp heating further, mixes with 25% oleum, makes the concentration of black sulfuric acid solution adjust to 98%.
14. methods according to claim 13, it is characterised in that wherein the sulfuric acid solution of this high concentration is 25% oleum solution.
15. methods according to claim 13, it is characterised in that described method is collectively constituted by infrared heating concentrating method and black sulfuric acid concentration regulating method.
16. methods according to claim 1, it is characterized in that, it comprises a concentration of hydrogen peroxide control method further, the recovery hydrogenperoxide steam generator that will produce through infrared lamp heating, mix with the hydrogenperoxide steam generator of high concentration, make the concentration of recovery hydrogenperoxide steam generator adjust to 30%.
17. methods according to claim 16, it is characterised in that wherein the hydrogenperoxide steam generator of this high concentration is 50% hydrogenperoxide steam generator.
18. methods according to claim 16, it is characterised in that described method is collectively constituted by infrared heating concentrating method and concentration of hydrogen peroxide control method.
19. methods according to claim 13, it is characterized in that, described method is by by this infrared heating concentrating method and this black sulfuric acid solution concentration control method, and the strong acidic ion resin/film ion-exchange purification method with a nanometer scale ceramics film filter purification process and/or a perfluorinated sulfonic acid polymer collectively constitutes further.
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| CN116282066A (en) * | 2022-12-22 | 2023-06-23 | 复榆(张家港)新材料科技有限公司 | Method for preparing hierarchical-pore high-silicon FAU zeolite from regenerated acidic mother solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116282066A (en) * | 2022-12-22 | 2023-06-23 | 复榆(张家港)新材料科技有限公司 | Method for preparing hierarchical-pore high-silicon FAU zeolite from regenerated acidic mother solution |
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