CN105585188A - Method for preparing boron-free ultrapure water - Google Patents
Method for preparing boron-free ultrapure water Download PDFInfo
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- CN105585188A CN105585188A CN201610096592.0A CN201610096592A CN105585188A CN 105585188 A CN105585188 A CN 105585188A CN 201610096592 A CN201610096592 A CN 201610096592A CN 105585188 A CN105585188 A CN 105585188A
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- boron
- resin
- ultra
- ultrapure water
- water
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- 239000012498 ultrapure water Substances 0.000 title claims abstract description 35
- 229910021642 ultra pure water Inorganic materials 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052796 boron Inorganic materials 0.000 claims abstract description 80
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 8
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract description 4
- 150000005846 sugar alcohols Polymers 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 11
- 238000001764 infiltration Methods 0.000 claims description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003957 anion exchange resin Substances 0.000 claims description 6
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 6
- 230000009291 secondary effect Effects 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000006065 biodegradation reaction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- RFSUNEUAIZKAJO-VRPWFDPXSA-N D-Fructose Natural products OC[C@H]1OC(O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-VRPWFDPXSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 235000009508 confectionery Nutrition 0.000 claims description 3
- 229940074391 gallic acid Drugs 0.000 claims description 3
- 235000004515 gallic acid Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 235000010356 sorbitol Nutrition 0.000 claims description 3
- 229960002920 sorbitol Drugs 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- 239000000811 xylitol Substances 0.000 claims description 3
- 238000005374 membrane filtration Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract 1
- 230000000536 complexating effect Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 229920005862 polyol Polymers 0.000 abstract 1
- 150000003077 polyols Chemical class 0.000 abstract 1
- 239000008399 tap water Substances 0.000 abstract 1
- 235000020679 tap water Nutrition 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 4
- 239000004327 boric acid Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000001962 electrophoresis Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4696—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrophoresis
-
- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
-
- 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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/422—Treatment of water, waste water, or sewage by ion-exchange using anionic exchangers
-
- 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
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/04—Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water
Landscapes
- 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)
- Treatment Of Water By Ion Exchange (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a method for preparing boron-free ultrapure water. Tap water is sequentially subjected to ultrafiltration, reverse osmosis, EDI device, UV biological degradation, boron removing process and polishing resin treatment to prepare the boron-free ultrapure water, wherein the boron removing process comprises polyol complexing reverse osmosis boron removing and two-stage boron specific resin boron removing. The ultrapure water has a content of boron element being less than 100PPT and the content of other elements reaching the PPT grade, thereby being ultrapure water with excellent comprehensive performance and an ideal water source for preparing ultrapure chemical materials in the semiconductor industry. The method for preparing boron-free ultrapure water is simple and convenient in process, is easy to implement, and can be used for effectively controlling the content of each substance in the water and reducing process cost by means of combination of multiple treatment methods to prepare high-quality PPT-grade ultrapure water; and a step-wise boron removing process can be used for completely removing tenacious boron impurities in the ultrapure water to overcome the industrial problem, thus being a milestone for ultrapure water development.
Description
Technical field
The present invention relates to water treatment technology field, particularly relate to a kind of preparation method without boron ultra-pure water.
Background technology
In semicon industry, in pure semiconductor product, mix the impurity element of denier, will make the resistivity of product occur to change greatly. For example, in pure boron, mix 1,000,000/-boron element, its resistivity will be reduced to 0.4 Ω cm from 214000 Ω cm quickly, namely the conduction of boron can be for having improved more than 50 ten thousand times. As can be seen here, semicon industry requires high to the degree of purity of chemical material.
Ultra-pure water is to prepare the indispensable raw material of semicon industry ultrapure chemical material used, and its degree of purity directly affects the performance of ultrapure chemical material, thereby is also restricting to a certain extent photosemiconductor industry, the especially development of chip industry.
Boron is the more difficult impurity element of removing in ultra-pure water, and its relatively high content directly affects ultrapure chemical material as the application of super-pure ammonia water in semiconductor product. Existing ultra-pure water mostly adopts pretreatment, reverse osmosis technology, super purification process and rear class to process four large steps, multistage filtering, high-performance ion-exchange unit, ultra filtration filter, uviol lamp, removes the multiple processing methods such as TOC device. But ultra-pure water prepared by existing these methods, its boron content still can not effectively be removed, or does not reach the requirement of ppt level.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method without boron ultra-pure water, can effectively remove the boron element in water, solves existing ultra-pure water preparation technology above shortcomings part.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method without boron ultra-pure water is provided, running water is passed through successively to ultrafiltration, counter-infiltration, EDI device, UV biodegradation, removes boron technique and polishing resin treatment, obtain described without boron ultra-pure water; Wherein, the described boron technique of removing comprises that polyhydric alcohol complex counter-infiltration removes boron and two-stage effects of boron resin removes boron.
In a preferred embodiment of the present invention, the method that described polyhydric alcohol complex counter-infiltration removes boron is: running water, after UV biodegradation is processed, regulates its pH value to acid, then adds wherein a certain amount of polyalcohol, after stirring, removes boron through reverse osmosis membrane filtration.
In a preferred embodiment of the present invention, described pH value is 3~6.5; The addition of described polyalcohol is 1~10ppm/L water.
In a preferred embodiment of the present invention, described polyalcohol is at least one in D-glucitol, sweet mellow wine, D-Fructose and xylitol.
In a preferred embodiment of the present invention, described two-stage effects of boron resin boron removal method is: remove boron by introducing one-level effects of boron resin through polyhydric alcohol complex counter-infiltration except the running water after boron, then the pH value that regulates running water is 8.5~9.5, then introduces secondary effects of boron resin except boron.
In a preferred embodiment of the present invention, described one-level effects of boron resin is gallic acid grafting highly acid anion exchange resin; Described secondary effects of boron resin is 2,3-dihydroxy-6-sodium sulfonate grafting strong-base anion-exchange resin or polyhydroxy amines styrene resin resinoid.
The invention has the beneficial effects as follows: a kind of preparation method without boron ultra-pure water of the present invention, simple process, easily realizes, it is combined and is used by multiple processing method, effectively control the content of each material in water, and reduce process costs, prepare high-quality PPT level ultra-pure water; Removing boron technique by substep, thoroughly remove boron impurity obstinate in ultra-pure water, overcome an industry difficult problem, is the milestone of ultra-pure water development.
Detailed description of the invention
Below preferred embodiment of the present invention is described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention is made to more explicit defining.
The embodiment of the present invention comprises:
Embodiment 1
Without a preparation method for boron ultra-pure water, concrete preparation process is as follows:
(1) hollow fiber filter that the running water after impurity is removed in three grades of pretreatment is less than to 0.01 micron with the pressure of 3~10MPa by ultrafiltration micropore, the harmful substances such as bacterium in filtering water, iron rust, colloid, retain original trace element and mineral matter in water;
(2) running water after ultrafiltration is introduced to reverse osmosis unit, except anhydrating, middle most of soluble salt is divided, microorganism and whole colloids;
(3) running water of reverse-osmosis treated is introduced in EDI device, removed the salinity in running water with electrophoresis, and thoroughly remove the bacterium in water body;
(4) by the UV UV-irradiation that is 185nm with wavelength through EDI device electrophoresis running water after treatment, thereby be carbon dioxide and water by the organic substance decomposing in running water;
(5) remove the boron element in UV biodegradation running water after treatment, mainly comprise that two steps are except boron technique, the first step is that polyhydric alcohol complex counter-infiltration is except boron, concrete grammar is: in running water, add watery hydrochloric acid, regulating its pH value is 3~6.5, then in every liter of running water, add the polyalcohol of 1~10ppm (to comprise D-glucitol, sweet mellow wine, at least one in D-Fructose and xylitol), after stirring, boric acid in polyalcohol and running water forms macromolecular complex compound, and then this running water that contains macromolecular complex thing is introduced to reverse osmosis unit with certain pressure, remove macromolecular complex thing, thereby realize the object of removing boron element, the clearance of the method boric acid is 80%,
Second step is that two-stage effects of boron resin is except boron, concrete grammar is: the running water after polyhydric alcohol complex counter-infiltration removes boron is introduced to one-level effects of boron resin, for gallic acid grafting highly acid anion exchange resin, constant temperature stirs 20~60min, make resin fully adsorb the boric acid in running water, realize the object except boron to water body from the beginning, the one-level effects of boron resin after absorption is resolved simultaneously, this process can be removed more than 95% boron element in running water; Then adding diluted sodium hydroxide solution to regulate the pH value of running water is 8.5~9.5, introduce again secondary effects of boron resin, be 2,3-dihydroxy-6-sodium sulfonate grafting strong-base anion-exchange resin or polyhydroxy amines styrene resin resinoid, constant temperature stirs 20~60min, makes resin fully adsorb the boric acid in water body from the beginning, realizes water body from the beginning except the object of boron, secondary effects of boron resin after absorption is resolved, this process can be removed boron elements whole in running water simultaneously;
(6) running water except after boron is introduced to EC150UP polishing resin, i.e. the special mixture iron exchange resin of ultra-pure water, running water is carried out to last comprehensive precision processing, ensures the water quality of ultra-pure water, obtains without boron ultra-high purity water.
The ultra-pure water that said method obtains, its boron content is less than 100PPT, and other constituent contents all can reach PPT level, are a kind of ultra-pure waters of excellent combination property, are the desirable water sources of preparing the ultrapure chemical material of semicon industry.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. without a preparation method for boron ultra-pure water, it is characterized in that, running water is passed through successively to ultrafiltration, counter-infiltration, EDI device, UV biodegradation, removes boron technique and polishing resin treatment, obtain described without boron ultra-pure water; Wherein, the described boron technique of removing comprises that polyhydric alcohol complex counter-infiltration removes boron and two-stage effects of boron resin removes boron.
2. the preparation method without boron ultra-pure water according to claim 1, it is characterized in that, the method that described polyhydric alcohol complex counter-infiltration removes boron is: running water is after UV biodegradation is processed, regulate its pH value to acid, then add wherein a certain amount of polyalcohol, after stirring, remove boron through reverse osmosis membrane filtration.
3. the preparation method without boron ultra-pure water according to claim 2, is characterized in that, described pH value is 3~6.5; The addition of described polyalcohol is 1~10ppm/L water.
4. the preparation method without boron ultra-pure water according to claim 3, is characterized in that, described polyalcohol is at least one in D-glucitol, sweet mellow wine, D-Fructose and xylitol.
5. the preparation method without boron ultra-pure water according to claim 1, it is characterized in that, described two-stage effects of boron resin boron removal method is: remove boron by introducing one-level effects of boron resin through polyhydric alcohol complex counter-infiltration except the running water after boron, then the pH value that regulates running water is 8.5~9.5, then introduces secondary effects of boron resin except boron.
6. the preparation method without boron ultra-pure water according to claim 5, is characterized in that, described one-level effects of boron resin is gallic acid grafting highly acid anion exchange resin; Described secondary effects of boron resin is 2,3-dihydroxy-6-sodium sulfonate grafting strong-base anion-exchange resin or polyhydroxy amines styrene resin resinoid.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106629975A (en) * | 2016-12-27 | 2017-05-10 | 南京慧城水处理设备有限公司 | Method used for removing trace boron in desalination seawater with boron selective chelating resin |
CN111039381A (en) * | 2018-10-15 | 2020-04-21 | 中国科学院过程工程研究所 | Method for improving quality of reverse osmosis seawater desalination produced water |
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Cited By (2)
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CN111039381A (en) * | 2018-10-15 | 2020-04-21 | 中国科学院过程工程研究所 | Method for improving quality of reverse osmosis seawater desalination produced water |
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