CN115286155B - Boron removal treatment method for spring water - Google Patents
Boron removal treatment method for spring water Download PDFInfo
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- CN115286155B CN115286155B CN202210935054.1A CN202210935054A CN115286155B CN 115286155 B CN115286155 B CN 115286155B CN 202210935054 A CN202210935054 A CN 202210935054A CN 115286155 B CN115286155 B CN 115286155B
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- water
- boron removal
- boron
- spring water
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 218
- 229910001868 water Inorganic materials 0.000 title claims abstract description 208
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 196
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 194
- 238000000034 method Methods 0.000 title claims abstract description 59
- 229920000742 Cotton Polymers 0.000 claims abstract description 104
- 229920002678 cellulose Polymers 0.000 claims abstract description 91
- 239000001913 cellulose Substances 0.000 claims abstract description 91
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000002253 acid Substances 0.000 claims abstract description 27
- FXSGDOZPBLGOIN-UHFFFAOYSA-N trihydroxy(methoxy)silane Chemical compound CO[Si](O)(O)O FXSGDOZPBLGOIN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000008569 process Effects 0.000 claims abstract description 23
- 238000001179 sorption measurement Methods 0.000 claims abstract description 18
- 230000008929 regeneration Effects 0.000 claims description 66
- 238000011069 regeneration method Methods 0.000 claims description 66
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 25
- 239000003513 alkali Substances 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 22
- XYRAEZLPSATLHH-UHFFFAOYSA-N trisodium methoxy(trioxido)silane Chemical compound [Na+].[Na+].[Na+].CO[Si]([O-])([O-])[O-] XYRAEZLPSATLHH-UHFFFAOYSA-N 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
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- 238000011049 filling Methods 0.000 claims description 7
- 238000005517 mercerization Methods 0.000 claims description 7
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical group CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 6
- 239000011707 mineral Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 230000001954 sterilising effect Effects 0.000 claims description 5
- 239000006004 Quartz sand Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000003475 lamination Methods 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- KEQFTVQCIQJIQW-UHFFFAOYSA-N N-Phenyl-2-naphthylamine Chemical compound C=1C=C2C=CC=CC2=CC=1NC1=CC=CC=C1 KEQFTVQCIQJIQW-UHFFFAOYSA-N 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 230000001172 regenerating effect Effects 0.000 claims description 2
- 238000009999 singeing Methods 0.000 claims description 2
- 230000004580 weight loss Effects 0.000 claims description 2
- 239000002250 absorbent Substances 0.000 claims 1
- 230000002745 absorbent Effects 0.000 claims 1
- 239000003463 adsorbent Substances 0.000 claims 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 abstract description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract description 10
- 239000004327 boric acid Substances 0.000 abstract description 10
- 239000002366 mineral element Substances 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 42
- -1 amino acid sodium salt Chemical class 0.000 description 31
- 229920003023 plastic Polymers 0.000 description 29
- 239000004033 plastic Substances 0.000 description 29
- 230000000694 effects Effects 0.000 description 26
- 239000004698 Polyethylene Substances 0.000 description 23
- 229920000573 polyethylene Polymers 0.000 description 23
- 239000007864 aqueous solution Substances 0.000 description 22
- 239000011347 resin Substances 0.000 description 16
- 229920005989 resin Polymers 0.000 description 16
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- 239000012535 impurity Substances 0.000 description 12
- 230000035622 drinking Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 229910052744 lithium Inorganic materials 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 229910052712 strontium Inorganic materials 0.000 description 10
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 10
- 229910003849 O-Si Inorganic materials 0.000 description 9
- 229910003872 O—Si Inorganic materials 0.000 description 9
- 239000006228 supernatant Substances 0.000 description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- 239000011575 calcium Substances 0.000 description 8
- 229910052791 calcium Inorganic materials 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 8
- 229910052749 magnesium Inorganic materials 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 235000020682 bottled natural mineral water Nutrition 0.000 description 5
- 235000020188 drinking water Nutrition 0.000 description 5
- 239000003651 drinking water Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 235000010755 mineral Nutrition 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- LDDMACCNBZAMSG-BDVNFPICSA-N (2r,3r,4s,5r)-3,4,5,6-tetrahydroxy-2-(methylamino)hexanal Chemical compound CN[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO LDDMACCNBZAMSG-BDVNFPICSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000010502 deborylation reaction Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000001502 supplementing effect Effects 0.000 description 3
- 239000002352 surface water Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 2
- MBBZMMPHUWSWHV-BDVNFPICSA-N N-methylglucamine Chemical compound CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO MBBZMMPHUWSWHV-BDVNFPICSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- 241001122767 Theaceae Species 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
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- 238000001125 extrusion Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- ZJBHFQKJEBGFNL-UHFFFAOYSA-N methylsilanetriol Chemical compound C[Si](O)(O)O ZJBHFQKJEBGFNL-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- LCLHHZYHLXDRQG-ZNKJPWOQSA-N pectic acid Chemical class O[C@@H]1[C@@H](O)[C@@H](O)O[C@H](C(O)=O)[C@@H]1OC1[C@H](O)[C@@H](O)[C@@H](OC2[C@@H]([C@@H](O)[C@@H](O)[C@H](O2)C(O)=O)O)[C@@H](C(O)=O)O1 LCLHHZYHLXDRQG-ZNKJPWOQSA-N 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
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- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000009287 sand filtration Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 230000009967 tasteless effect Effects 0.000 description 2
- 235000013616 tea Nutrition 0.000 description 2
- 230000002110 toxicologic effect Effects 0.000 description 2
- 231100000027 toxicology Toxicity 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 125000003535 D-glucopyranosyl group Chemical group [H]OC([H])([H])[C@@]1([H])OC([H])(*)[C@]([H])(O[H])[C@@]([H])(O[H])[C@]1([H])O[H] 0.000 description 1
- 206010020112 Hirsutism Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229920002230 Pectic acid Polymers 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- AEMOLEFTQBMNLQ-BKBMJHBISA-N alpha-D-galacturonic acid Chemical compound O[C@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-BKBMJHBISA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
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- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- 239000000194 fatty acid Substances 0.000 description 1
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- 150000004665 fatty acids Chemical class 0.000 description 1
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- 159000000000 sodium salts Chemical class 0.000 description 1
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/444—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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/108—Boron compounds
Abstract
The invention provides a boron removal treatment method of mountain spring water, which takes a cotton cellulose coil modified by methyl silicic acid as a boron removal adsorption material, and a polyhydroxy unit in a long chain of the cotton cellulose modified by methyl silicic acid and B (OH) 4 ‑ Form moderate combination of intensity, absorb boric acid or borate in the water, have higher selectivity and capacity of boron removal, and can be regenerated by hot water of 90-100 ℃ or normal temperature dilute acid with the concentration of 0.2-0.3 mol/L; the borate content in the spring water is directly treated from 0.5-2.0mg/L to 0.2-0.3mg/L, 0.3-0.4mg/L or 0.4-0.5mg/L according to B, the content of other mineral elements and COD are basically unchanged, and the taste of the obtained spring water is not different from that before treatment; the whole investment and the operation cost of the boron removal process are low, and the method has a certain application prospect.
Description
Technical Field
The invention belongs to the technical field of drinking water purification treatment, and particularly relates to a boron removal treatment method for spring water.
Background
Bottled or barreled spring water is important food, tea and drinking water for residents in cities and towns in China at present, and has certain acceptable taste and water quality; the product quality has no national standard, but has a plurality of local standards and enterprise standards.
The main sources of the spring water include surface water such as spring, well, stream, lake and the like with better water quality in mountainous areas and hills, and also high-quality underground mineral water which can not reach or can not stably reach the GB8537 drinking natural mineral water (the latest standard is GB 8537-2018). Some mineral water meeting the quality requirement of GB8537 is operated as mountain spring water. The processing procedures before bottling or barreling of the spring water generally comprise source water sedimentation, quartz sand filtration, activated carbon filtration, photoelectric or ozone disinfection and sterilization, microfiltration or ultrafiltration and the like.
GB8537 water source for drinking natural mineral water, which is naturally gushed from underground depths or collected by drilling, contains a certain amount of minerals, trace elements or other components, is not polluted in a certain area and takes preventive measures to avoid polluted water; under normal conditions, dynamic indexes such as chemical components, flow, water temperature and the like are relatively stable in a natural period fluctuation range and meet the specified requirements; is mainly characterized in that one or more of the boundary indexes of lithium, strontium, zinc, metasilicic acid, selenium, free carbon dioxide, soluble total solid and the like meet the specified requirements. GB8537 has high index requirement for drinking natural mineral water, and water sources and products meeting the standard are rare, so the product price is high, and the yield and the consumption are far lower than those of mountain spring water.
In the source water of spring water, the content of borate is greatly different under the influence of various factors, and is difficult to control and less concerned in the water treatment process; for example, surface water of mountainous areas and hills or shallow groundwater which is a main source of spring water, the water quality condition of the surface water is influenced by rain, snow, precipitation, surface soil planting, vegetation and the like, and the content of borate often has obvious seasonal fluctuation; the borate content of underground mine water also varies with formation conditions. The average value of the total boron content of the soil in China is 64mg/kg.
GB8537-2018 drinks natural mineral water, and the content limit of the toxicological index borate in terms of B is 5mg/L. The natural mineral water has the advantages of supplementing trace mineral elements such as lithium, strontium, zinc, metasilicic acid, selenium and the like required by human bodies, so the process of changing the content of mineral elements except iron and manganese is generally not included in the treatment before bottling or barreling.
In GB5749-2022 and GB5749-2006 sanitary standards for drinking water, the limit values of the content of boron in a toxicological index are 1.0mg/L and 0.5mg/L respectively, and the boron content is controlled when necessary as an expansion index or an unconventional index. The supply of the water, namely tap water is large, the treatment process usually comprises a flocculation impurity removal process of adding water purifying agents such as polymeric ferric aluminum sulfate and the like, the flocculation impurity removal process has certain boron removal capacity, and the boron removal effect is obvious when the content of boron in source water is high; however, the treatment of spring water does not include such flocculation impurity removal process, so as to avoid the complication of the process and the reduction of the water quality.
In many local standards or enterprise standards of bottled (barreled) drinking spring water, the same 5mg/L boron content limit value as GB8537 mineral water is adopted, so most enterprises do not specifically control the boron content of the drinking spring water products, namely, the problem that the boron intake is too large when the boron content is too high as barreled spring water serving as main food, tea and drinking water is actually ignored. In the process of establishing local standards or enterprise standards of the mountain spring water for drinking in the bottle (bucket), the suggested values of WHO are possibly referred to: the daily requirement of the basic boron for adults is about 0.375mg, and the average daily intake safety range of acceptable crowds is 1-13mg; however, it is also statistically believed that daily boron intake of more than 5mg will affect the health of many people, and that food itself will also bring in a certain amount of boron. The applicant carries out statistics on the source water and product detection data of mountain spring water of a typical monthly-measure subsidiary company in the last fifteen years, and finds that the boron content in a rich water period is 0.2-0.3mg/L mostly, and the boron content in a dry water period is 0.4-0.6mg/L and is 1.2mg/L at most; in the public detection report of barreled products of different years and months in a certain well-known spring water enterprise, the boron content of some batches is 0.2-0.3mg/L, and the boron content of other batches is 0.4-0.6mg/L.
Therefore, in the treatment process of some drinking spring water, proper boron removal is needed, and the boron content of the drinking spring water product in a bottle (barrel) is specifically controlled by combining the source water condition and the consumption habit, so that the problem of overlarge boron intake of consumers is avoided.
In the treatment of drinking spring water, optional boron removal method includes boron selective resin adsorption method, wherein the inner pore surface of boron selective resin such as D403 and D564 is grafted with a large amount of N-methyl glucosamine to form tertiary amine polyol functional group capable of selectively adsorbing and chelating boron, and boric acid or borate in water is B (OH) 4 - The form and the functional group form high-strength complexation, the boron content in water can be processed to be below 0.2mg/L or even below 0.1mg/L, and a mountain spring water product with the required boron content can be produced by mixing low-boron water and high-boron water when necessary. However, the boron selective resin adsorption method has the disadvantages that the resin is very expensive, the boron removal regeneration by acid with the concentration of more than 0.5mol/L and the alkali washing regeneration with the concentration of more than 0.3mol/L are needed, the whole cost is high, other materials grafted with N-methyl glucosamine, such as cellulose grafted with N-methyl glucosamine, have similar problems, and the industry of drinking mountain spring water is difficult to accept. The methods of electrodialysis, reverse osmosis and the like also have certain boron removal effect, but generally, the method is inconvenient to apply because the content of other mineral elements is obviously changed at the same time.
In the development of seawater desalination for producing drinking water, research on boron removal is also conducted using cellulosic materials such as absorbent cotton. The cellulose material has the advantages that the price is far lower than that of boron selective resin, the boron selective resin has certain boron removal capacity and precision, but the cellulose material needs to be regenerated by acid washing with the concentration of more than 0.3mol/L, and absorbent cotton is loose and is not convenient to be applied in continuous water flow treatment; many enterprises drinking spring water are lack of acid procedures and facility conditions.
Disclosure of Invention
In order to solve the problems, the invention provides a boron removal treatment method of mountain spring water by using a cotton cellulose coil modified by methyl silicic acid as a boron removal adsorption material.
The invention provides a boron removal treatment method of mountain spring water, which takes a cotton cellulose coil modified by methyl silicic acid as a boron removal adsorption material, and a polyhydroxy unit in a long chain of the cotton cellulose modified by methyl silicic acid and B (OH) 4 - The combination with moderate strength is formed, the boric acid or borate in the water is adsorbed, the high boron removal selectivity and capacity are realized, and the regeneration can be realized by using hot water with the temperature of 90-100 ℃ or normal-temperature dilute acid with the concentration of 0.2-0.3 mol/L; the content of borate in the spring water calculated by B is directly processed to a specific range of 0.2-0.5mg/L from 0.5-2.0mg/L, such as 0.2-0.3mg/L, 0.3-0.4mg/L or 0.4-0.5mg/L, the content of other mineral elements and COD are basically unchanged, and the taste of the obtained spring water is not different from that before processing; the whole investment and the operation cost of the boron removal process are low, and the method has a certain application prospect.
The boron removal treatment method of mountain spring water comprises the following steps: settling source water, filtering with quartz sand and active carbon, controlling temperature at 15-25 deg.C for removing boron, sterilizing with ultraviolet ray or ozone, micro-filtering or ultrafiltering, and bottling or barreling to obtain mountain spring aquatic product;
the method comprises the following steps of (1) carrying out boron removal treatment in a boron removal tank filled with a cotton cellulose boron removal adsorption material modified by methyl silicic acid; the methyl silicic acid modified cotton cellulose boron removal adsorbing material is prepared by the following steps: (a) Carrying out mercerization modification and drying on cotton yarns with the outer diameter of 0.3-1.0mm by a liquid-reducing method to obtain a methyl silicic acid modified cotton cellulose wire; (b) Methyl silicic acid modified cotton fiberThe cellulose wire is wound into a spherical, ellipsoidal or columnar coil with the external dimension of 30-50mm to obtain the cotton cellulose boron removal adsorbing material modified by the methyl silicic acid; the mercerizing modification conditions in the step (a) are as follows: firstly, the temperature is 20-30 ℃, the solution contains 200-220g/L of NaOH, 30-50g/L of sodium methylsilicate and H 2 O 2 2-3g/L of stabilizer AR 702-20 g/L and 0.5-1.0g/L of penetrant GFC, soaking in alkali liquor for 120-240s, stretching for 3-4 times in the alkali soaking process, soaking in acid liquor containing 10-30g/L of HCl at 20-40 ℃ for 20-60min, squeezing to remove the solution, and washing with water to pH6-8.
In the preparation process of the methyl silicic acid modified cotton cellulose boron removal adsorbing material, coarse cotton yarns with the outer diameter of 0.3-1.0mm are adopted in the step (a), and the methyl silicic acid modified cotton cellulose boron removal adsorbing material has the advantages that more pore passages with the diameter of more than 50 micrometers are formed in the step (b), so that mass transfer in a coil is facilitated, and the cotton cellulose boron removal adsorbing material with the outer diameter of 30-50mm can be adopted; the specification of the cotton yarn can be 6S/4, 6S/6, 12S/4 and 12S/6, the outer diameter of the cotton yarn is about 0.6mm, 0.8mm, 0.3mm and 0.5mm in sequence, and the price is low.
Before the mercerization modification in the step (a), singeing treatment can be carried out on the cotton yarn under the treatment conditions that the flame temperature is 900-1000 ℃, the weight reduction of the cotton yarn is controlled to be less than or equal to 2wt%, most of exposed cotton fibers, namely hairiness, on the surface of the cotton yarn can be burnt, the internal mass transfer effect of the lumpy cotton cellulose boron removal adsorbing material can be finally improved, and the boron removal capacity and the regeneration rate are improved.
The cotton cellulose boron removal adsorbing material modified by the methyl silicic acid in the step (b) adopts a winding mode of oblique lamination, the included angle between adjacent line layers along the central axis of the yarn is 20-30 degrees, the distance between yarns in the layers is less than or equal to 0.1mm, and the stacking density in a boron removal tank is 400-550kg/m 3 The high boron removal capacity and the low bed water flow pressure drop can be obtained, and the coil structure is stable and is not easy to loosen in the processes of storage, transportation and filling; the bulk density and strength can be adjusted by the tension and the wire spacing in the coiling and agglomerating process.
In the boron removal treatment method of the spring water, the treatment flow of the water in the boron removal tank can be 0.4-5BV/h, preferably 1-2BV/h, particularly according to the treatment flow of the water in the spring waterThe concentration of boron and the concentration of mineral elements; the borate content in mountain spring water can be directly treated from 0.5-2.0mg/L to a more narrow specific range of 0.2-0.5mg/L, such as 0.2-0.3mg/L, 0.3-0.4mg/L or 0.4-0.5mg/L, and the content of other mineral elements is basically unchanged and has less influence on the boron removal effect. BV means bed volume of the silicon acid modified cotton cellulose boron removal adsorption material. The boron removal capacity of the methyl silicic acid modified cotton cellulose boron removal adsorption material in the boron removal treatment of spring water is more than 6g/kg, and the boron removal capacity of a boron removal bed layer is 3kg/m 3 The water treatment amount in a single period can reach 3000-5000/m 3 Or higher. The service life should be above 3 years, inferred from the tests or applications in the examples.
In the boron removal treatment method of the mountain spring water, the boron content of the outlet water of the cotton cellulose boron removal adsorption material modified by the methyl silicic acid in a boron removal tank approaches or reaches the upper limit of a control standard or is subjected to boron removal saturation, and then the in-tank in-situ regeneration can be carried out by using hot water at the temperature of 90-100 ℃ or normal-temperature dilute acid with the concentration of 0.2-0.3 mol/L; the spring water with B content lower than 1.0mg/L can be used in regeneration, including boron-removed spring water with B content of 0.2-0.3mg/L, the hot water obtained by heating or prepared dilute acid can be used as regeneration liquid, the flow direction of the regeneration liquid is identical to that of spring water in boron removal treatment, the flow rate is 0.5-3BV/h, the liquid consumption is 2-8BV, then the spring water with B content lower than 1.0mg/L and 1-10BV/h including boron-removed spring water is used to flush to below 35 deg.C or above pH6, in which the spring water without boron removal can be directly used for regeneration and cooling, and the regeneration and cooling effects when boron-removed spring water is used are slightly good. The boron removal capacity of the methyl silicic acid modified cotton cellulose boron removal adsorption material can be restored to be more than 90% of the original value after the primary hot water regeneration at 90-100 ℃, and the regeneration efficiency can be basically maintained during the secondary and subsequent hot water regeneration at 90-100 ℃; the boron removal capacity can be recovered to be more than 98 percent of the original value after the primary diluted acid regeneration, and the regeneration efficiency can be basically maintained by the secondary and subsequent acid washing regeneration; after long-term use and multiple regeneration, the boron removal capacity is reduced little, and the boron removal precision is basically unchanged. The pH value of the spring water is generally 6-8.
The principle of the boron removing treatment method of mountain spring water according to the practical experience of the inventor and the effect of the embodiment and the comparative example is explained as follows:
1. the cotton fiber is a relatively pure cellulose material, the cellulose content is as high as 95-97%, the crystallinity is higher than 70%, impurities mainly comprise pectic substances, nitrogen-containing substances, waxy substances and inorganic salt, and a small amount of cotton seed hull scraps are also mixed in the cotton yarn; cotton cellulose has a long chain structure, and the basic unit is D-glucopyranosyl having three hydroxyl groups including two secondary hydroxyl groups and one primary hydroxyl group, linked by glycosidic bonds, with a degree of polymerization of about 15000, which enables cellulose to bind boric acid or B (OH) 4 - The boron is removed, and primary carbon hydroxyl in the boron has high activity.
2. The mercerizing modification process of cotton yarn by a liquid-reducing method in the step (a) is mainly characterized in that the reaction and modification of cellulose and the removal of impurities occur under the condition of alkali liquor. Wherein the main reactions of the cellulose comprise: the method comprises the following steps of (1) damaging partial hydrogen bond connection among long chains through the action of primary carbon hydroxyl with higher activity and NaOH with higher concentration, and generating dislocation and local loosening among the long chains under the tension stretching action to reduce the crystallinity of cellulose to about 50%; simultaneously, partial primary hydroxyl reacts with sodium methylsilicate to generate a certain amount of-CH 2 -O-Si(CH 3 )(ONa) 2 and/or-CH 2 -O-Si(CH 3 ) (OH) (ONa), which have some swelling effect, may further reduce the crystallinity of cellulose. The reaction of the impurities comprises: pectic substance with pectic acid derivative as main component is hydrolyzed to generate pectic acid and further converted into sodium salt for dissolving out, and molecular chain breakage is also generated to improve the solubility of pectin in alkali liquor; the amido bonds in the protein molecules in the nitrogen-containing substance are hydrolyzed and broken to generate amino acid sodium salt which is dissolved out; dissolving out higher fatty alcohol, fatty acid, alcohol ester and hydrocarbon in the waxy substance under the emulsification, saponification and dispersion effects of NaOH and penetrating agent; the main components of the cotton seed hull scraps are cellulose and a small part of lignin, and the rest of tannin, polysaccharide substances and a small amount of protein and grease are dissolved and oxidized in alkali liquor, so that the cotton seed hull scraps are swelled, fluffed,Is easy to fall off. Most of the alkali liquor is extruded and recycled when the last tension stretching is carried out before the acid liquor impregnation; in the acid liquor dipping and water washing processes, the-CH 2 -O-Si(CH 3 )(ONa) 2 、-CH 2 -O-Si(CH 3 ) (OH) (ONa) group to-CH 2 -O-Si(CH 3 )(OH) 2 The impurity product is further dissolved out. The mercerized and modified cotton yarn has obvious swelling and good hydrophilicity, the orientation degree of fibers is obviously improved, the fibers have the same luster as silk, but the flexibility is not obvious different from that of the mercerized and modified cotton yarn.
3. In the methyl silicic acid modified cotton cellulose wire rod obtained in the step (a), the-CH generated by primary carbon hydroxyl and sodium methyl silicate 2 -O-Si(CH 3 )(OH) 2 Not only is a part of hydroxyl added to the cellulose, but also the capacity of the cellulose combined with boric acid is slightly improved, and the regeneration difficulty of the borosilicate-removed cotton cellulose adsorbing material modified by the methyl silicate in the step (b) after boron removal is reduced, so that the satisfactory regeneration effect can be achieved after the borosilicate-removed cotton cellulose adsorbing material is regenerated by hot water at 90-100 ℃ or normal-temperature dilute acid with the concentration of 0.2-0.3mol/L, and the reason is that: albeit the generated-CH 2 -O-Si(CH 3 )(OH) 2 The quantity is not much, the proportion of one glucose group unit to one glucose group unit is not reached, the distribution is more uniform, and the most of the glucose group units with boron removal capability in the long chain of the cellulose and boric acid or B (OH) are properly reduced 4 - The boron removal precision can also meet the requirement of mountain spring water treatment.
4. The methylsilicic acid modified cotton cellulose wire obtained in step (a) is white, tasteless, good in flexibility, and its granular impurity can not be seen under the optical microscope, and when it is repeatedly prepared, the silicon content difference is small, so that it can indicate reaction condition of methylsilicate and-CH 2 -O-Si(CH 3 )(OH) 2 The generation condition of the device is stable and reliable.
5. The methyl silicate modified cotton cellulose wire obtained in the step (a) is smooth in wire running in the process of winding the coil in the step (b), the prepared methyl silicate modified cotton cellulose boron removal adsorption material is good in strength and toughness, and can be regenerated by hot water at 90-100 ℃ after boron removal, and the two aspects are difficult to achieve after cotton yarn is subjected to mercerization by using aqueous glass alkali liquor.
The sodium methylsilicate contained in the alkali liquor is replaced by the sodium silicate with the same or smaller silicon content, the flexibility of the wire rod is obviously reduced, some granular impurities can be seen under an optical microscope, the wire coil wound in the step (b) is obviously hardened, the boron removal capacity is low, and the regeneration effect of the wire rod by using hot water with the temperature of 90-100 ℃ or normal-temperature dilute acid with the concentration of 0.2-0.3mol/L is poor.
6. The conventional application of sodium methyl silicate is the hydrophobic modification of inorganic materials, especially silicate-containing materials such as cement and concrete, and the function principle is to absorb carbon dioxide in air or added acid components to react to generate methyl silanetriol which then undergoes dehydration reaction with exposed silicon hydroxyl of silicate, aluminum silicate and aluminosilicate on the surface of the silicate-containing inorganic materials to form firm Si-O-Si (CH) 3 )(OH) 2 The chemical bonding of (2) is combined on the inner hole and the surface of the silicate-containing inorganic material in a large quantity, the methyl ends are exposed, the exposed methyl ends are densely distributed and are very stable at the temperature of below 250 ℃, and therefore, the long-acting and stable hydrophobic and hydrophobic effects are achieved. The molecular structure of the sodium methyl silicate is that hydrogen of one hydroxyl in methyl silanetriol is replaced by sodium.
However, the cotton cellulose wire modified by methyl silicic acid in the invention has good hydrophilic performance, and the modification of methyl silicic acid does not play a hydrophobic role, and the reasons include 2 and 3.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto.
Example 1
A cotton yarn (type 6S/4, outer diameter about 0.5 mm) is modified in an alkali liquor method yarn mercerizing tester by about 0.1kg in a roll, and the basic process is to perform alkali immersion, acid cleaning, water washing and drying under the conditions of continuous single-line running and continuous tension. The specific operating conditions are as follows: tension 65MPa (single yarn tension estimated and controlled based on the cross-sectional area of the wet yarn measured at the time of washing with water); alkali liquor (10L) of an alkali leaching tank contains 210g/L of NaOH, 40g/L of sodium methyl silicate, 22.5g/L of H2O, 702 g/L of a stabilizing agent AR, 0.8g/L of a penetrant GFC, the temperature is 25 ℃, nitrogen is used for protection, the alkali leaching time is 180s, then the alkali liquor is removed through an extrusion roller, and then acid pickling is carried out; pickling bath acid solution (40L) containing HCl 20-22g/L at 30 deg.C for 30min, removing acid solution by squeezing roller, and washing with water; the yarn in the washing tank is in countercurrent contact with deionized water, the water temperature is 30 ℃, the washing time is 20min to pH6.0-6.5, then the yarn is dewatered by an extrusion roller, and then the yarn is wound on a bobbin for drying; the drying temperature is 80 ℃, and the cotton cellulose wire modified by the methyl silicic acid is obtained after 3 hours. The triple squeeze rolls can control the wet yarn content to less than 40wt% on a dry yarn basis.
Example 2
The methylsilicic acid-modified cotton cellulose yarn of this example was prepared essentially as in example 1, with the difference that before the mercerization modification, the cotton yarn was also singed at a flame temperature of 900-1000 ℃ and a weight loss of 1.3wt%.
3 parts of the methylsilicic acid-modified cotton cellulose strand of example 2, each of about 0.1kg, were repeatedly prepared.
Example 3
A methylsilicic acid-modified cotton cellulose strand according to this example was prepared essentially as in example 1, with the difference that the sodium methylsilicate content in the lye of the lye tank was 50g/L.
Example 4
A methylsilicic acid-modified cotton cellulose strand of the present example was prepared substantially as in example 1, except that the mercerization time was controlled to 240 seconds.
The methylsilicic acid-modified cotton cellulose strands obtained in examples 1 to 4 were all white, odorless, and very flexible, and no granular foreign matter was observed under an optical microscope.
Comparative example 1
The cotton cellulose thread of this comparative example was prepared essentially as in example 1, except that the alkali solution did not contain sodium methyl silicate.
Comparative example 2
The cotton cellulose strand of this comparative example was prepared essentially as in example 1, except that the sodium methylsilicate content in the lye was 60g/L.
Comparative example 3
The cotton cellulose strand of this comparative example was prepared essentially as in example 1, except that the water washing was carried out directly after the alkali immersion without acid washing for 60min.
Comparative example 4
The cotton cellulose strand of this comparative example was prepared essentially as in example 1, except that the water washing was carried out directly after the alkali immersion without acid washing for 300min.
Comparative example 5
The cotton cellulose strand of this comparative example was prepared substantially as in example 1, except that the tension was controlled to 30MPa.
Comparative example 6
A cotton cellulose strand of this comparative example was prepared essentially as in example 1, except that sodium methylsilicate in the lye was replaced with 25.7g/L of water glass having a modulus of 3.0 on a solids basis (corresponding to a silicon content of 40g/L of sodium methylsilicate).
Comparative example 7
A cotton cellulose yarn of this comparative example was prepared essentially as in example 1, except that sodium methyl silicate in the alkali solution was replaced with a 3.0 modulus water glass at 12.8g/L on a solids basis (50% of the silicon content of 40g/L of sodium methyl silicate).
Comparative example 8
A cotton cellulose strand of this comparative example was prepared essentially as in example 1, except that sodium methyl silicate in the lye was replaced with a water glass having a modulus of 3.0, 6.4g/L on a solids basis (25% of the silicon content of 40g/L of sodium methyl silicate).
Comparative example 9
A boron selective resin commercial D403 (outer diameter 0.8 to 0.9 mm) having a large amount of N-methylglucamine grafted on the surface of the inner pores was used as the deboronated material of this comparative example.
Comparative example 10
A boron selective resin commercial D564 (outer diameter 0.7 to 0.9 mm) in which a large amount of N-methylglucamine was grafted on the surface of the inner pores was used as the deboronated material of this comparative example.
Example 5
(5-1) the methylsilicic acid-modified cotton cellulose threads obtained in examples 1 to 4 (in which 4 parts of the methylsilicic acid-modified cotton cellulose threads prepared in example 2), the cotton cellulose threads obtained in comparative examples 1 to 8, and the boron-selective resins obtained in comparative examples 9 to 10 were subjected to a deboning test, respectively, as follows: adding boric acid into deionized water to obtain 25 deg.C water solution containing B10mg/L (measured pH 6.7), loading 500ml into 17 1000ml polyethylene plastic beakers, respectively adding 1.0g of cotton cellulose wires cut into 4-5mm length, stirring once every 3min, processing for 60min, collecting supernatant, filtering, and measuring B content. As a result, the methylsilicic acid-modified cotton cellulose threads of examples 1 to 4 were able to treat the B content of the aqueous solution to 0.3mg/L or less; the cotton cellulose wires of comparative examples 1 to 8, all of which were able to treat the B content of the aqueous solution to less than 0.4 mg/L; the boron-selective resins of comparative examples 9 to 10 were all able to handle the B content of the aqueous solution to less than 0.2 mg/L.
(5-2) fishing out the wires and the resin after boron removal in the step (5-1), extruding to remove liquid, putting the wires and the resin into a group of 100ml polyethylene plastic bottles with capacity scales, respectively adding 100ml boiling water (deionized water, 100 ℃), putting the bottles into a 90 ℃ oven for regeneration, uniformly stirring once every 3min, respectively adding deionized water to 100ml after treating for 60min, sealing and cooling to room temperature, respectively taking supernatant, and filtering to measure the content of B. As a result, the B content of the aqueous solution in the cotton cellulose wire beakers of examples 1 to 4 and comparative example 5 was 45.0mg/L or more, which indicates that the hot water regeneration effect was good; the aqueous solutions in the cotton cellulose wire beakers of comparative examples 1, 6 and 8 contained 20.3 to 20.6mg/L of B, the aqueous solution in the cotton cellulose wire beaker of comparative example 2 contained 35.1mg/L of B, the aqueous solution in the cotton cellulose wire beaker of comparative example 3 contained 40.0mg/L of B, the aqueous solution in the cotton cellulose wire beaker of comparative example 4 contained 40.2mg/L of B, and the aqueous solution in the boron selective resin beakers of comparative examples 9 and 10 contained less than 5.0mg/L of B, and the hot water regeneration effect was not good.
(5-3) fishing out the regenerated wires of (5-2) examples 1-4 respectively, extruding to remove liquid, putting the wires back to 1000ml of polyethylene plastic beakers, adding deionized water and boric acid to prepare 500ml of 25 ℃ aqueous solution (pH 6.7) containing 10mg/L of B, carrying out secondary boron removal, uniformly stirring once every 3min, filtering supernatant after 60min treatment, and measuring the content of B, wherein the content of B in the aqueous solution can be treated to be below 0.3 mg/L. The hot water regeneration at 90-100 ℃ was continued by the method (5-2), and as a result, the amount of B in the aqueous solution in each beaker was 45.0mg/L or more, indicating that the hot water regeneration effect was good.
(5-4) according to the method (5-3), each wire rod of the example 1-4 is continuously subjected to the boron removal of the aqueous solution at 25 ℃ containing 10mg/L of B and the hot water regeneration at 90-100 ℃ for the tenth time, and the effect of (5-3) can be basically repeated.
Example 6
(6-1) the cotton cellulose threads of each of examples 1 to 4 (4 parts of the methylsilicic acid-modified cotton cellulose thread prepared in example 2) of example 5 (5-4) after hot water regeneration and the cotton cellulose threads of comparative example 5 (1.0 g each) of 5-2) after hot water regeneration were subjected to the deboration test in the following manner: deionized water and boric acid are added to prepare 25 ℃ water solution (measured pH 6.5) containing 20mg/L of B, 500ml of the water solution is respectively filled in 1000ml of polyethylene plastic beakers, the mixture is uniformly stirred once every 3min, and after 120min of treatment, supernatant is respectively taken and filtered, and the content of B is measured. As a result, the cotton cellulose strands of examples 1 to 4 and comparative example 5 were treated to have a B content of 1.1mg/L, 1.4mg/L, 1.6mg/L, 0.8mg/L, and 3.2mg/L in this order.
(6-2) fishing out the wires subjected to boron removal in the step (6-1), extruding to remove liquid, putting the wires into a group of 200ml polyethylene plastic bottles with capacity scales, respectively adding 200ml boiling water (deionized water, 100 ℃), putting the bottles into a 90 ℃ oven for regeneration, uniformly stirring once every 5min, respectively supplementing deionized water to 200ml after treating for 90min, sealing and cooling to room temperature, respectively taking supernatant, and filtering to measure the content of B. As a result, the B contents of the aqueous solutions in the cotton cellulose wire beakers of examples 1 to 4 were all 45.0mg/L or more, and the B contents of the aqueous solutions in the cotton cellulose wire beakers of comparative example 5 were 40.5mg/L, and the boron removal capacities were all restored to 90% or more of the original values, indicating that the hot water regeneration effect was good.
(6-3) fishing out each regenerated wire rod of (6-2) examples 1-4, extruding to remove liquid, putting back to 1000ml polyethylene plastic beaker, continuing to carry out (6-1) boron removal of 25 ℃ water solution containing 20mg/L of B and (6-2) hot water regeneration at 90-100 ℃, repeating till the tenth time, and as a result, completely repeating the boron removal effect of (6-1) and the regeneration effect of (6-2), namely, the second and subsequent hot water regeneration at 90-100 ℃ can also keep boron removal capacity more than 90% of original value.
(6-4) fishing out the regenerated wires of (6-3) examples 1-4 and (5-2) comparative example 5, extruding to remove liquid, putting the regenerated wires back to a 1000ml polyethylene plastic beaker, continuing to perform (6-1) boron removal treatment on the 25 ℃ aqueous solution containing 20mg/L of B, fishing out the boron-removed wires, extruding to remove liquid, putting the wires in a group of 100ml polyethylene plastic bottles with capacity scales, respectively adding 100ml of normal temperature dilute hydrochloric acid with the concentration of 0.2mol/L for regeneration, uniformly stirring once every 3min, filtering each supernatant after 30min treatment, and measuring the B content to calculate the B dissolution rate, wherein the boron removal capacity of the cotton cellulose wires of examples 1-4 and comparative example 5 can recover to more than 98% of the original value.
(6-5) fishing out the regenerated wires of (6-3) examples 1-4 respectively, extruding to remove liquid, putting the wires back to a 1000ml polyethylene plastic beaker, continuing to perform (6-4) the boron removal treatment of the 25 ℃ aqueous solution containing 20mg/L of B and the regeneration of 0.2mol/L normal temperature dilute hydrochloric acid in a 100ml polyethylene plastic bottle, and repeating for ten times, wherein the boron removal effect of (6-1) and the regeneration effect of the dilute acid of (6-4) are completely repeated.
(6-6) boron selective resin of comparative examples 9 to 10, 1.0g, was subjected to (6-1) the boron removal of 500ml of the 25 ℃ aqueous solution containing 20mg/L of B described in (6-1) and the regeneration of 0.2mol/L of normal temperature dilute hydrochloric acid in the 100ml polyethylene plastic bottle described in (6-4) in a 1000ml polyethylene plastic beaker, respectively, with the result that the amount of dissolved boron was only 15% and 23% of the amount of adsorbed boron.
(6-7) in a 1000ml polyethylene plastic beaker, 1.0g of the boron selective resin of comparative examples 9 to 10 was subjected to (6-1) 500ml of the aqueous solution containing 20mg/L of B at 25 ℃ described above and (6-4) regeneration with dilute hydrochloric acid at ordinary temperature in the 100ml polyethylene plastic bottle, but at a concentration of 0.3mol/L, respectively, to result in dissolved boron amounts of 92% and 93% of the adsorbed boron amount.
(6-8) boron selective resin of comparative examples 9 to 10, 1.0g, was subjected to (6-1) the deboronation of 500ml of the aqueous solution at 25 ℃ containing 20mg/L of B described in (6-1) and the regeneration of normal temperature dilute hydrochloric acid in the polyethylene plastic bottle of 100ml described in (6-4) in a polyethylene plastic beaker, respectively, but at a concentration of 0.4mol/L, resulting in the dissolved boron amounts of 97% and 98% of the adsorbed boron amounts.
In the above experiments of examples 5 to 6, the low-temperature boron removal effect and the regeneration effect with hot water or dilute acid at room temperature were not much different between the 4 parts of the methylsilicic acid-modified cotton cellulose strand prepared in example 2, which indicates that the reaction conditions during the preparation process, particularly the reaction conditions of sodium methylsilicate and the formation of-CH 2-O-Si (CH 3) (0H) 2, were stable and reliable.
Example 7
An 18.9L bucket of mountain spring water (boron 0.7mg/L, strontium 0.25mg/L, lithium 0.21mg/L, calcium 230mg/L, magnesium 46mg/L, metasilicic acid 28mg/L, pH7.4, CODMn 2.6mg/L in terms of O2) was taken, boric acid was added to the bucket as necessary to adjust the amount to 10.0mg/L of boron, no floc was formed after leaving for 5 days, and boron 5.0mg/L was again sampled and measured as the mountain spring water solution for the test of this example.
(7-1) Deboronization tests were carried out on the methylsilicic acid-modified cotton cellulose strands obtained in examples 1 to 4, respectively, as follows: respectively loading the spring water solution (25 ℃, pH 7.3) into 1000ml polyethylene plastic beakers, respectively adding 1.0g of cotton cellulose wires which are cut into 4-5mm in length, respectively stirring uniformly every 3min, taking supernatant after 90min treatment, filtering, and measuring the content of B. As a result, the methylsilicic acid-modified cotton cellulose strands of examples 1 to 4 were all able to treat the aqueous solution to a B content of 0.3mg/L or less.
(7-2) fishing out the wires subjected to boron removal in the step (7-1), extruding to remove liquid, putting the wires into a group of 200ml polyethylene plastic bottles with capacity scales, respectively adding 200ml boiling water (deionized water, 100 ℃), putting the bottles into a 90 ℃ oven for regeneration, uniformly stirring once every 5min, respectively supplementing deionized water to 500ml after treating for 90min, sealing and cooling to room temperature, respectively taking supernatant, and filtering to measure the content of B. As a result, the B content of the aqueous solution in the cotton cellulose wire beakers of examples 1 to 4 was 45.0mg/L or more, and the boron removal capacity was recovered to 90% or more of the original value, indicating that the hot water regeneration effect was good.
(7-3) taking out each wire rod after (7-2) examples 1-4 regeneration, squeezing to remove the liquid, putting back the wire rod into a 1000ml polyethylene plastic beaker, continuing to perform (7-1) boron removal of the 25 ℃ mountain spring water solution containing 10mg/L of B and (7-2) hot water regeneration at 90-100 ℃, repeating the above steps till the tenth time, and as a result, the boron removal effect of (7-1) and the regeneration effect of (7-2) can be completely repeated, namely, the boron removal capacity can be kept more than 90% of the original value by the second and subsequent hot water regeneration at 90-100 ℃.
(7-4) fishing out the regenerated wires in the (7-3) embodiments 1-4, extruding to remove liquid, then putting back to a 1000ml polyethylene plastic beaker, continuing to perform (7-1) boron removal treatment on the mountain spring water solution with the concentration of B10mg/L and at the temperature of 25 ℃, fishing out the wires after boron removal, extruding to remove liquid, putting in a group of 100ml polyethylene plastic bottles with marked lines with capacity, respectively adding 100ml of normal-temperature dilute hydrochloric acid with the concentration of 0.2mol/L for regeneration, uniformly stirring once every 3min, filtering supernatant after treatment for 40min, measuring the content of B, and calculating the dissolution rate of B, wherein the boron removal capacity of the cotton cellulose wires in the embodiments 1-4 can be recovered to be more than 97% of the original value.
Example 8
The methylsilicic acid modified cotton cellulose wires obtained in the examples 1 to 4 and the cotton cellulose wires obtained in the comparative example 7 are wound into 3 cylindrical coils (solid) with the outer diameter of 25mm and the height of 45mm respectively by a winding machine, the winding mode is oblique lamination, the included angle between adjacent wire layers along the central axis of the yarn is 25 degrees, the distance between yarns in the layers is less than or equal to 0.1mm, the tension in the winding and coiling processes is properly controlled, the density of the coils measured in the examples 1, 3 to 4 and 7 is 0.73 to 0.75g/mL, and the coil in the example 2 is 0.82g/mL. In the process of winding the coil, the cotton cellulose wire in the examples 1 to 4 is smoothly routed, the strength and the toughness of the prepared coil are better, and the coil prepared by the wire in the comparative example 7 is obviously harder; no granular impurities were seen between the cotton fibers of the example 1-4 strands, while granular impurities were seen between the cotton fibers of the comparative example 7 strands under an optical microscope.
(8-1) taking 1 each of the columnar coils made from the wires in the examples 1-4, respectively filling the columnar coils into the lower part of a polyethylene plastic pipe with the inner diameter of 25mm and the height of 1000mm, compacting and vertically fixing the columnar coils, continuously feeding mountain spring water containing 10.0mg/L of boron, 0.25mg/L of strontium, 0.21mg/L of lithium, 230mg/L of calcium, 46mg/L of magnesium, 28mg/L of metasilicic acid and pH of 7.4, which is described in the example 10, from the upper opening of the plastic pipe, controlling the flow rate of the mountain spring water to be 400ml/h (BV 9.0/h) to carry out a boron removal treatment test at 25 ℃, measuring the boron content of bottom effluent every 2 hours, and controlling the boron content to be lower than 0.20mg/L when each effluent is 6L and the boron content of the effluent is lower than 0.30mg/L when each effluent is 8L, wherein the columnar coils made from the wires in the examples 2 are still lower than 0.20mg/L when each effluent is 8L, and the effect is the best; when 8L of effluent is discharged, the effluent is stirred uniformly, the measured contents of strontium, lithium, calcium, magnesium and metasilicic acid are basically the same as those before boron removal, COD is basically unchanged, and the mouthfeel is not different from that before treatment.
(8-2) after 8L of water is discharged from each polyethylene plastic pipe (8-1), room-temperature water above the coil is immediately pumped out, a soft rubber sleeve with the height of 950mm is arranged outside the plastic pipe, 95 ℃ circulating hot water is introduced, 95 ℃ boron-removed spring water (containing boron, 0.18mg/L, strontium, 0.25mg/L, lithium, 0.21mg/L, calcium, 230mg/L, magnesium, 46mg/L and metasilicic acid, 28mg/L and pH 7.1) is injected above the coil in the plastic pipe, the water discharge flow rate is controlled to be 400ml/h (BV 9.0/h), the boron content is measured once every 10min, and the result is that the boron content of the discharged water is gradually reduced to 0.28mg/L from 46-53mg/L within 3h, and the regeneration is finished.
(8-3) stopping circulating hot water in the soft rubber sleeve added outside the regenerated plastic pipe in the step (8-2), introducing circulating water at 25 ℃, removing hot water above the coil, after the coil is cooled to room temperature, repeating the boron removal of the spring water at 25 ℃ in the step (8-1) and the regeneration of the hot water at 95 ℃ in the step (8-2) for 6 times, and basically repeating the conditions of (8-1) and (8-2) in each water outlet detection result.
(8-4) stopping adding the circulating hot water in the soft rubber sleeve arranged outside the regenerated plastic pipe in the step (8-3), introducing 15 ℃ circulating water, removing the hot water above the coil, cooling the coil to 20 ℃, cooling the room-temperature mountain spring water to 15 ℃ through a constant temperature tank, removing boron, regenerating the hot water at 95 ℃ in the step (8-2), repeating the steps for 3 times, and basically repeating the steps (8-1) and (8-2) according to the detection result of each water outlet.
Example 9
According to the wire preparation method of the embodiment 2 and the wire coil preparation method of the embodiment 8, a methyl silicate modified cotton cellulose wire is entrusted to be processed, spherical and solid wire coils with the outer diameter of 38-42mm are further manufactured, 100.3kg of boron-removing adsorbing material for industrial test is used, the winding mode of the spherical wire coils is obliquely laminated, the included angle between adjacent wire layers along the central axis of the yarn is 25-28 degrees, the distance between yarns in the layers is less than or equal to 0.1mm, the tension in the winding and winding processes is properly controlled, and the density of the spherical wire coils is measured to be 0.76g/mL. The prepared wires are white, tasteless and good in flexibility; 10 parts of each representative sample was observed under an optical microscope, and no granular impurity was observed.
In the embodiment, a boron removal test lateral line is arranged in a production workshop of barreled spring water, main equipment comprises a vertical boron removal test tank made of polypropylene materials and a matched hot water electric heater for regeneration, the states of normal-temperature boron removal and hot water regeneration can be switched through a water pipe control valve, the inflow water during the normal-temperature boron removal is mountain spring water flow after sedimentation, quartz sand filtration and active carbon filtration, the outflow water is subjected to ozone removal, disinfection and sterilization, the outflow water is subjected to ultrafiltration and then is bottled and sold on a filling line, and the waste hot water during the regeneration is discharged. The size of the boron removal tank is 350mm in inner diameter and 2200mm in height, the spherical coil boron removal adsorption material is completely filled, the filling volume is about 195L (the filling density is 514kg/m & lt 3 & gt), a proper amount of polypropylene plastic special-shaped ring distributed water flow is filled below a top water inlet and above a bottom water outlet, no dead volume is filled in the tank, and the filler is prevented from shaking and moving after the water is filled in the tank.
(9-1) in the primary deboronation operation process of the side line deboronation test, the index typical values of the inflow mountain spring water flow are 0.6-0.8mg/L of boron, 0.23mg/L of strontium, 0.19mg/L of lithium, 230mg/L of calcium, 40mg/L of magnesium and 30mg/L of metasilicic acid, 2.2mg/L of CODMn (measured as O2), pH7.3 and water temperature of 22-24 ℃; controlling the water flow rate to be 390L/h (2 BV/h), flushing for 2h after water is fed, discharging the discharged water, removing ozone from the discharged water, sterilizing, ultrafiltering, and then putting the water into a filling line for barreling and selling. On 0-40 days of the boron removal test, the effluent contains 0.15-0.20mg/L of boron; on the 41 th to 43 th days, the inflow rate is changed to 487L/h (2.5 BV/h), and the effluent contains 0.32 to 0.35mg/L of boron; on the 44 th to 46 th days, the water inflow rate is changed to 585L/h (3 BV/h), and the effluent contains 0.41 to 0.43mg/L of boron; after the 47 th day, the inflow rate is changed back to 390L/h (2 BV/h, the regeneration is maintained), the boron content of the effluent is 0.23-0.25mg/L, and the boron content of the effluent is increased to 0.28mg/L at the 83 th day; on the 100 th day, the boron content of the effluent rises to 0.30mg/L, the boron adsorption amount is calculated to be more than 0.5wt% of the adsorption material, and the treated water amount exceeds 950m & lt 3 > compared with the inlet water and the outlet water, the contents of strontium, lithium, calcium, magnesium and metasilicic acid, the pH value, the water temperature and the COD are basically unchanged, and the mouthfeel is not different from that before treatment.
(9-2) changing the (9-1) boron removal tank into a boron removal spring water containing 0.28mg/L of boron, 0.23mg/L of strontium, 0.19mg/L of lithium, 230mg/L of calcium, 40mg/L of magnesium, 30mg/L of metasilicic acid and pH7.3 for heating to obtain a hot water with the flow rate of 390L/h (2 BV/h) and the temperature of 95-100 ℃, and taking and measuring the boron content once every 20min, so that the boron content of the effluent water is gradually increased to 40mg/L within 3h and then gradually decreased to 0.8mg/L, then the heater is powered off, the water flow is unchanged, and the regeneration is finished when the boron removal spring water containing 0.28mg/L is continuously flushed to 35 ℃ of the effluent water. The regeneration process was continued for 7h with 2.7m3 of water.
(9-3) continuing to perform (9-1) boron removal of the spring water and (9-2) regeneration of the hot water at the temperature of 95-100 ℃, repeating the steps till the third time, and basically repeating the steps (9-1) and (9-2) according to the detection results of the effluent.
(9-4) continuing (9-1) boron removal of the spring water and (9-2) regeneration of the hot water at the temperature of 95-100 ℃, but directly adopting the non-boron-removed spring water as the hot water and a cooling water source during regeneration, basically repeating the conditions of (9-1) and (9-2) on the detection results of each effluent, gradually increasing the boron content of the effluent to 41mg/L within 3h during regeneration, then gradually reducing the boron content to 1.2mg/L, then powering off a heater, and continuously flushing for 4h until the regeneration is finished when the temperature of the effluent is 32 ℃; carrying out fifth boron removal after regeneration is finished, confirming the relation between boron removal precision and water amount to basically repeat (9-1), and increasing the boron content of the discharged water to 0.28mg/L at 80 days; at 96 days, the boron content in the effluent rises to 0.30mg/L, the boron adsorption amount is calculated to be more than 0.5wt% of the adsorption material, and the treated water amount exceeds 900m 3 (ii) a Compared with the inlet water and the outlet water, the contents of strontium, lithium, calcium, magnesium and metasilicic acid, the pH value, the water temperature and the COD are basically unchanged, and the mouthfeel is not different from that before treatment.
Claims (9)
1. A boron removal treatment method of mountain spring water comprises the following steps: settling source water, filtering with quartz sand and active carbon, controlling temperature at 15-25 deg.C for removing boron, sterilizing with ultraviolet ray or ozone, micro-filtering or ultrafiltering, and bottling or barreling to obtain mountain spring aquatic product;
wherein the boron removal treatment is carried out by filling a cotton cellulose boron removal adsorption material modified by methyl silicic acidCarrying out the treatment in a boron removal tank; the methyl silicic acid modified cotton cellulose boron removal adsorption material is prepared by the following steps: (a) Carrying out mercerization modification and drying on cotton yarns with the outer diameter of 0.3-1.0mm by an alkali liquor method to obtain a methyl silicic acid modified cotton cellulose wire; (b) Winding the cotton cellulose wire modified by the methyl silicic acid into a spherical, ellipsoidal or columnar coil with the external dimension of 30-50mm to obtain the cotton cellulose boron removal adsorbing material modified by the methyl silicic acid; the mercerizing modification conditions in the step (a) are as follows: firstly, the temperature is 20-30 ℃, the solution contains 200-220g/L of NaOH, 30-50g/L of sodium methylsilicate and H 2 O 2 2-3g/L of stabilizer AR 702-20 g/L and 0.5-1.0g/L of penetrant GFC, soaking in alkali liquor for 120-240s, stretching for 3-4 times in the alkali soaking process, soaking in acid liquor containing 10-30g/L of HCl at 20-40 ℃ for 20-60min, squeezing to remove the solution, and washing with water to pH6-8.
2. The method of boron removal from spring water of claim 1, wherein said cotton yarn of step (a) has a gauge of 6S/4, 6S/6, 12S/4 or 12S/6.
3. The method for boron removal treatment of spring water as claimed in claim 1, wherein before said mercerization modification in step (a), cotton yarn is further subjected to singeing treatment under flame temperature 900-1000 ℃ with weight loss of cotton yarn controlled to be less than or equal to 2wt%.
4. The method for boron removal from mineral water according to claim 1, wherein the boron removal adsorbent material of cotton cellulose modified with methyl silicate in step (b) is wound in a manner of oblique lamination, the included angle between adjacent layers along the central axis of the yarn is 20-30 °, the spacing between yarns in the layers is less than or equal to 0.1mm, and the bulk density is 400-550kg/m 3 。
5. The method for boron removal treatment of spring water as claimed in claim 4, wherein said methyl silicic acid modified cotton cellulose boron removal adsorbing material of step (b) has bulk density and strength adjusted by tension and line spacing during winding and agglomerating.
6. The method for boron removal treatment of spring water according to claim 1, wherein the treatment flow rate of water in the boron removal tank is 0.4-5BV/h.
7. The method for boron removal treatment of mineral water as claimed in claim 1, wherein said methyl silicate modified cotton cellulose boron removal absorbent material in boron removal tank is regenerated in-situ in 90-100 ℃ hot water or 0.2-0.3mol/L diluted acid at normal temperature.
8. The method for boron removal from spring water according to claim 7, wherein spring water having a B content of less than 1.0mg/L is used for regeneration, and the resulting hot water is heated to obtain a regenerated liquid; the flow direction of the regeneration liquid is the same as that of the spring water during the boron removal treatment, the flow rate is 0.5-3BV/h, the liquid consumption is 2-8BV, and then the regeneration liquid is washed to below 35 ℃ by 1-10BV/h of spring water with the B content lower than 1.0 mg/L.
9. The method for boron removal from spring water of claim 7, wherein dilute acid prepared from spring water having a B content of less than 1.0mg/L is used as the regenerating liquid; the flow direction of the regeneration liquid is the same as that of the spring water during the boron removal treatment, the flow rate is 0.5-3BV/h, the liquid consumption is 2-8BV, and then the regeneration liquid is washed to the pH value of more than 6 by 1-10BV/h of spring water with the B content of less than 1.0 mg/L.
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