CN103339317A - 使用氧化剂在还原条件下进行微生物控制的方法 - Google Patents
使用氧化剂在还原条件下进行微生物控制的方法 Download PDFInfo
- Publication number
- CN103339317A CN103339317A CN201280006357XA CN201280006357A CN103339317A CN 103339317 A CN103339317 A CN 103339317A CN 201280006357X A CN201280006357X A CN 201280006357XA CN 201280006357 A CN201280006357 A CN 201280006357A CN 103339317 A CN103339317 A CN 103339317A
- Authority
- CN
- China
- Prior art keywords
- aldehyde
- halogen
- source
- ammonium
- stable compound
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims description 38
- 239000007800 oxidant agent Substances 0.000 title claims description 24
- 230000000813 microbial effect Effects 0.000 title abstract description 4
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 46
- 150000002367 halogens Chemical class 0.000 claims abstract description 46
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 150000001299 aldehydes Chemical class 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 24
- 230000001590 oxidative effect Effects 0.000 claims description 24
- 229910010277 boron hydride Inorganic materials 0.000 claims description 18
- -1 dihydroxymethyl dimethyl hydantoin Chemical compound 0.000 claims description 18
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 229920001131 Pulp (paper) Polymers 0.000 claims description 11
- 244000005700 microbiome Species 0.000 claims description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 9
- 239000000460 chlorine Substances 0.000 claims description 8
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 8
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 8
- 238000004061 bleaching Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 6
- 150000001469 hydantoins Chemical class 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 4
- PMDCZENCAXMSOU-UHFFFAOYSA-N N-ethylacetamide Chemical compound CCNC(C)=O PMDCZENCAXMSOU-UHFFFAOYSA-N 0.000 claims description 4
- XGEGHDBEHXKFPX-UHFFFAOYSA-N N-methyl urea Chemical compound CNC(N)=O XGEGHDBEHXKFPX-UHFFFAOYSA-N 0.000 claims description 4
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- CVSVTCORWBXHQV-UHFFFAOYSA-N creatine Chemical compound NC(=[NH2+])N(C)CC([O-])=O CVSVTCORWBXHQV-UHFFFAOYSA-N 0.000 claims description 4
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 4
- 229940015043 glyoxal Drugs 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- GTCAXTIRRLKXRU-UHFFFAOYSA-N methyl carbamate Chemical compound COC(N)=O GTCAXTIRRLKXRU-UHFFFAOYSA-N 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- AWMNXQXKGOSXDN-GORDUTHDSA-N (e)-ethylideneurea Chemical compound C\C=N\C(N)=O AWMNXQXKGOSXDN-GORDUTHDSA-N 0.000 claims description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims description 2
- KGLPWQKSKUVKMJ-UHFFFAOYSA-N 2,3-dihydrophthalazine-1,4-dione Chemical compound C1=CC=C2C(=O)NNC(=O)C2=C1 KGLPWQKSKUVKMJ-UHFFFAOYSA-N 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 claims description 2
- SHVCSCWHWMSGTE-UHFFFAOYSA-N 6-methyluracil Chemical compound CC1=CC(=O)NC(=O)N1 SHVCSCWHWMSGTE-UHFFFAOYSA-N 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- 239000004471 Glycine Substances 0.000 claims description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 2
- WZELXJBMMZFDDU-UHFFFAOYSA-N Imidazol-2-one Chemical compound O=C1N=CC=N1 WZELXJBMMZFDDU-UHFFFAOYSA-N 0.000 claims description 2
- VGGLHLAESQEWCR-UHFFFAOYSA-N N-(hydroxymethyl)urea Chemical compound NC(=O)NCO VGGLHLAESQEWCR-UHFFFAOYSA-N 0.000 claims description 2
- FZERHIULMFGESH-UHFFFAOYSA-N N-phenylacetamide Chemical compound CC(=O)NC1=CC=CC=C1 FZERHIULMFGESH-UHFFFAOYSA-N 0.000 claims description 2
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 claims description 2
- DSMLVDLNGGAGGK-UHFFFAOYSA-N [P].C(O)OS(O)(=O)=O Chemical compound [P].C(O)OS(O)(=O)=O DSMLVDLNGGAGGK-UHFFFAOYSA-N 0.000 claims description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- HNYOPLTXPVRDBG-UHFFFAOYSA-N barbituric acid Chemical compound O=C1CC(=O)NC(=O)N1 HNYOPLTXPVRDBG-UHFFFAOYSA-N 0.000 claims description 2
- CODNYICXDISAEA-UHFFFAOYSA-N bromine monochloride Chemical compound BrCl CODNYICXDISAEA-UHFFFAOYSA-N 0.000 claims description 2
- AVMMISONJSPCFD-UHFFFAOYSA-N bromine;chloroethene Chemical compound [Br].ClC=C AVMMISONJSPCFD-UHFFFAOYSA-N 0.000 claims description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 229960003624 creatine Drugs 0.000 claims description 2
- 239000006046 creatine Substances 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- BEBCJVAWIBVWNZ-UHFFFAOYSA-N glycinamide Chemical compound NCC(N)=O BEBCJVAWIBVWNZ-UHFFFAOYSA-N 0.000 claims description 2
- VPVSTMAPERLKKM-UHFFFAOYSA-N glycoluril Chemical compound N1C(=O)NC2NC(=O)NC21 VPVSTMAPERLKKM-UHFFFAOYSA-N 0.000 claims description 2
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 claims description 2
- 150000002475 indoles Chemical class 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- XBCXJKGHPABGSD-UHFFFAOYSA-N methyluracil Natural products CN1C=CC(=O)NC1=O XBCXJKGHPABGSD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- GKRZNOGGALENQJ-UHFFFAOYSA-N n-carbamoylacetamide Chemical compound CC(=O)NC(N)=O GKRZNOGGALENQJ-UHFFFAOYSA-N 0.000 claims description 2
- YCWSUKQGVSGXJO-NTUHNPAUSA-N nifuroxazide Chemical group C1=CC(O)=CC=C1C(=O)N\N=C\C1=CC=C([N+]([O-])=O)O1 YCWSUKQGVSGXJO-NTUHNPAUSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 claims description 2
- 150000003053 piperidines Chemical class 0.000 claims description 2
- 238000004076 pulp bleaching Methods 0.000 claims description 2
- 239000013055 pulp slurry Substances 0.000 claims description 2
- VTGOHKSTWXHQJK-UHFFFAOYSA-N pyrimidin-2-ol Chemical compound OC1=NC=CC=N1 VTGOHKSTWXHQJK-UHFFFAOYSA-N 0.000 claims description 2
- 150000003233 pyrroles Chemical class 0.000 claims description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 2
- 150000004040 pyrrolidinones Chemical class 0.000 claims description 2
- YOWAEZWWQFSEJD-UHFFFAOYSA-N quinoxalin-2-amine Chemical compound C1=CC=CC2=NC(N)=CN=C21 YOWAEZWWQFSEJD-UHFFFAOYSA-N 0.000 claims description 2
- RWQNBRDOKXIBIV-UHFFFAOYSA-N thymine Chemical compound CC1=CNC(=O)NC1=O RWQNBRDOKXIBIV-UHFFFAOYSA-N 0.000 claims description 2
- 150000003673 urethanes Chemical class 0.000 claims description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims 2
- GUQMDNQYMMRJPY-UHFFFAOYSA-N 4,4-dimethyl-1,3-oxazolidine Chemical compound CC1(C)COCN1 GUQMDNQYMMRJPY-UHFFFAOYSA-N 0.000 claims 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims 1
- 229910001616 alkaline earth metal bromide Inorganic materials 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- 230000003115 biocidal effect Effects 0.000 abstract description 6
- 239000003139 biocide Substances 0.000 abstract description 5
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 2
- 238000012360 testing method Methods 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000012279 sodium borohydride Substances 0.000 description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- XZXYQEHISUMZAT-UHFFFAOYSA-N 2-[(2-hydroxy-5-methylphenyl)methyl]-4-methylphenol Chemical compound CC1=CC=C(O)C(CC=2C(=CC=C(C)C=2)O)=C1 XZXYQEHISUMZAT-UHFFFAOYSA-N 0.000 description 1
- QNGVNLMMEQUVQK-UHFFFAOYSA-N 4-n,4-n-diethylbenzene-1,4-diamine Chemical compound CCN(CC)C1=CC=C(N)C=C1 QNGVNLMMEQUVQK-UHFFFAOYSA-N 0.000 description 1
- YIROYDNZEPTFOL-UHFFFAOYSA-N 5,5-Dimethylhydantoin Chemical compound CC1(C)NC(=O)NC1=O YIROYDNZEPTFOL-UHFFFAOYSA-N 0.000 description 1
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 description 1
- 229940107816 ammonium iodide Drugs 0.000 description 1
- QHYIGPGWXQQZSA-UHFFFAOYSA-N azane;methanesulfonic acid Chemical compound [NH4+].CS([O-])(=O)=O QHYIGPGWXQQZSA-UHFFFAOYSA-N 0.000 description 1
- PQRDTUFVDILINV-UHFFFAOYSA-N bcdmh Chemical compound CC1(C)N(Cl)C(=O)N(Br)C1=O PQRDTUFVDILINV-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001332 colony forming effect Effects 0.000 description 1
- 125000000950 dibromo group Chemical group Br* 0.000 description 1
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- WSDISUOETYTPRL-UHFFFAOYSA-N dmdm hydantoin Chemical compound CC1(C)N(CO)C(=O)N(CO)C1=O WSDISUOETYTPRL-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- YIEDHPBKGZGLIK-UHFFFAOYSA-L tetrakis(hydroxymethyl)phosphanium;sulfate Chemical compound [O-]S([O-])(=O)=O.OC[P+](CO)(CO)CO.OC[P+](CO)(CO)CO YIEDHPBKGZGLIK-UHFFFAOYSA-L 0.000 description 1
- AVWRKZWQTYIKIY-UHFFFAOYSA-N urea-1-carboxylic acid Chemical compound NC(=O)NC(O)=O AVWRKZWQTYIKIY-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/14—Boron; Compounds thereof
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/08—Removal of fats, resins, pitch or waxes; Chemical or physical purification, i.e. refining, of crude cellulose by removing non-cellulosic contaminants, optionally combined with bleaching
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/36—Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/1026—Other features in bleaching processes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/1084—Bleaching ; Apparatus therefor with reducing compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/11—Halides
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
通过添加醛或醛源，接着添加活性卤素杀生物剂来控制含有硼氢化物残留的水系统中的微生物的生长。该活性卤素杀生物剂优选通过N-氢化合物来稳定。
Description
技术领域
本发明涉及一种控制在含有硼氢化物的水系统（aqueous system）中的微生物生长的方法，该水系统例如施加硼氢化物基还原漂白剂后得到的溶液或悬浮液。本发明还涉及一种在有还原条件的水系统中稳定活性卤素杀生物剂的方法。
背景技术
化学物质或组合物的氧化或还原的能力通常是由其氧化-还原（“氧化还原（redox）”）电位（ORP）来量化的。物质或组合物的ORP越低（即，越负），其还原效果越强。
还原漂白剂经常使用于造纸应用中。这种类型的漂白过程中的一种采用硼氢化物（BH4 -）化学品。当提高纸张的亮度的同时，这样的解决方案的使用也会导致生产的纸浆中硼氢化物的残留。这些残留造成提供极端的还原条件（ORP低至-500至-600mV）。硼氢化物残留使得纸浆保存和后续造纸机沉积物的控制更加困难，这是因为许多主要的造纸杀粘菌剂和防腐剂（如二溴次氮基二乙酮-酰胺、异噻唑啉酮），以及特别是氧化性杀生物剂在硼氢化物的存在下是不稳定的。
令人惊讶的是，已经发现，通过使用醛或醛源，在还原条件下（负ORP）施加氧化性杀生物剂至含有残留的硼氢化物的系统是可行的，且即使在这种条件下也可以提供残余的卤素和微生物控制。
在还原条件下卤素的中和作用是众所周知的，且通过标准方法（如ORP控制器或滴定分析方法）通常会妨碍适当的系统控制。已经发现，使用醛或醛源以使得ORP达到大于约-350mV的水平，使得通常不相容的还原剂和氧化剂材料能够在足以用于通过标准的N,N-二乙基-对-苯二胺（DPD）滴定分析方法进行微生物控制应用并分析的时间周期共存。
发明内容
根据本发明，通过调节和维持ORP>-350mV，优选>-300mV，更优选>-250mV时，通过在引入氧化剂到所述水系统之前，将醛或醛源与含硼氢化物的水系统接触一段时间，然后通过添加氧化剂化学品（如次氯酸钠）、稳定氧化剂（如溴氯二甲基乙内酰脲）、或氧化剂化学品和稳定剂化学品的组合物（如次氯酸钠与5,5-二甲基乙内酰脲组合），来控制在含有硼氢化物残留的水系统中的微生物生长。
本文中醛源（或醛供体）是一种能够释放，或分解成一个或多个醛分子的化合物。下面给出的摩尔比涉及存在或产生的醛的量，或具有两个或两个以上的醛基（如乙二醛或戊二醛）的醛的量，涉及一价醛的当量。
优选的醛和醛源包括二羟甲基二甲基乙内酰脲（dimethyloldimethylhydantoin）、戊二醛、三嗪、六亚甲基四胺、甲醛、乙二醛、四羟甲基硫酸磷（bis[tetrakis(hydroxymethyl)phosphonium]sulfate）、乙缩醛（如二甲氧基甲烷）、和上述物质的混合物。
优选的氧化剂或氧化剂的混合物包括卤素源，如次氯酸钠、次氯酸钠和溴化钠，溴氯乙内酰脲，二溴乙内酰脲，二氯乙内酰脲。在一种优选的实施方案中，活性卤源选自：元素氯、元素溴、溴氯化物、碱金属次卤酸盐、碱土金属次卤酸盐、单或二卤代乙内酰脲、卤化氰尿酸酯、卤化氰脲酸、和上述物质彼此之间的混合物和/或带有溴化钠。最优选的活性卤素源是碱金属次卤酸盐，特别是次氯酸钠。
氧化剂或氧化剂的混合物也可以与含有至少一种卤素稳定化合物（如任选取代的N-氢化合物）的溶液或组合物结合。具体而言，包含至少一个N-氢化合物的组合物选自：对位-甲苯磺酰胺、5,5-二烷基乙内酰脲、甲磺酰胺、巴比土酸、5-甲基尿嘧啶、咪唑啉、吡咯烷酮、吗啉、乙酰苯胺、乙酰胺、N-乙基乙酰胺、邻苯二甲酰亚胺、苯并酰胺、丁二酰亚胺、N-羟甲基脲、N-甲基脲、乙酰脲、脲基甲酸酯、氨基甲酸甲酯、邻苯二甲酰肼、吡咯、吲哚、甲酰胺、N-甲基甲酰胺、双氰胺、氨基甲酸乙酯、1,3-二甲基缩二脲、甲基苯基缩二脲、4,4-二甲基-2-恶唑烷酮、6-甲基尿嘧啶、2-咪唑啉酮、亚乙基脲、2-嘧啶酮、氮杂环丁-2-酮、2-吡咯烷酮、己内酰胺、苯基亚磺酰亚胺（phenylsulfinimide）、苯基亚磺酰亚胺基酰胺（phenylsulfin-imidylamide）、二芳基亚磺酰亚胺（diarylsulfinimides）、二烷基亚磺酰亚胺（dialkylsulfinimide）、异噻唑啉-1,1-二氧化物、乙内酰脲、甘氨酸、哌啶、哌嗪、乙醇胺、甘氨酰胺、肌酸、甘脲、氨、铵盐、和尿素。
优选的铵盐包括卤化铵，如氟化铵、氯化铵、溴化铵或碘化铵，硫酸铵，硫酸氢铵，碳酸氢铵，碳酸铵，氨基甲酸铵，烷基磺酸铵（如甲磺酸铵），烷基硫酸铵，和羧酸铵（如甲酸铵，乙酸铵），以及上述物质的混合物。
整个说明书中，相对量有时由范围来定义，并由范围的下边界和上边界所定义。每个下边界可以与每个上边界结合来定义范围。下边界和上边界应被视为单独的元素。
含有至少一个N-氢化合物的上述组合物可以有效地稳定在还原条件下在水溶液中的活性卤素源。
硼氢化物与醛化合物的摩尔比优选为2:1至1:20，更优选为1:1至1:15，最优选为1:2至1:10。
活性卤素与附加的N-氢化合物的摩尔比优选在20:1至0.1:1的范围内，优选在10:1至0.2:1的范围内，最优选在5:1至2:1的范围内。
上述组合物可有利地使用在水溶液中，该水溶液具有在3至11的范围内的pH值，优选在5至10的范围内的pH值，并且更优选在7至9.5的范围内的pH值。
为了稳定在水溶液中的活性卤素源，在水溶液中的所述活性卤素源可以混合上述组合物。
替代地，在水溶液中的活性卤素源可以将其混合含有上述组合物的上述水溶液来稳定。
可以从根据本发明在还原条件下使用氧化剂和稳定氧化剂受益的应用包括纸浆和造纸、再生纸制浆和造纸、纸浆或生物质量漂白、织物漂白、以及类似的应用。
在一种优选的实施方式中，通过N-氢化合物稳定的活性卤素（作为Cl2）的浓度为0.1至20ppm。在这里和下文中，表述“作为Cl2（asCl2）”表示元素氯的浓度化学计量等于给定的系统中的活性卤素的浓度。
优选的水系统是纸浆和造纸浆料和浆剂、回收纸浆浆料、纸浆浓坯料（pulp thick stock）、脱墨纸浆浆料、纸浆漂白浆料和液体、织物漂白液和粘土泥浆。
根据本发明，通过在共施加活性卤素之前的短暂时间段施加醛类化合物，以及通过在还原条件下使用氧化剂的能力，可以实现微生物控制的优化的成本性能。由于在还原条件下氧化剂的快速中和，以及无法监视系统中的残留的氧化剂，在还原条件下使用氧化剂已被禁止至今。目前的发明提供了用于协同地利用这些化合物类的方法。
以下的非限制性实施例旨在更详细地说明本发明。
具体实施方式
表述“CFU/mL”是指每毫升菌落形成单位。除非另有说明，所有的浓度单位为按重量计的百分比或ppm。
在21℃混合含有硼氢化钠的水溶液，以得到具有初始硼氢化物（如硼氢化钠）含量为30-50ppm的溶液，碱度（作为CaCO3）为400ppm，pH值为8.5-9.5。将溶液的温度保持在21℃，并以指定的时间间隔测量溶液的ORP。该过程包括以相对于硼氢化物含量的公知的摩尔比加入已知量的醛供体（如二羟甲基二甲基乙内酰脲或乙二醛）到实施例，并随后进行时间相关的ORP。
为了证明在还原条件下的氧化剂的相容性，将次氯酸钠与N-氢化合物（如5,5-二甲基乙内酰脲钠）结合，并以不同的时间间隔加入到上述的溶液中，结果导致不同的ORP。然后随着时间的推移残余的卤素浓度通过标准的DPD总卤素的方法来测量。
实施例1：
在表1中显示了醛供体减弱硼氢化物还原性漂白水的ORP的能力，显示了醛供体的添加之后，ORP结果随着时间的推移而增加。
表1
实施例2：
为了证明本发明的方法即使在还原条件下（负ORP）的稳定卤素氧化剂的有效性，将次氯酸钠添加到以上面描述的方式制备的硼氢化钠溶液，用二羟甲基二甲基乙内酰脲钠处理的溶液且对残留的总卤素（作为Cl2）进行分析。为了对比，对残余的总卤素（作为Cl2）不使用二羟甲基二甲基乙内酰脲钠进行分析。
表2
实施例3：
研究了即使在还原条件下的卤素释放时表现出杀生物性能的稳定的氧化剂的能力。将NaBH4加入到来自北美（North American）造纸厂的处理水，目标是残留的硼氢化物（作为NaBH4）含量为35ppm。对未处理的对照、硼氢化物处理的对照、醛处理过的样品、以及醛+稳定的卤素处理的样品（目标2ppm总Cl2剂量）进行了测试。测量了在37℃下在3小时后的初始和最终的ORP，以及3小时后的存在的残留卤素。在测试之前24-48小时由纸浆提供微生物种群，并在37℃下储存，从而使微生物生长达到高的测试水平。
使用Warren MI，Biosan Laboratories，Inc.的SaniCheck浸渍玻片分析微生物种群。报告的种群是通过比较标准图表四舍五入到最接近的10次方的需氧细菌（aerobic）总数。该测试结果示于表3。
表3
上面的实施例表明，醛供体的存在提高了ORP，且在负的ORP值的卤素稳定提供了一种方法，通过该方法氧化剂在还原条件下表现出微生物控制而不立即中和。
Claims (24)
1.一种控制在含有硼氢化物残留的水系统中的微生物生长的方法，所述方法包括添加醛或醛源到所述水系统中，然后添加氧化剂，所述氧化剂是活性卤素源，以使得在还原条件下提供残留氧化剂水平。
2.根据权利要求1所述的方法，其中，所述醛或醛源以足以达到大于-350mV的ORP的量来添加。
3.根据权利要求2所述的方法，其中，所述醛或醛源以足以达到大于-300mV的ORP的量来添加。
4.根据权利要求3所述的方法，其中，所述醛或醛源以足以达到大于-250mV的ORP的量来添加。
5.根据权利要求1至4中的任何一项所述的方法，其中，所述醛或醛源选自：二羟甲基二甲基乙内酰脲、戊二醛、三嗪、六亚甲基四胺、甲醛、4,4-二甲基恶唑烷、四氢-3,5-二甲基-2H-1,3,5-噻二嗪-2-硫酮、乙二醛、四羟甲基硫酸磷、乙缩醛、和上述物质的混合物。
6.根据权利要求1至5中的任何一项所述的方法，其中，所述活性卤素源选自：元素氯、元素溴、溴氯化物、碱金属次卤酸盐、碱土金属次卤酸盐、结合溴化物的碱金属或碱土金属溴化物、单卤代乙内酰脲、二卤代乙内酰脲、卤化氰尿酸酯、卤化氰脲酸、和上述物质的混合物。
7.根据权利要求6所述的方法，其中，所述活性卤素源选自：溴氯乙内酰脲、二溴乙内酰脲、二氯乙内酰脲、和上述物质的混合物。
8.根据权利要求6所述的方法，其中，所述活性卤素源选自：次氯酸钠和次氯酸钠/溴化钠。
9.根据权利要求1至8中的任何一项所述的方法，其中，所述活性卤素源与包含至少一种卤素稳定化合物的溶液或组合物结合。
10.根据权利要求9所述的方法，其中，所述至少一种卤素稳定化合物为N-氢化合物，该N-氢化合物选自：对位-甲苯磺酰胺、5,5-二烷基乙内酰脲、甲磺酰胺、巴比土酸、5-甲基尿嘧啶、咪唑啉、吡咯烷酮、吗啉、乙酰苯胺、乙酰胺、N-乙基乙酰胺、邻苯二甲酰亚胺、苯并酰胺、丁二酰亚胺、N-羟甲基脲、N-甲基脲、乙酰脲、脲基甲酸甲酯、氨基甲酸甲酯、邻苯二甲酰肼、吡咯、吲哚、甲酰胺、N-甲基甲酰胺、双氰胺、氨基甲酸乙酯、1,3-二甲基缩二脲、甲基苯基缩二脲、4,4-二甲基-2-恶唑烷酮、6-甲基尿嘧啶、2-咪唑啉酮、亚乙基脲、2-嘧啶酮、氮杂环丁-2-酮、2-吡咯烷酮、己内酰胺、苯基亚磺酰亚胺、苯基亚磺酰亚胺基酰胺、二芳基亚磺酰亚胺、二烷基亚磺酰亚胺、异噻唑啉-1,1-二氧化物、乙内酰脲、甘氨酸、哌啶、哌嗪、乙醇胺、甘氨酰胺、肌酸、甘脲、氨、铵盐、和尿素。
11.根据权利要求10所述的方法，其中，所述至少一种卤素稳定化合物选自：卤化铵、硫酸铵、硫酸氢铵、碳酸氢铵、碳酸铵、氨基甲酸铵、烷基磺酸铵、烷基硫酸铵、和羧酸铵、以及上述物质的混合物。
12.根据权利要求1至11中的任何一项所述的方法，其中，硼氢化物与醛或醛源的摩尔比为2:1至1:20。
13.根据权利要求12所述的方法，其中，硼氢化物与醛或醛源的所述摩尔比为1:1至1:15。
14.根据权利要求13所述的方法，其中，硼氢化物与醛或醛源的所述摩尔比为1:2至1:10。
15.根据权利要求10至14中的任何一项所述的方法，其中，活性卤素与额外的N-氢化合物的摩尔比在20:1至0.1:1的范围内。
16.根据权利要求15所述的方法，其中，活性卤素与额外的N-氢化合物的所述摩尔比在10:1至0.2:1的范围内。
17.根据权利要求16所述的方法，其中，活性卤素与额外的N-氢化合物的所述摩尔比在5:1至2:1的范围内。
18.根据权利要求10至17中的任何一项所述的方法，其中，所述包含至少一种卤素稳定化合物的溶液或组合物是具有pH值在3至11的范围内的水溶液。
19.根据权利要求18所述的方法，其中，所述包含至少一种卤素稳定化合物的溶液或组合物是具有pH值在5至10的范围内的水溶液。
20.根据权利要求19所述的方法，其中，所述包含至少一种卤素稳定化合物的溶液或组合物是具有pH值在7至9.5的范围内的水溶液。
21.根据权利要求10至20中的任何一项所述的方法，其中，所述活性卤素源在水溶液中，并且与所述包含所述至少一种卤素稳定化合物的组合物混合。
22.根据权利要求10至20中的任何一项所述的方法，其中，所述活性卤素源在水溶液中，并且与包含所述包含所述至少一种卤素稳定化合物的所述组合物的水溶液混合。
23.根据权利要求10至22中的任何一项所述的方法，其中，由所述至少一种卤素稳定化合物稳定的活性卤素的浓度为0.1至20ppm。
24.根据权利要求1至23中的任何一项所述的方法，其中，所述水系统选自：纸浆和造纸浆料与浆剂、回收纸浆浆料、纸浆浓坯料、脱墨纸浆浆料、纸浆漂白浆料和液体、生物质漂白浆料和液体、织物漂白液和粘土泥浆。
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| CN105735045A (zh) * | 2014-12-25 | 2016-07-06 | 栗田工业株式会社 | 纸制造装置及排水处理方法 |
| CN109418261A (zh) * | 2017-08-25 | 2019-03-05 | 三博生化科技（上海）有限公司 | 一种氧化还原电位调整剂、其制备方法及其应用 |
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| RU2609245C2 (ru) | 2011-09-30 | 2017-01-31 | Кемира Ойй | Предотвращение деградации крахмала при производстве целлюлозы, бумаги или картона |
| US9908796B2 (en) | 2012-10-23 | 2018-03-06 | Ecolab Usa Inc. | Use of oxidizing and non-oxidizing biocides for control of bacteria tolerant to stabilized-oxidant treatment |
| SI3357870T1 (sl) | 2013-02-07 | 2022-10-28 | A. Y. Laboratories Ltd. | Postopek in naprava za izdelavo biocida |
| US10118849B2 (en) | 2013-04-26 | 2018-11-06 | Arch Chemicals, Inc. | Method and kit for treating recreational water |
| AR105031A1 (es) * | 2015-06-25 | 2017-08-30 | Dow Global Technologies Llc | Composición microbicida |
| FI128324B (en) * | 2017-06-21 | 2020-03-31 | Kemira Oyj | Process for making fiber web |
| EP3450623B1 (en) | 2017-08-29 | 2023-06-28 | Kemira Oyj | Method for controlling growth of microorganisms and/or biofilms in an industrial process |
| EP3450626B1 (en) | 2017-08-29 | 2020-05-06 | Kemira Oyj | Method for controlling growth of microorganisms and/or biofilms in an industrial process |
| US11857939B2 (en) | 2020-09-04 | 2024-01-02 | Buckman Laboratories International, Inc. | Predictive systems and methods for proactive intervention in chemical processes |
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- 2012-01-20 WO PCT/EP2012/050856 patent/WO2012101051A1/en active Application Filing
- 2012-01-20 CN CN201280006357.XA patent/CN103339317B/zh active Active
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| CN1535250A (zh) * | 2001-06-29 | 2004-10-06 | 隆萨公司 | 产生卤素的杀生物剂、卤素稳定剂和含氮杀生物剂的混合物 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105735045A (zh) * | 2014-12-25 | 2016-07-06 | 栗田工业株式会社 | 纸制造装置及排水处理方法 |
| CN105735045B (zh) * | 2014-12-25 | 2018-09-25 | 栗田工业株式会社 | 纸制造装置及排水处理方法 |
| CN109418261A (zh) * | 2017-08-25 | 2019-03-05 | 三博生化科技（上海）有限公司 | 一种氧化还原电位调整剂、其制备方法及其应用 |
| CN109418261B (zh) * | 2017-08-25 | 2021-10-26 | 三博生物科技(上海)有限公司 | 一种氧化还原电位调整剂、其制备方法及其应用 |
Also Published As
| Publication number | Publication date |
|---|---|
| US8808500B2 (en) | 2014-08-19 |
| EP2668329A1 (en) | 2013-12-04 |
| AR085028A1 (es) | 2013-08-07 |
| CN103339317B (zh) | 2016-01-20 |
| JP5985511B2 (ja) | 2016-09-06 |
| US20130302443A1 (en) | 2013-11-14 |
| JP2014509253A (ja) | 2014-04-17 |
| WO2012101051A1 (en) | 2012-08-02 |
| HK1190176A1 (zh) | 2014-06-27 |
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