CN100577726C - 抗生物腐败的聚合物乳液 - Google Patents
抗生物腐败的聚合物乳液 Download PDFInfo
- Publication number
- CN100577726C CN100577726C CN200410044572A CN200410044572A CN100577726C CN 100577726 C CN100577726 C CN 100577726C CN 200410044572 A CN200410044572 A CN 200410044572A CN 200410044572 A CN200410044572 A CN 200410044572A CN 100577726 C CN100577726 C CN 100577726C
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- China
- Prior art keywords
- poly
- polymer emulsion
- compound
- cation
- vinyl
- 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.)
- Expired - Lifetime
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- 239000000839 emulsion Substances 0.000 title claims abstract description 150
- 229920000642 polymer Polymers 0.000 title claims abstract description 103
- 239000000203 mixture Substances 0.000 claims abstract description 71
- 150000001875 compounds Chemical class 0.000 claims abstract description 44
- 239000002253 acid Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 125000000129 anionic group Chemical group 0.000 claims abstract description 11
- -1 cation compound Chemical class 0.000 claims description 78
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 41
- 238000009472 formulation Methods 0.000 claims description 22
- 125000000217 alkyl group Chemical group 0.000 claims description 21
- 230000000813 microbial effect Effects 0.000 claims description 20
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 19
- 150000003839 salts Chemical class 0.000 claims description 17
- 239000008199 coating composition Substances 0.000 claims description 16
- 239000013543 active substance Substances 0.000 claims description 12
- 239000003945 anionic surfactant Substances 0.000 claims description 12
- 238000011109 contamination Methods 0.000 claims description 12
- VAZJLPXFVQHDFB-UHFFFAOYSA-N 1-(diaminomethylidene)-2-hexylguanidine Polymers CCCCCCN=C(N)N=C(N)N VAZJLPXFVQHDFB-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N ethyl acetate Substances CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- JGFDZZLUDWMUQH-UHFFFAOYSA-N Didecyldimethylammonium Chemical compound CCCCCCCCCC[N+](C)(C)CCCCCCCCCC JGFDZZLUDWMUQH-UHFFFAOYSA-N 0.000 claims description 8
- 229960000686 benzalkonium chloride Drugs 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000005660 chlorination reaction Methods 0.000 claims description 8
- 229940078672 didecyldimethylammonium Drugs 0.000 claims description 8
- 150000002148 esters Chemical class 0.000 claims description 8
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical class C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 claims description 6
- 229960001927 cetylpyridinium chloride Drugs 0.000 claims description 6
- 229940123208 Biguanide Drugs 0.000 claims description 5
- 150000003863 ammonium salts Chemical class 0.000 claims description 5
- 150000004283 biguanides Chemical class 0.000 claims description 5
- RBSBTRALZZSVBA-OTUMHNDOSA-N (2s)-4-[(13r)-13-hydroxy-13-[(2r,5r)-5-[(1r)-1-hydroxytridecyl]oxolan-2-yl]tridecyl]-2-methyl-2h-furan-5-one Chemical compound O1[C@@H]([C@H](O)CCCCCCCCCCCC)CC[C@@H]1[C@H](O)CCCCCCCCCCCCC1=C[C@H](C)OC1=O RBSBTRALZZSVBA-OTUMHNDOSA-N 0.000 claims description 4
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 4
- RBSBTRALZZSVBA-FXBHKIKWSA-N Solamin Natural products O=C1C(CCCCCCCCCCCC[C@@H](O)[C@@H]2O[C@H]([C@H](O)CCCCCCCCCCCC)CC2)=C[C@H](C)O1 RBSBTRALZZSVBA-FXBHKIKWSA-N 0.000 claims description 4
- QUMHDXJIDPCZCB-UHFFFAOYSA-N Solamine Natural products CN(C)CCCCNCCCCN(C)C QUMHDXJIDPCZCB-UHFFFAOYSA-N 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 3
- 229940009662 edetate Drugs 0.000 claims 7
- 150000003868 ammonium compounds Chemical class 0.000 claims 2
- 150000001767 cationic compounds Chemical class 0.000 abstract description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract 2
- 239000000470 constituent Substances 0.000 abstract 2
- 239000004094 surface-active agent Substances 0.000 abstract 2
- 244000005700 microbiome Species 0.000 description 26
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 22
- 239000000523 sample Substances 0.000 description 19
- 239000003795 chemical substances by application Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- 239000007788 liquid Substances 0.000 description 14
- 239000001965 potato dextrose agar Substances 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 229920001577 copolymer Polymers 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 230000002421 anti-septic effect Effects 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 230000008719 thickening Effects 0.000 description 9
- 239000012855 volatile organic compound Substances 0.000 description 9
- 229920001817 Agar Polymers 0.000 description 8
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 8
- 239000000654 additive Substances 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 8
- 239000008272 agar Substances 0.000 description 8
- 239000002738 chelating agent Substances 0.000 description 8
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- 239000006916 nutrient agar Substances 0.000 description 7
- 230000002335 preservative effect Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000013530 defoamer Substances 0.000 description 6
- MOYKHGMNXAOIAT-JGWLITMVSA-N isosorbide dinitrate Chemical compound [O-][N+](=O)O[C@H]1CO[C@@H]2[C@H](O[N+](=O)[O-])CO[C@@H]21 MOYKHGMNXAOIAT-JGWLITMVSA-N 0.000 description 6
- 229960000201 isosorbide dinitrate Drugs 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 241000233866 Fungi Species 0.000 description 5
- 239000004902 Softening Agent Substances 0.000 description 5
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 5
- 230000001580 bacterial effect Effects 0.000 description 5
- CYDRXTMLKJDRQH-UHFFFAOYSA-N benzododecinium Chemical class CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 CYDRXTMLKJDRQH-UHFFFAOYSA-N 0.000 description 5
- 125000002091 cationic group Chemical group 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000006101 laboratory sample Substances 0.000 description 5
- 239000002609 medium Substances 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- 241000186145 Corynebacterium ammoniagenes Species 0.000 description 4
- 241000589614 Pseudomonas stutzeri Species 0.000 description 4
- 241000607717 Serratia liquefaciens Species 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000002070 germicidal effect Effects 0.000 description 4
- 238000011534 incubation Methods 0.000 description 4
- 239000004816 latex Substances 0.000 description 4
- 229920000126 latex Polymers 0.000 description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 4
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 230000001954 sterilising effect Effects 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- 239000010455 vermiculite Substances 0.000 description 4
- 229910052902 vermiculite Inorganic materials 0.000 description 4
- 235000019354 vermiculite Nutrition 0.000 description 4
- 239000000080 wetting agent Substances 0.000 description 4
- CTTJWXVQRJUJQW-UHFFFAOYSA-N 2,2-dioctyl-3-sulfobutanedioic acid Chemical compound CCCCCCCCC(C(O)=O)(C(C(O)=O)S(O)(=O)=O)CCCCCCCC CTTJWXVQRJUJQW-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 244000283763 Acetobacter aceti Species 0.000 description 3
- 235000007847 Acetobacter aceti Nutrition 0.000 description 3
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 3
- RUPBZQFQVRMKDG-UHFFFAOYSA-M Didecyldimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC RUPBZQFQVRMKDG-UHFFFAOYSA-M 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 241000032686 Gluconacetobacter liquefaciens Species 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
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- 239000002585 base Substances 0.000 description 3
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- 229950006191 gluconic acid Drugs 0.000 description 3
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
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- 230000004083 survival effect Effects 0.000 description 3
- UUIVKBHZENILKB-UHFFFAOYSA-N 2,2-dibromo-2-cyanoacetamide Chemical compound NC(=O)C(Br)(Br)C#N UUIVKBHZENILKB-UHFFFAOYSA-N 0.000 description 2
- DHVLDKHFGIVEIP-UHFFFAOYSA-N 2-bromo-2-(bromomethyl)pentanedinitrile Chemical compound BrCC(Br)(C#N)CCC#N DHVLDKHFGIVEIP-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
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- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 description 1
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- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/04—Nitrogen directly attached to aliphatic or cycloaliphatic carbon atoms
-
- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- A—HUMAN NECESSITIES
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- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
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- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Landscapes
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- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
本发明涉及一种保护聚合物乳液不受生物腐败性微生物侵蚀和腐败的方法,该方法采用聚合物乳液与经选择的阳离子化合物和乙二胺酸化合物组合。所述的聚合物乳液含有表面活性剂和/或阴离子成分。本发明也涉及抗生物腐败性微生物腐败的聚合物乳液组合物,所述的聚合物乳液组合物包括表面活性剂和/或阴离子成分、乙二胺酸化合物和阳离子化合物。
Description
技术领域
本发明涉及一种保护聚合物乳液不受生物腐败性微生物侵蚀和腐败的抗生物腐败的聚合物乳液。
发明背景
水性聚合物乳液(乳胶)易受微生物污染而导致产品腐败变质。聚合物乳液是微小的有机聚合物粒子在水中的分散体。这些聚合物粒子稳定地悬浮于水相环境中,所述的水相环境中另外加有有机基质,例如表面活性剂和保护胶体。表面活性剂、保护胶体(例如聚(乙烯醇)和羟乙基纤维素)、增稠剂、其它添加剂以及聚合物本身均提供了大量供微生物新陈代谢用的碳营养物。因此,由于微生物的侵袭和繁殖,聚合物乳液易于腐败变质。工业上普遍采用,在生产完成后直接添加各种工业杀虫剂(抗菌剂),来防止这种产品腐败变质。常用的工业杀虫剂的例子是:1,2-苯并异噻唑啉-3-酮(BIT),及5-氯-2-甲基-4-异噻唑啉-3-酮(CIT)与2-甲基-4-异噻唑啉-3-酮(MIT)的混合物。常用于聚合物乳液防腐的其它杀虫剂的例子包括1,2-二溴-2,4-二氰基丁烷(DBDCB)、2,2-二溴-3-次氮基丙酰胺(DBNPA)、2-溴-2-硝基-1,3-丙二醇(BNPD)、醛衍生物、甲醛释放剂、海因和氯化芳族化合物。
这些常用的杀虫剂通常足以保护各种类型的聚合物乳液,以防止大部分由细菌和真菌引起的工业腐败变质。然而,聚合物乳液更易于被某些类型的微生物腐蚀。例如,可在酸性环境中生存和/或代谢醇的生物腐败性微生物(biodeteriogenic microbes),如液化葡糖酸醋酸杆菌(Gluconoacetobacter liquefaciens)(GABL),甚至在常用工业杀虫剂存在下,也在聚合物乳液中生成并茁壮成长。生物腐败性微生物包括对产品和材料的商业价值可产生不利影响的细菌和真菌。一些生物腐败性微生物已变得非常适应子这些乳液环境,以至于在产品的整个保存期(例如6至12个月),常规工业杀虫剂不足以防止产品腐败变质。明显上升的聚合物乳液生物腐败问题已经导致人们有必要确定更有效的防腐剂体系。
已知聚合物乳液中的VOC(挥发性有机化合物),如果不是杀菌作用,则能起到某种程度的抑菌作用,即能抑制生物腐败性微生物的生长。存在于聚合物乳液中的VOC的例子是未反应的单体,例如乙酸乙烯酯、乙酸、甲醇、乙醛和甲醛。应颁布的规章制度和对环境的关注,聚合物乳液技术的最新发展趋向于减少残余的VOC。从微生物学观点看,减少VOC在许多方面影响聚合物乳液。例如:1)它带来了一个更利于微生物生长的乳液环境;2)它可能允许出现新的微生物,这种新微生物更能适应新乳液环境;3)它向当前的防腐剂技术提出另外的挑战;以及4)它导致需要新的防腐方法,在产品的保存期内阻止生物腐败。
虽然存在非常多数量的杀虫剂,它们可有效地杀死微生物,为聚合物乳液和其它工业产品提供良好的防腐作用,但仅有限数量的杀虫剂对高级生物体(例如:人)表现出可接受的低毒性。当聚合物乳液的最终用途要求有美国食品与药物管理局(FDA)的许可证时,可加入到聚合物乳液中的有效杀虫剂的选择变得更加有限。很多聚合物乳液用于制造生活消费品,例如食品包装用的粘合剂和纸、尿布、纸巾、婴儿拭布和妇女卫生用品。由于这种与皮肤的接触和与食物的间接接触,所以在这些应用中所使用的聚合物乳液必须有合适的FDA许可证。这些FDA许可证是基于良好的毒理学分布,包括无皮肤敏化作用。为了使聚合物乳液得到必需的FDA许可证,聚合物乳液的所有组分(包括防腐技术)在聚合物乳液良好性能所要求的浓度下使用时,必须符合FDA严格的毒理学标准。FDA认同的杀虫剂的用量有限制。有时,最小的生物学上有效的浓度大于最大的可允许使用的用量。这通常导致产品过早地被生物污染和生物腐败。另外,微生物不断进化,新的微生物开始出现,它们显现出对一些较普通的工业杀虫剂的抗性,特别是对可允许用量下的普通工业杀虫剂表现出抗性。严格规定的环境、特殊消费品制造说明书、公众的关注和产品责任使杀虫剂的选择和使用更加复杂化。例如,异噻唑啉酮广泛地用作许多消费品的抗菌剂,但已知它们对皮肤致敏,这引起众多的消费品生产厂家的关注。这种对健康的关注和微生物的抗性正引导人们探寻防腐替代品和新的防腐方法。阳离子化合物(如季铵化合物)在抗菌领域中众所周知,并广泛地用作表面消毒剂。例如,它们用于医院、学校、疗养所、饭店和住宅区的地板、墙、工作台面、设备表面、食品接触面等的消毒灭菌。另外,含阳离子化合物的洗涤剂组合物广泛用于单一制品形成对这类表面进行清洁和消毒、杀菌。阳离子化合物也用来抑制水(例如游泳池)中的藻类和微生物的生长。阳离子化合物在有限的范围用于工业产品的防腐,以及用于阻止水溶液体系中微生物的生长。
阳离子化合物在消毒剂组合物和在聚合物乳液防腐剂中应用的实例,讨论如下:
US 6,066,674(Hioki等,2000)教导了一种杀菌-消毒洗涤剂组合物,其由阳离子杀菌剂、金属螯合剂和至少一种表面活性剂组成,所述的表面活性剂选自阴离子、非离子和两性表面活性剂。据报道,在阴离子表面活性剂存在下,必需用金属螯合剂,例如EDTA钠盐、柠檬酸钠和三聚磷酸钠,来保持阳离子物质的杀菌活性。
US 2002/0099113A1(Rabasco等,2002)教导了一种防止微生物侵蚀和腐败胶体稳定的聚合物乳液的方法,它采用经选择的阳离子化合物。这篇文献也涉及包括胶体稳定的聚合物乳液和阳离子化合物的组合物,其中所述的阳离子化合物是防止生物腐败性微生物的污染。该聚合物乳液包含少量或不含非离子或阴离子表面活性剂和包含少量或不含阴离子成分。
US 6,383,505B1(Kaiser等,2002)披露了一种包括水包油乳液的局部使用的抗菌洗液,所述的水包油乳液含有油相中的润肤剂液滴和水相中抗菌剂的分散剂。据报导,是阴离子和非离子表面活性剂的组合物使乳液稳定,并使阳离子抗菌剂基本保持在水相中。
仍需要一种保护聚合物乳液以防产品被微生物生物腐败的方法,特别是对于采用表面活性剂使其稳定和/或含有阴离子成分聚合物乳液以及VOC含量较低的聚合物乳液。
发明简述
本发明涉及一种保护聚合物乳液不受生物腐败性微生物侵蚀和腐败的方法,该方法采用聚合物乳液与经选择的阳离子化合物和乙二胺酸化合物(称为EDA化合物)组合,所述的乙二胺酸化合物结构式如下:
其中R1、R2和R3分别为H、C1~C12的烷基或-(CH2)1-8COOH。EDA化合物也可为上面结构式化合物的一盐、二盐、三盐或四盐。盐的例子为:碱金属盐、碱土金属盐、铵或具有如下结构式的铵衍生盐:
其中R4、R5、R6和R7分别为H或C1~C12的烷基;只要该盐溶于水。优选的化合物是乙二胺四乙酸及其一盐、二盐、三盐和四盐;特别是乙二胺四乙酸的四钠盐。更具体地说,本发明涉及一种保护聚合物乳液不受生物腐败性微生物侵蚀和腐败的方法,该方法采用与上述EDA化合物及其盐组合的经选择的阳离子化合物。所述的聚合物乳液包含表面活性剂和/或阴离子成分。
本发明也涉及抗生物腐败性微生物侵蚀和腐败的聚合物乳液组合物。所述的聚合物乳液组合物包括表面活性剂和/或阴离子成分、EDA化合物和阳离子化合物。
阳离子化合物与EDA化合物结合使用来防止生物腐败性微生物腐蚀聚合物,有效的阳离子化合物的例子是:取代的吡啶盐,例如氯化十六烷吡啶;四烷基取代的铵盐,例如氯化二癸基二甲基铵;苯甲烷铵衍生物,例如C12~C18烷基二甲基杀藻铵、氯化苄乙氧铵、洗必太;多胍(polymeric guanides)和双胍,例如聚(六亚甲基双胍)盐酸盐;及其它聚阳离子化合物,例如聚乙烯吡啶和聚乙烯亚胺。阳离子化合物在与EDA化合物结合使用时,对于VOC含量低(例如低于1000ppmVOC)的聚合物乳液的防腐也特别有效。
EDA化合物与阳离子化合物的组合物作为独立的防腐剂很有效,对细菌和真菌长期表现出广谱杀菌活性,或者也可与其它杀虫剂(例如异噻唑啉酮衍生物)结合使用。
本发明的聚合物乳液组合物可与其它原料混合、按配方配制,用于制备粘合剂、建筑涂料、纸张涂层、无纺布粘合剂等。例如,虽然本发明的聚合物乳液组合物可单纯用作粘合剂,但这种聚合物乳液组合物常常根据具体的最终用途而进行配制。
为了生产抗生物腐败性微生物污染的水性粘合剂或涂料组合物,可能需要加入附加量的阳离子杀虫剂和EDA化合物,以补偿由配方添加物引起的稀释。
发明祥述
本发明的聚合物乳液是合成聚合物和共聚物在水介质中的分散体。用于生产这种聚合物乳液的基本原料是单体、引发剂和稳定剂。单体的例子包括乙酸乙烯酯、乙烯和其它的烯烃、二烯烃(例如丁二烯)、各种丙烯酸烷基酯、各种甲基丙烯酸烷基酯、苯乙烯、氯乙烯、乙烯酯、丙烯酰胺、甲基丙烯酰胺、N-羟甲基丙烯酰胺、顺丁烯二酸和本领域已知的其它单体。用于本发明目的的聚合物乳液的例子包括:聚(乙酸乙烯酯)乳液;聚(乙酸乙烯酯)共聚物乳液,例如聚(乙酸乙烯酯-乙烯)共聚物(VAE)乳液;聚(乙酸乙烯酯-丙烯酸类)乳液,例如聚(乙酸乙烯酯-丙烯酸丁酯)乳液和聚(乙酸乙烯酯-丙烯酸(2-乙基)己酯)乳液;聚丙烯酸类乳液;聚甲基丙烯酸类乳液;聚(苯乙烯-丙烯酸类)乳液;其它聚苯乙烯共聚物乳液;聚(氯乙烯-乙烯)共聚物乳液等;其中所述的丙烯酸类可包括C3~C10的链烯酸及其酯,所述的C3~C10链烯酸如丙烯酸、甲基丙烯酸、巴豆酸和异巴豆酸。这些聚合物乳液可采用本领域已知的各种表面活性剂、保护胶体或本领域已知的其它物质使其稳定,所述的保护胶体如羟乙基纤维素或聚(乙烯醇)。特别适用于本发明的聚合物乳液包含非离子和/或阴离子表面活性剂,和/或包含阴离子成分。
非离子表面活性剂的例子是由Rhone-Poulenc供应的lgepal表面活性剂。lgepal表面活性剂是烷基苯氧基聚(乙烯氧基)乙醇的系列物,含有约7~18个碳原子的烷基,以及约4~100个乙烯氧基单元,例如辛基苯氧基聚(乙烯氧基)乙醇、壬基苯氧基聚(乙烯氧基)乙醇和十二烷基苯氧基聚(乙烯氧基)乙醇。非离子表面活性剂的其它例子包括乙氧基脂肪醇、己糖醇(包括脱水山梨醇、山梨醇、一缩甘露醇和二缩甘露醇)酐的聚氧化烯衍生物、部分长链脂肪酸酯,例如一月桂酸脱水山梨醇酯、一棕榈酸脱水山梨醇酯、一硬脂酸脱水山梨醇酯、三硬脂酸脱水山梨醇酯、一油酸脱水山梨醇酯和三油酸脱水山梨醇酯的聚氧化烯衍生物。
常用的阴离子表面活性剂的例子包括:磺基丁二酸酯;烷基或烷基化芳基硫酸酯;及乙氧化烷基醇或烷基化芳基酚膦酸酯或硫酸酯。
阴离子成分的例子包括丙烯酸、乙烯基磺酸钠、顺丁烯二酸、甲基丙烯酸、巴豆酸、2-丙烯酰氨基-2-甲基丙烷磺酸和本领域已知的其它单体,以及由于采用引发剂(如过硫酸盐)而引入的阴离子聚合物链端。VOC含量低于1000ppm的聚合物乳液也特别适于本发明。存在于聚合物乳液中的VOC是未反应的单体、乙酸、甲醇、乙醛和甲醛。
对本发明的聚合物乳液可进行调配,以用于其它最终用途,例如粘合剂、建筑涂料、纸张涂层和粘结剂(如无纺布粘结剂)。当配制成粘合剂组合物时,聚合物乳液可占整个配方重量的60~90份。在粘合剂组合物配方中常用的添加剂包括增塑剂、消泡剂、增稠剂、分散剂、交联剂、润湿剂、增粘剂、聚乙烯醇和填料。
有代表性的增塑剂包括:二元醇,如二丙二醇;二苯甲酸酯类,如二苯甲酸二丙二醇酯和二苯甲酸二甘醇酯;邻苯二甲酸酯,如邻苯二甲酸二丁酯;液体聚酯,如苯甲酸和邻苯二甲酸的三甘醇聚酯;以及水基粘合剂领域已知的其它增塑剂。增塑剂的用量通常为整个配方重量的2~30份。
有代表性的消泡剂包括硅类或烃类物质。消泡剂的用量通常最多为整个配方重量的1份。
有代表性的增稠剂包括酪蛋白、煅制氧化硅、瓜耳胶、膨润土、oliginates、淀粉、羟乙基纤维素、其它纤维素、聚醚多醇和水基粘合剂领域已知的其它增稠剂。增稠剂的用量通常最多为整个配方重量的5份。
有代表性的交联剂包括:二醛,例如戊二醛;金属,例如锌和锆;蜜胺甲醛树脂、二环氧化物和环氧树脂。交联剂的用量通常最多为整个配方重量的10份。
有代表性的润湿剂包括氯化钙、二元醇、丙三醇、尿素、山梨糖醇和水基粘合剂领域已知的其它润湿剂。润湿剂的加入量通常最多为整个配方重量的20份。
有代表性的增粘剂包括松香、酯胶、烃类树脂、氢化松香、(木浆)浮油松香、萜烯树酯和水基粘合剂领域已知的其它增粘剂。增粘剂通常以分散体的形式使用,其用量最多为粘合剂组合物整个配方重量的35份。
有代表性的填料包括碳酸钙、粘土、云母、硅石、滑石和水基粘合剂领域已知的其它填料。填料的用量通常最多为整个配方重量的40份。
当配制成建筑涂料组合物时,聚合物乳液可以25~75重量份的含量存在。在建筑涂料组合物配方中常用的添加剂包括增塑剂、消泡剂、增稠剂、分散剂、pH控制剂、聚结溶剂、冻-融添加剂、罐装和干膜防腐剂、颜料、填料和阴离子与非离子表面活性剂。
建筑涂料组合物中有代表性的增塑剂包括苯甲酸酯。增塑剂的用量通常为整个配方重量的1~2份。
建筑涂料组合物中有代表性的消泡剂包括矿物油类消泡剂和疏水性硅石(hydrophobic silica)。消泡剂的用量通常为整个配方重量的0.3~0.6份。
建筑涂料组合物中有代表性的增稠剂包括羟乙基纤维素和疏水改性羟乙基纤维素,它们的用量通常为整个配方重量的0.5~1.0份。另外,丙烯酸乙酯/丙烯酸共聚物和疏水改性的氨基甲酸乙酯乙氧化物用作增稠剂,这些增稠剂的用量通常为整个配方重量的1.5~3.0份。
建筑涂料组合物中有代表性的分散剂包括聚(丙烯酸)、聚(甲基丙烯酸)和二异丁烯/马来酐共聚物。分散剂的用量通常为整个配方重量的0.8~1.0份。
建筑涂料组合物中有代表性的pH控制剂包括氨基甲基丙醇和氢氧化铵。pH控制剂的用量通常为整个配方重量的0.2~0.3份。
建筑涂料组合物中有代表性的聚结溶剂包括2,2,4-三甲基异丁酸酯和乙二醇二丁醚。聚结溶剂的用量通常为整个配方重量的1~2份。
建筑涂料组合物中有代表性的冻-融添加剂包括乙二醇和丙二醇。冻-融添加剂的用量通常为整个配方重量的1~4份。
建筑涂料组合物中有代表性的防腐剂包括1,2-苯并异噻唑啉-3-酮、2-氯-2-甲基-4-异噻唑啉-3-酮与2-甲基-4-异噻唑啉-3-酮的混合物、甲醛释放剂、2-辛基-4-异噻唑啉-3-酮和羟基吡啶硫酮锌。防腐剂的最多为整个配方重量的0.2份。
建筑涂料组合物中有代表性的颜料和填料包括二氧化钛、碳酸钙、粘土、云母、硅石、滑石和水基建筑涂料领域中已知的其它颜料和填料。二氧化钛是建筑涂料中最常用的颜料,它的用量通常为整个配方重量的8~25份。
建筑涂料组合物中有代表性的非离子表面活性剂包括烷基酚乙氧化物。非离子表面活性剂的用量通常为整个配方重量的0.3~0.6份。
建筑涂料组合物中采用的有代表性的阴离子表面活性剂包括磺基琥珀酸二辛酯、十二烷基苯磺酸和磷酸酯,以及烷基酚硫酸酯。阴离子表面活性剂的用量通常最多为整个配方重量的0.2份。
微生物污染聚合物乳液,这可导致一系列的影响,包括颜色变化、气味、粘度变化、pH的变化和可见的表面增长。已知在本领域中聚合物乳液易于被各种各样的生物腐败性微生物污染。经查明,污染聚合物乳液的微生物的例子包括:亲水性气单胞菌(Aeromonas hydrophilia)、粪产硷杆菌、产氨棒状杆菌(Corynebacterium ammoniagenes)、产气肠杆菌、大肠杆菌、肺炎杆菌、绿浓杆菌、普通变形杆菌、Providenciarettgeri、假单胞菌stutzeri(Pseudomonas stutzeri)、Shewanella腐败剂(Shewanella putrefaciens)、沙雷氏菌liquefaciens(Serratialiquefaciens)、Acinetobacter baumannii、Burkholderia cepacia、Chryseobacterium meningosepticum、Sphingobacterium spiritivorum、Ralstonia pickettii、液化葡糖酸醋酸杆菌(Gluconoacetobacterliquefaciens)、白地霉、曲霉属类、孢子丝菌类、特德哈氏属、芽枝霉属类、Rhodoturula glutinis、guillermondi念珠菌(Candidaguillermondi)、青霉属类和热带假丝酵母。
本发明已得出,阳离子杀菌剂与EDA化合物组合能有效地保护聚合物乳液以防由各种细菌引起的微生物腐败,所述的聚合物乳液包含阴离子成分,和/或该聚合物乳液是用阴离子和/或非离子表面活性剂乳化的。
适用于本发明聚合物乳液防腐的阳离子化合物包括:取代的吡啶盐,例如氯化十六烷吡啶(CPC),其中所述的取代是烷基、环烷基或2~18个碳原子的芳基取代;四烷基取代的铵盐,例如氯化二癸基二甲基铵,其中所述的烷基分别为1~18个碳原子的烷基;烷基二甲基杀藻铵,其中所述的烷基为1~18个碳原子的烷基;氯化苄乙氧铵;聚(六亚甲基双胍)盐酸盐和其它的双胍;洗必太;聚阳离子化合物,如聚(六亚甲基双胍)盐酸盐等。优选的阳离子衍生物包括四取代的季铵衍生物、双胍、聚双胍和烷基吡啶盐,其中的烷基含2~18个碳原子。在本发明聚合物乳液体系中,当这些阳离子杀菌剂不与EDA化合物结合使用时,它们是无效的防腐剂。
本发明的EDA化合物可采用本领域众所周知的方法来制备。例如:乙二胺、甲醛和氰化钠的反应;乙二胺与氯乙酸的反应。由这种方法制得的化合物与适当的碱反应,来制备EDA化合物的盐。市场上可买得到的EDTA,例如来自Dow Chemical的EDTA,以及来自BAST Corp.的和EDTA。
EDA和阳离子化合物可在聚合物乳液生产过程中的任何时刻与聚合物乳液混合;优选阳离子化合物在后生产过程中作为最后的添加剂加入到聚合物乳液中。EDA化合物和阳离子化合物加入到聚合物乳液中的次序并不重要,优选EDA化合物先加入到聚合物乳液中,然后再加入阳离子化合物。为了防止微生物污染,加入到聚合物乳液中的阳离子化合物的总量或剂量可为10ppm~1wt%,优选50ppm~5000ppm,更优选50ppm~500ppm,以聚合物乳液的湿重计。为了防止微生物污染,加入到聚合物乳液中的EDA化合物的总量或剂量可为10ppm~1wt%,优选50ppm~5000ppm,最优选50ppm~500ppm,以聚合物乳液的湿重计。
本发明的EDA化合物/阳离子化合物组合物可单独使用,或与其它已知的工业杀菌剂一起使用,其它已知的工业杀菌剂例如:BIT;CIT;MIT;DBDCB;DBNPA;DNPD;醛衍生物,如戊二醛和甲醛;甲醛释放剂,如二羟甲基二甲基海因,咪唑烷基脲衍生物,聚甲氧基二环噁唑烷和1-(3-氯烯丙基)-3,5,7-三氮杂-1-氮鎓金刚烷盐酸盐;海因;酚,如邻苯基苯酚钠;及氯化芳族化合物,如对-氯-间-甲酚和氯二甲酚。
参考下面的实施例,对本发明作进一步的阐明,下面的实施例仅作为本发明的示范性例子。
在乙二胺四乙酸(EDTA)辅助剂存在和不存在的情况下,通过向VAE聚合物乳液中加入不同剂量的阳离子化合物,来检验几种阳离子化合物的防腐效果,其中一些聚合物乳液含有低于1000ppm的乙酸乙烯酯单体。然后,所得到的聚合物乳液进行严格的生物抗性实验,实验详情描述如下。
实施例1
采用下面步骤,来评估几种阳离子化合物对VAE共聚物乳液的防腐效果,这种VAE共聚物乳液是用阴离子表面活性剂稳定的,并含有低于1000ppm的乙酸乙烯酯单体。
实验的微生物
亲水性气单胞菌(Aeromonas hydrophilia)、粪产硷杆菌、产氨棒状杆菌(Corynebacterium ammoniagenes)、产气肠杆菌、大肠杆菌、肺炎杆菌、绿浓杆菌、普通变形杆菌、Providencia rettgeri、假单胞菌stutzeri(Pseudomonas stutzeri)、Shewanella腐败剂(Shewanella putrefaciens)、沙雷氏菌liquefaciens(Serratia liquefaciens)、Acinetobacter baumannii、Burkholderia cepacia、Chryseobacterium meningosepticum、Sphingobacterium spiritivorum、Ralstonia pickettii和液化葡糖酸醋酸杆菌(Gluconoacetobacter liquefaciens)。
混合细菌池培菌液的制备
通过在琼脂表面接种,使每种细菌的培养物各自在营养琼脂培养基斜面上生长,除GABL在马铃薯葡萄糖琼脂培养基斜面上生长外。营养琼脂培养基斜面在30℃下培养24~48小时,马铃薯葡萄糖琼脂培养基斜面在25℃下培养48~72小时。经过这段培养期之后,用1/4浓度的林格氏溶液从琼脂表面洗下细菌菌落,收集得到细胞。将所有斜面的上的洗涤物合并到一个无菌的锥形烧瓶中。在实验过程中,调整斜面的数量和用来洗涤细菌菌落的林格氏溶液的量,从而得到最终混合微生物活菌计数为108~1010CFU/mL。
由Microbiology International提供和Don Whitley Scientific,Ltd.制造的快速自动细菌阻抗技术(RABIT),是利用阻抗微生物学原理,来检测和评估给定样品中的微生物活性。应用RABIT,通过测量微生物能动呼吸所产生的二氧化碳的量,来监测微生物代谢。在RABIT实验槽中的电极一部分被含氢氧化钾的碱性琼脂覆盖住。当接种过的实验样品在RABIT上进行监测时,微生物代谢所产生的二氧化碳被碱性琼脂吸收,而导致电导率的变化。电导率随着时间进行监测,并且将电导率达到一个预先指定降低速率所需时间定义为检测时间(TTD)。因此,TTD越短,存在的微生物的数量越高。在RABIT 72小时监测期间的任何时候,当电导率的三次连续降低等于或大于预定的值(厂家推荐为-10微西门子)时,可定义为未通过生物抗性实验。另外,可预先规定一个电导率的总变化,来定义未通过生物抗性实验。
生物抗性实验步骤
含试验抗菌剂的每种试验乳液样品(每种50g)用1.0mL的混合细菌培菌液接种。混合完全后,将该样品放置于30℃的培育箱中。经过1,2和6天的培育后,将每种样品划线平板在营养琼脂和马铃薯葡萄糖琼脂上,来观测继续存活的微生物的量。在观测微生物生长情况之前,营养琼脂平板在30℃下培育48小时,马铃薯葡萄糖琼脂平板在25℃下培养48~72小时。在培育的第7天,每种试验乳液样品再用新制备的混合细菌培菌液进行接种,混合完全后,然后放回培育箱中。自第二次接种再培育1,2和6天后,该样品再一次划线平板在营养琼脂和马铃薯葡萄糖琼脂上。在实验开始后的第14天,试验乳液第三次用另外新制备的混合细菌培菌液进行接种,然后放回培育箱中。自第三次接种再培育1,2,6和13天后,该样品又一次划线平板在营养琼脂和马铃薯葡萄糖琼脂上,来观测继续存活的微生物。当从营养琼脂或马铃薯葡萄糖琼脂划线平板测定法观测到微生物活菌计数>300CFU/10μL时,定义实验未通过生物抗性实验。
采用RABIT的生物抗性实验步骤
将少量的微生物营养物(通常是酵母汁)加入到含试验抗菌剂的每种乳液试验样品(50g)中。所得到的样品然后用1.0mL的混合细菌培菌液接种。混合完全后,每种试验样品取一份(5g)放入各自的RABIT间接电导率管中。然后将间接电导率管放进温度设定为30℃的RABIT培育箱组件中,72小时监测电导率的变化。在RABIT监测期间,剩余的每种试验样品存放在30℃的培育箱中。在RABIT监测完成时,那份样品放回它们各自的样品容器中。然后,每种试验样品用新制备的混合细菌培菌液再接种。混合完全后,如上所述,每种试验样品取一份(5g)又放入新的RABIT间接电导率管中,在RABIT上进行监测。每三到四天重复一次接种和RABIT电导率监测步骤,直到样品不合格或经过几次接种后样品没有不合格。
表1表明,在加入和不加入EDTA盐(乙二胺四乙酸的四钠盐)或其它金属螯合剂的情况下,各种类型的阳离子化合物的防腐效力,即控制和抑制细菌在192 VAE共聚物乳液中的生长,该共聚物乳液Tg为~10℃,用阴离子表面活性剂使其稳定,并含有低于1000ppm的乙酸乙烯酯单体。由数据清楚地表明,取决于EDTA的存在,这种聚合物乳液环境中的防腐效力存在显著的不同。例如,对于300ppm剂量的氯化二癸基二甲基铵,由于在用混合细菌培菌液第一次接种后,马上就未通过生物抗性实验,所以其不具有防腐效力。类似剂量的聚(六亚呷基双胍)盐酸盐、CPC(在众多的漱口药中发现的活性抗菌剂)和苯甲烷铵(benzalkonium)衍生物正好无效。单独的EDTA和其它金属螯合剂也不适用。然而,当这些相同的阳离子化合物与EDTA组合使用时,意外地取得防腐效果,这些杀菌组合物极好地保护聚合物乳液免遭由细菌污染所引起的腐败。基于已有技术教导的,即其它金属螯合剂(如柠檬酸和马来酸)与EDTA作用一样,则这些结果是意想不到的;然而,它们没有表现出像本发明的阳离子化合物那样的作用。
表1
在AIRFLEX 192 VAE聚合物中混合细菌的生物抗性实验结果
*活性成分
BTC 1010和824由Stepan Co.提供;Vantocil IB由Avecia Biocides提供;
EDTA盐=EDTA的四钠盐;DGH=正-十二烷基盐酸胍
实施例2
生物抗性实验步骤按照实施例1所述的进行。表2表明,在加入和不加入EDTA盐(乙二胺四乙酸,四钠盐)或其它金属螯合剂的情况下,各种类型的阳离子化合物的防腐效力,即控制和抑制细菌在AIRFLEX 410VAE共聚物乳液中的生长,该共聚物乳液Tg为~4℃,用非离子表面活性剂使其稳定,并含有低于1000ppm的乙酸乙烯酯单体。由数据清楚地表明,取决于有或没有EDTA盐,这种聚合物乳液环境中的防腐效力显著不同。例如,对于300ppm剂量的氯化二癸基二甲基铵,由于在用混合细菌培菌液第一次接种后,马上就未通过生物抗性实验,所以其不具有防腐效力。类似剂量的聚(六亚甲基双胍)盐酸盐、CPC(在众多的漱口药中发现的活性抗菌剂)和苯甲烷铵(benzalkonium)衍生物正好无效。单独的EDTA盐和其它金属螯合剂也不适用。然而,当这些相同的阳离子化合物与EDTA盐组合使用时,意外地取得防腐效果,这些杀菌组合物极好地保护聚合物乳液免遭由细菌污染所引起的腐败。由于与已有技术教导的相反,所以这些结果意想不到,其它金属螯合剂(如柠檬酸和马来酸)没有表现出像本发明聚合物乳液中的阳离子化合物那样的作用。
表2
在AIRFLEX 410 VAE聚合物中混合细菌的生物抗性实验结果
*活性成分
EDTA盐=EDTA的四钠盐;DGH=正-十二烷基盐酸胍
实施例3
在加入和不加入EDTA盐的情况下,根据以下步骤来测定几种阳离子化合物的防腐效力,即控制和抑制霉菌和酵母在VAE共聚物乳液中的生长,该共聚物乳液用非离子表面活性剂使其稳定,并含有低于1000ppm的乙酸乙烯酯。
酵母:
Rhodoturula glutinis、guillermondi念珠菌(Candida guillermondi)和热带假丝酵母。
霉菌:白地霉、曲霉属类、孢子丝菌类、特德哈氏属、芽枝霉属类
混合酵母培菌液的制备
通过在琼脂表面接种,使每种酵母的培养物各自在马铃薯葡萄糖琼脂平板上生长。然后马铃薯葡萄糖琼脂平板在25℃下培养3~7天。经过这段培养期之后,用1/4浓度的格氏溶液从琼脂表面洗下菌落,收集得到酵母细胞。将洗涤物合并到一个无菌的锥形烧瓶中。在实验过程中,调整所用平板的数量和用来洗涤细胞的格氏溶液的量,从而最后得到最终微生物的计数为106~107CFU/mL。
混合霉菌培菌液的制备
通过在琼脂表面接种,使每种霉菌的培养物各自在马铃薯葡萄糖琼脂平板上生长。然后马铃薯葡萄糖琼脂平板在25℃下培养3~7天。经过这段培养期之后,用0.005%磺基琥珀酸二辛酯水溶液从琼脂表面洗下菌落,收集得到霉菌细胞。洗涤物通过无菌粗棉布过滤,将滤液合并到一个无菌的锥形烧瓶中。在实验过程中,调整所用平板的数量和用来洗涤细胞的0.005%磺基琥珀酸二辛酯的量,从而得到最终微生物的计数为106~107CFU/mL。
真菌生物抗性实验步骤
每种含试验抗菌剂的聚合物乳液试验样品(50g)用0.5mL的混合酵母培菌液接种。混合完全后,然后将敞开着的样品容器放入较大的第二个容器中,第二个容器含有20g无菌蛭石和80g无菌水。然后每种实验样品用0.5mL的混合霉菌培菌液接种,小心地将霉菌培菌液分布在乳液实验样品的整个表面上。样品不再进一步混合。为了使实验样品表面受到的干扰最小,将盖子盖在较大的蛭石容器上,使较小的乳液实验样品容器敞开着口在蛭石容器中。然后该样品在25℃下培育28天。经过28天的培育期后,揭去蛭石容器的盖子,不要扰动实验样品的表面,肉眼观测表面上存在的所有真菌的生长。在将这些观测情况记录为无生长、少量生长、中度生长、大量生长或密集生长之后,将该样品彻底混合,每种样品划线平板在马铃薯葡萄糖琼脂(PDA)上,来观测继续存活的微生物的量。在观测微生物生长情况之前,马铃薯葡萄糖琼脂平板在25℃下培养3~5天。
表3列出,在加入和不加入EDTA盐的情况下,一些具体的阳离子化合物在Airflex 410VAE聚合乳液中抗击酵母和霉菌的防腐效力的数据。单独的阳离子化合物和单独的EDTA盐均不能防止酵母和霉菌的生长。然而,当EDTA盐与Vantocil IB或BTC 1010阳离子剂组合使用时,酵母和霉菌的生长意外地被抑制住,并且乳液样品针对这些微生物而适当防腐。
表3
杀菌剂 | 表面真菌的生长 | 在PDA上的生长 |
空白(无杀菌剂) | 密集生长 | 密集 |
200ppm EDTA盐 | 少量生长 | 密集 |
200ppm Vantocil IB | 少量生长 | 密集 |
200ppmBTC 1010 | 中度生长 | 密集 |
100ppm Vantocil IB/100ppm EDTA盐 | 少量生长 | 无生长 |
300ppm BTC 1010/200ppm EDTA盐 | 少量生长 | 无生长 |
200ppm BTC 1010/200ppm EDTA盐 | 少量生长 | 密集 |
EDTA盐=EDTA的四钠盐
Claims (23)
1.一种抗生物腐败性微生物污染的水性聚合物乳液组合物,其包括与阳离子化合物和乙二胺酸化合物组合的水性聚合物乳液,所述的乙二胺酸化合物结构式如下:
其中R1、R2和R3分别为H、C1~C12烷基、-(CH2)1-8COOH;或具有上述结构式的乙二胺酸化合物的一盐、二盐、三盐或四盐;其中所述的阳离子化合物选自取代的吡啶盐、四烷基取代的铵盐、双胍、聚阳离子化合物、其中烷基为1~18个碳原子烷基的烷基二甲基杀藻铵及其混合物;其中所述的取代的吡啶盐是烷基、环烷基或2~18个碳原子的芳基取代的,四烷基取代的铵化合物上的每个烷基分别含1~18个碳原子;所述的聚合物乳液含有一种或多种表面活性剂和/或阴离子成分,
其中所述的乙二胺酸化合物和阳离子化合物各自以10ppm~1wt%的含量存在,以聚合物乳液的湿重计。
2.根据权利要求1所述的聚合物乳液组合物,其中所述的聚阳离子化合物是聚双胍。
3.根据权利要求1所述的聚合物乳液组合物,其中所述的乙二胺酸化合物是乙二胺四乙酸盐。
4.根据权利要求1所述的聚合物乳液组合物,该聚合物乳液组合物包含阴离子表面活性剂、非离子表面活性剂或阴离子表面活性剂和非离子表面活性剂两者。
5.根据权利要求1所述的聚合物乳液组合物,其中所述的阳离子化合物选自聚(六亚甲基双胍)盐酸盐、氯化二癸基二甲基铵、氯化十六烷吡啶、洗必太、氯化苄乙氧铵、C12~C18烷基二甲基杀藻铵混合物及这些阳离子化合物的混合物;所述的乙二胺酸化合物是乙二胺四乙酸盐。
6.根据权利要求1所述的聚合物乳液组合物,其中所述的聚合物乳液是选自聚(乙酸乙烯酯-乙烯)共聚物、聚(乙酸乙烯酯)、聚(乙酸乙烯酯-丙烯酸丁酯)、聚(乙酸乙烯酯-丙烯酸(2-乙基)己酯)、聚丙烯酸类、聚甲基丙烯酸类、聚(苯乙烯-丙烯酸类)和聚(氯乙烯-乙烯)共聚物的聚合物乳液。
7.根据权利要求1所述的聚合物乳液组合物,其中所述的聚合物乳液是聚(乙酸乙烯酯-乙烯)共聚物或聚(乙酸乙烯酯)的聚合物乳液。
8.根据权利要求1所述的聚合物乳液组合物,其中所述的乙二胺酸化合物和阳离子化合物各自以50ppm~5000ppm的含量存在,以聚合物乳液的湿重计。
9.根据权利要求1所述的聚合物乳液组合物,其中所述的乙二胺酸化合物和阳离子化合物各自以50ppm~500ppm的含量存在,以聚合物乳液的湿重计。
10.一种抗生物腐败性微生物污染的水性聚合物乳液组合物,其包括与阳离子化合物和乙二胺四乙酸盐组合的水性聚合物乳液,所述的阳离子化合物选自聚(六亚甲基双胍)盐酸盐、氯化二癸基二甲基铵、氯化十六烷吡啶、洗必太、C12~C18烷基二甲基杀藻铵混合物及这些阳离子化合物的混合物,其中所述的乙二胺四乙酸盐和阳离子化合物各自以10ppm~1wt%的含量存在,以聚合物乳液的湿重计。
11.一种防止生物腐败性微生物污染聚合物乳液的方法,该方法包括:
使水性聚合物乳液与有效量的乙二胺酸化合物和阳离子化合物组合;其中所述的乙二胺酸化合物结构式如下:
其中R1、R2和R3分别为H、C1~C12烷基、-(CH2)1-8COOH;或具有上述结构式的乙二胺酸化合物的一盐、二盐、三盐或四盐;所述阳离子化合物选自取代的吡啶盐、四烷基取代的铵盐、多胍、聚阳离子化合物、其中烷基为1~18个碳原子烷基的烷基二甲基杀藻铵及其混合物;其中所述的取代的吡啶盐是烷基、环烷基或2~18个碳原子的芳基取代的,四烷基取代的铵化合物上的每个烷基分别含1~18个碳原子;所述的聚合物乳液含有一种或多种表面活性剂和/或阴离子成分,
其中所述的乙二胺酸化合物和阳离子化合物各自以10ppm~1wt%的含量存在,以聚合物乳液的湿重计。
12.根据权利要求11所述的方法,其中所述的聚阳离子化合物是聚双胍。
13.根据权利要求11所述的方法,其中所述的聚合物乳液组合物包含阴离子表面活性剂、非离子表面活性剂或阴离子表面活性剂和非离子表面活性剂两者。
14.根据权利要求11所述的方法,其中所述的阳离子化合物选自聚(六亚甲基双胍)盐酸盐、氯化二癸基二甲基铵、氯化十六烷吡啶、洗必太、氯化苄乙氧铵、C12~C18烷基二甲基杀藻铵混合物及这些阳离子化合物的混合物;所述的乙二胺酸化合物是乙二胺四乙酸盐。
15.根据权利要求11所述的方法,其中所述的聚合物乳液是选自聚(乙酸乙烯酯-乙烯)共聚物、聚(乙酸乙烯酯)、聚(乙酸乙烯酯-丙烯酸丁酯)、聚(乙酸乙烯酯-丙烯酸(2-乙基)己酯)、聚丙烯酸类、聚甲基丙烯酸类、聚(苯乙烯-丙烯酸类)和聚(氯乙烯-乙烯)共聚物的聚合物乳液。
16.根据权利要求11所述的方法,其中所述的聚合物乳液是聚(乙酸乙烯酯-乙烯)共聚物或聚(乙酸乙烯酯)的聚合物乳液。
17.根据权利要求11所述的方法,其中所述的乙二胺酸化合物和阳离子化合物的用量各自为50ppm~5000ppm,以聚合物乳液的湿重计。
18.根据权利要求11所述的方法,其中所述的乙二胺酸化合物和阳离子化合物的用量各自为50ppm~500ppm,以聚合物乳液的湿重计。
19.一种防止生物腐败性微生物污染聚合物乳液的方法,该方法包括:
使聚合物乳液与有效量的阳离子化合物和乙二胺四乙酸盐组合;所述的阳离子化合物选自聚(六亚甲基双胍)盐酸盐、氯化二癸基二甲基铵、氯化十六烷吡啶、洗必太、C12~C18烷基二甲基杀藻铵混合物及这些阳离子化合物的混合物,其中所述的乙二胺四乙酸盐和阳离子化合物各自以10ppm~1wt%的含量存在,以聚合物乳液的湿重计。
20.一种包括权利要求1所述的聚合物乳液组合物的粘合剂制剂。
21.一种包括权利要求1所述的聚合物乳液组合物的涂料制剂。
22.一种包括权利要求10所述的聚合物乳液组合物的粘合剂制剂。
23.一种包括权利要求10所述的聚合物乳液组合物的涂料制剂。
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MY136592A (en) | 2008-10-31 |
KR100626190B1 (ko) | 2006-09-20 |
TW200425835A (en) | 2004-12-01 |
CN1550520A (zh) | 2004-12-01 |
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US20040235982A1 (en) | 2004-11-25 |
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