CN101547736B - 微胶囊 - Google Patents
微胶囊 Download PDFInfo
- Publication number
- CN101547736B CN101547736B CN2007800448181A CN200780044818A CN101547736B CN 101547736 B CN101547736 B CN 101547736B CN 2007800448181 A CN2007800448181 A CN 2007800448181A CN 200780044818 A CN200780044818 A CN 200780044818A CN 101547736 B CN101547736 B CN 101547736B
- Authority
- CN
- China
- Prior art keywords
- monomer
- microcapsules
- weight
- acid
- 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 - Fee Related
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 101
- 239000000178 monomer Substances 0.000 claims abstract description 149
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 48
- 239000002775 capsule Substances 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 43
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 37
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 31
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims abstract description 18
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 14
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 13
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims abstract description 13
- 239000011976 maleic acid Substances 0.000 claims abstract description 13
- 229920000867 polyelectrolyte Polymers 0.000 claims description 57
- -1 monomer I Chemical compound 0.000 claims description 40
- 239000006185 dispersion Substances 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 29
- 230000007062 hydrolysis Effects 0.000 claims description 26
- 238000006460 hydrolysis reaction Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 22
- 239000000839 emulsion Substances 0.000 claims description 21
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 20
- 239000000126 substance Substances 0.000 claims description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 14
- 239000011118 polyvinyl acetate Substances 0.000 claims description 14
- 239000003999 initiator Substances 0.000 claims description 12
- 239000004744 fabric Substances 0.000 claims description 11
- 239000004035 construction material Substances 0.000 claims description 8
- GZBSIABKXVPBFY-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OCC(CO)(CO)CO GZBSIABKXVPBFY-UHFFFAOYSA-N 0.000 claims description 7
- 239000013529 heat transfer fluid Substances 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010526 radical polymerization reaction Methods 0.000 claims description 6
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 5
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 5
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims description 5
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 5
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 5
- 150000005846 sugar alcohols Polymers 0.000 claims description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 4
- TYMYJUHDFROXOO-UHFFFAOYSA-N 1,3-bis(prop-2-enoxy)-2,2-bis(prop-2-enoxymethyl)propane Chemical compound C=CCOCC(COCC=C)(COCC=C)COCC=C TYMYJUHDFROXOO-UHFFFAOYSA-N 0.000 claims description 4
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical group C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- 230000009466 transformation Effects 0.000 claims description 4
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 3
- SJIXRGNQPBQWMK-UHFFFAOYSA-N 2-(diethylamino)ethyl 2-methylprop-2-enoate Chemical compound CCN(CC)CCOC(=O)C(C)=C SJIXRGNQPBQWMK-UHFFFAOYSA-N 0.000 claims description 3
- QENRKQYUEGJNNZ-UHFFFAOYSA-N 2-methyl-1-(prop-2-enoylamino)propane-1-sulfonic acid Chemical compound CC(C)C(S(O)(=O)=O)NC(=O)C=C QENRKQYUEGJNNZ-UHFFFAOYSA-N 0.000 claims description 3
- ATVJXMYDOSMEPO-UHFFFAOYSA-N 3-prop-2-enoxyprop-1-ene Chemical compound C=CCOCC=C ATVJXMYDOSMEPO-UHFFFAOYSA-N 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 3
- 229960000834 vinyl ether Drugs 0.000 claims description 3
- ZWUBFMWIQJSEQS-UHFFFAOYSA-N 1,1-bis(ethenyl)cyclohexane Chemical compound C=CC1(C=C)CCCCC1 ZWUBFMWIQJSEQS-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 claims description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 claims description 2
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 2
- 150000005690 diesters Chemical class 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- DNTMQTKDNSEIFO-UHFFFAOYSA-N n-(hydroxymethyl)-2-methylprop-2-enamide Chemical compound CC(=C)C(=O)NCO DNTMQTKDNSEIFO-UHFFFAOYSA-N 0.000 claims description 2
- LFGUHOLEYXHXKZ-UHFFFAOYSA-N Acetylsyringasaeure-methylester Natural products COC(=O)C1=CC(OC)=C(OC(C)=O)C(OC)=C1 LFGUHOLEYXHXKZ-UHFFFAOYSA-N 0.000 claims 1
- NVLPQIPTCCLBEU-UHFFFAOYSA-N allyl methyl sulphide Natural products CSCC=C NVLPQIPTCCLBEU-UHFFFAOYSA-N 0.000 claims 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- 125000006686 (C1-C24) alkyl group Chemical group 0.000 abstract 1
- 239000004566 building material Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 43
- 239000000084 colloidal system Substances 0.000 description 27
- 229920001577 copolymer Polymers 0.000 description 27
- 125000002091 cationic group Chemical group 0.000 description 25
- 238000006116 polymerization reaction Methods 0.000 description 24
- 239000000463 material Substances 0.000 description 22
- 229910052500 inorganic mineral Inorganic materials 0.000 description 16
- 239000011707 mineral Substances 0.000 description 16
- 235000010755 mineral Nutrition 0.000 description 16
- 239000002253 acid Substances 0.000 description 15
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 description 14
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 12
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 12
- 238000005338 heat storage Methods 0.000 description 12
- 229920001519 homopolymer Polymers 0.000 description 12
- 239000004568 cement Substances 0.000 description 11
- 150000003254 radicals Chemical class 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000000835 fiber Substances 0.000 description 10
- 239000003921 oil Substances 0.000 description 10
- 239000001993 wax Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- 239000003431 cross linking reagent Substances 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 125000000129 anionic group Chemical group 0.000 description 8
- 229920001448 anionic polyelectrolyte Polymers 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000011232 storage material Substances 0.000 description 8
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 description 7
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 7
- 229920006317 cationic polymer Polymers 0.000 description 7
- 239000006260 foam Substances 0.000 description 7
- 239000010440 gypsum Substances 0.000 description 7
- 229910052602 gypsum Inorganic materials 0.000 description 7
- RCLLINSDAJVOHP-UHFFFAOYSA-N n-ethyl-n',n'-dimethylprop-2-enehydrazide Chemical compound CCN(N(C)C)C(=O)C=C RCLLINSDAJVOHP-UHFFFAOYSA-N 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 229940044654 phenolsulfonic acid Drugs 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- XFPJDCPUXZTBML-UHFFFAOYSA-N 2-ethenyl-1h-imidazole;methyl hydrogen sulfate Chemical compound COS(O)(=O)=O.C=CC1=NC=CN1 XFPJDCPUXZTBML-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 6
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 6
- 150000007522 mineralic acids Chemical class 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 6
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical group C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 5
- 229920002125 Sokalan® Polymers 0.000 description 5
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 5
- 229940073608 benzyl chloride Drugs 0.000 description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000007859 condensation product Substances 0.000 description 5
- 229960003750 ethyl chloride Drugs 0.000 description 5
- 150000002978 peroxides Chemical class 0.000 description 5
- IUGYQRQAERSCNH-UHFFFAOYSA-N pivalic acid Chemical compound CC(C)(C)C(O)=O IUGYQRQAERSCNH-UHFFFAOYSA-N 0.000 description 5
- 239000004584 polyacrylic acid Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229920000877 Melamine resin Polymers 0.000 description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 4
- 229920000831 ionic polymer Polymers 0.000 description 4
- ZQXSMRAEXCEDJD-UHFFFAOYSA-N n-ethenylformamide Chemical compound C=CNC=O ZQXSMRAEXCEDJD-UHFFFAOYSA-N 0.000 description 4
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 4
- PKJBRKTYYNRVSN-UHFFFAOYSA-N 10-(aminomethyl)-9,10-dihydroanthracene-1,2-diol Chemical compound OC1=CC=C2C(CN)C3=CC=CC=C3CC2=C1O PKJBRKTYYNRVSN-UHFFFAOYSA-N 0.000 description 3
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 description 3
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 150000000996 L-ascorbic acids Chemical class 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 239000011398 Portland cement Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000001246 colloidal dispersion Methods 0.000 description 3
- HOWGUJZVBDQJKV-UHFFFAOYSA-N docosane Chemical compound CCCCCCCCCCCCCCCCCCCCCC HOWGUJZVBDQJKV-UHFFFAOYSA-N 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- YCOZIPAWZNQLMR-UHFFFAOYSA-N heptane - octane Natural products CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 235000010288 sodium nitrite Nutrition 0.000 description 3
- CLWAXFZCVYJLLM-UHFFFAOYSA-N 1-chlorohexadecane Chemical compound CCCCCCCCCCCCCCCCCl CLWAXFZCVYJLLM-UHFFFAOYSA-N 0.000 description 2
- GDBCGGFNFKMPAE-UHFFFAOYSA-N 1-decylnaphthalene Chemical compound C1=CC=C2C(CCCCCCCCCC)=CC=CC2=C1 GDBCGGFNFKMPAE-UHFFFAOYSA-N 0.000 description 2
- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 2
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明涉及包含胶囊核和胶囊壁的微胶囊,其中基于单体总重量,胶囊壁由如下单体构成:30-90重量%的至少一种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸(单体I),10-70重量%二乙烯基和多乙烯基单体的混合物(单体II),其中多乙烯基单体的比例基于单体II为2-90重量%,以及0-30重量%至少一种其它单体(单体III)。本发明还涉及一种制备所述微胶囊方法以及它们在织物、粘合建筑材料和传热流体中的用途。
Description
本发明涉及包含胶囊核和胶囊壁的微胶囊,其中胶囊壁由丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸,交联剂以及合适的话其它单体构成。本发明还涉及一种制备它们的方法以及它们在织物、粘合建筑材料和传热流体中的用途。
近年来,已经研究了作为新型材料组合的具有潜热储存介质的织物。也已知为相变材料(PCM)的潜热储存介质的作用方式基于在固/液相变过程中引起转化焓,这意味着吸收能量或将能量释放至环境中。因此,它们可用于将温度在固定的温度范围内保持恒定。
EP-A 1 029 018教导了具有高度交联的甲基丙烯酸酯聚合物的胶囊壁和潜热储存核的微胶囊在粘合建筑材料如混凝土或石膏中的用途。DE-A-101 39 171描述了微胶囊化的潜热储存材料在石膏板中的用途。此外,WO 2005/116559教导了微胶囊化的潜热储存材料在粗纸板中与三聚氰胺甲醛树脂一起作为粘合剂的用途。
EP-A 1 321 182教导了具有高度交联的甲基丙烯酸酯聚合物的胶囊壁的微胶囊化的潜热储存材料以及提及了它们在织物中的用途。该参考文献教导了具有特别低的粒度为≤4μm的胶囊比例的微胶囊分散体。
EP-A 1 251 954和WO 2005/105291教导了基于聚甲基丙烯酸并且具有或不具有作为交联剂的丁二醇二丙烯酸酯的微胶囊。将粒度为1.2μm的胶囊用于浸渍纤维。
在织物领域用作整理剂的重要标准为对干洗的耐久性,即对氯化或全氯化溶剂的耐受性。在常规微胶囊的情况下经常存在重量损失,这表明不够紧密或有缺陷的胶囊。这种冲洗损失可在5-15重量%的范围内。
两个在先欧洲申请No.06117092.4和No.06122419.2提出了用聚电解质额外改性表面的微胶囊以解决该问题。
除了低的冲洗损失外,低的蒸发率也是对胶囊的重要要求,因为通常在高温下加工胶囊。同时,织物应用要求蒸发率性能能够应对施加的较短的热负荷,长期的良好牢度是在建筑领域应用的要求。
本发明的目的是提供对于宽范围的胶囊尺寸分布具有低蒸发率的微胶囊。
我们发现该目的通过包含胶囊核和胶囊壁的微胶囊实现,其中基于单体总重量,胶囊壁由如下单体构成:
30-90重量%的一种或多种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸(单体I),
10-70重量%二乙烯基和多乙烯基单体的混合物(单体II),其中多乙烯基单体的比例基于单体II为2-90重量%,以及
0-30重量%一种或多种其它单体(单体III),
一种制备它们的方法以及它们在织物、粘合建筑材料和传热流体中的用途。
本发明微胶囊包含胶囊核和胶囊壁。胶囊核主要(超过95重量%)由亲油物质组成。胶囊的平均粒度(Z均,通过光散射)为0.5-100μm,优选1-80μm,特别是1-50μm。
在一个优选实施方案中,胶囊的平均粒度为1.5-2.5μm,优选1.7-2.4μm。并且90%的颗粒的粒度(直径)≤4μm,优选≤3.5μm,特别是≤3μm。微胶囊分散体的最大值一半处的全宽优选为0.2-1.5μm,特别是0.4-1μm。
在同样优选的实施方案中,胶囊的平均粒度为>2.5-20μm,优选3.0-15μm。
胶囊核与胶囊壁的重量比通常为50∶50-95∶5。优选核/壁比为70∶30-93∶7。
胶囊壁的聚合物通常以共聚形式包含基于单体总重量为至少30重量%,优选至少35重量%,更优选至少40重量%以及通常不超过90重量%,优选不超过80重量%,更优选不超过75重量%的丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸(单体I)。
根据本发明,胶囊壁的聚合物通常以共聚形式包含基于单体总重量为至少10重量%,优选至少15重量%,更优选至少20重量%且通常不超过70重量%,优选不超过60重量%,更优选不超过50重量%的二乙烯基和多乙烯基单体的混合物(单体II一起)。可将一种或多种二乙烯基单体以及一种或多种多乙烯基单体共聚。
单体II包含二乙烯基和多乙烯基单体的混合物,其中多乙烯基单体的比例基于二乙烯基单体和多乙烯基单体的总和为2-90重量%。多乙烯基单体的比例基于二乙烯基单体和多乙烯基单体的总和优选为5-80重量%,更优选10-60重量%。对于平均粒度为<2.5μm的微胶囊,多乙烯基单体的比例基于二乙烯基单体和多乙烯基单体的总和优选为20-80重量%,特别是30-60重量%。对于平均粒度为≥2.5μm的微胶囊,多乙烯基单体的比例基于二乙烯基单体和多乙烯基单体的总和优选为5-40重量%,特别是10-30重量%。
此外,聚合物可以共聚形式包含基于单体的总重量为至多30重量%,优选至多20重量%,特别是至多10重量%,更优选至多5重量%且至少1重量%其它单体III,优选单体IIIa。
优选胶囊壁仅由组I和II的单体构成。
合适的单体I包括丙烯酸和/或甲基丙烯酸的C1-C24烷基酯(单体Ia)。它们进一步包括不饱和C3和C4羧酸如丙烯酸、甲基丙烯酸以及马来酸(单体Ib)。特别优选单体I为丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯和丙烯酸正丁酯和/或对应的甲基丙烯酸酯。优选丙烯酸异丙酯、丙烯酸异丁酯、丙烯酸仲丁酯和丙烯酸叔丁酯和对应的甲基丙烯酸酯。通常优选甲基丙烯酸酯和甲基丙烯酸。
在一个优选实施方案中,微胶囊壁由25-75重量%马来酸和/或丙烯酸,特别是甲基丙烯酸构成。
合适的二乙烯基单体包括二乙烯基苯、三乙烯基苯和二乙烯基环己烷和三乙烯基环己烷。优选二乙烯基单体为二醇与丙烯酸或甲基丙烯酸的二酯以及这些二醇的二烯丙基和二乙烯基醚。例如可提及乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、甲代烯丙基甲基丙烯酰胺、丙烯酸烯丙酯和甲基丙烯酸烯丙酯。特别优选丙二醇二丙烯酸酯、丁二醇二丙烯酸酯、戊二醇二丙烯酸酯和己二醇二丙烯酸酯和对应的甲基丙烯酸酯。
优选多乙烯基单体为多元醇与丙烯酸和/或甲基丙烯酸的聚酯以及这些多元醇的多烯丙基和多乙烯基醚。优选三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、季戊四醇三丙烯酸酯和季戊四醇四丙烯酸酯以及它们的工业级混合物。
优选丁二醇二丙烯酸酯和季戊四醇四丙烯酸酯、己二醇二丙烯酸酯和季戊四醇四丙烯酸酯、丁二醇二丙烯酸酯和三羟甲基丙烷三丙烯酸酯以及己二醇二丙烯酸酯和三羟甲基丙烷三丙烯酸酯的组合。
单体III为不同于单体I和II的其它单体,如乙酸乙烯酯、丙酸乙烯酯、乙烯基吡啶和苯乙烯或α-甲基苯乙烯。特别优选具有带电荷或可离子化基团且不同于单体I和II的单体III,如衣康酸、马来酸酐、丙烯酸2-羟基乙酯、甲基丙烯酸2-羟基乙酯、丙烯酰胺基-2-甲基丙烷磺酸、甲基丙烯腈、丙烯腈、甲基丙烯酰胺、N-乙烯基吡咯烷酮、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、甲基丙烯酸二甲基氨基乙酯和甲基丙烯酸二乙基氨基乙酯。
基于单体总重量,胶囊壁优选由如下单体构成:
30-90重量%单体Ia和Ib的混合物,其中单体Ib的比例基于所有单体I、II和III的总重量为<25重量%,
10-70重量%二乙烯基和多乙烯基单体(单体II)的混合物,其中多乙烯基单体的比例低于单体II为2-90重量%,以及
0-30重量%其它单体III。
在另一优选实施方案中,基于单体总重量,胶囊壁由如下单体构成:
30-90重量%单体Ia和Ib的混合物,其中单体Ib的比例基于所有单体I、II和III的总重量为≥25重量%,
10-70重量%二乙烯基和多乙烯基单体(单体II)的混合物,其中多乙烯基单体的比例低于单体II为2-90重量%,以及
0-30重量%其它单体III。
本发明微胶囊可经由所谓的原位聚合得到。微胶囊的形成原理基于由单体、自由基引发剂、保护胶体和待胶囊化的亲油物质制备稳定的水包油乳液。然后,通过加热引发单体聚合,合适的话通过进一步升温来控制,所得聚合物形成围绕亲油性物质的胶囊壁。该一般原理例如描述于DE-A-10 139 171中,此处完全引入其内容作为参考。
微胶囊通常在至少一种有机或无机保护胶体存在下制备。所述有机或无机保护胶体可为离子型或中性。保护胶体不仅可单独使用,而且可以多种带相同或不同电荷的保护胶体的混合物使用。
优选有机保护胶体为水溶性聚合物,这些保护胶体使水的表面张力从73mN/m的最大值降低到45-70mN/m,因此确保了密封胶囊壁的形成,并且形成具有0.5-50μm,优选0.5-30μm,特别是0.5-10μm的优选粒度的微胶囊。
有机中性保护胶体例如包括纤维素衍生物如羟乙基纤维素、甲基羟乙基纤维素、甲基纤维素和羧甲基纤维素,聚乙烯基吡咯烷酮,乙烯基吡咯烷酮的共聚物,明胶,阿拉伯树胶,黄原胶,酪蛋白,聚乙二醇、聚乙烯醇和部分水解的聚乙酸乙烯酯以及甲基羟丙基纤维素。优选有机中性保护胶体为聚乙烯醇和部分水解的聚乙酸乙烯酯以及甲基羟丙基纤维素。
有机阴离子保护胶体包括海藻酸钠、聚甲基丙烯酸及其共聚物、磺乙基丙烯酸酯、磺乙基甲基丙烯酸酯、磺丙基丙烯酸酯、磺丙基甲基丙烯酸酯、N-(磺基乙基)马来酰亚胺、2-丙烯酰胺基-2-烷基磺酸、苯乙烯磺酸和乙烯基磺酸的共聚物。优选有机阴离子保护胶体为萘磺酸和萘磺酸-甲醛缩合物,尤其是聚丙烯酸和苯酚磺酸-甲醛缩合物。
Pickering体系为有用的无机保护胶体的实例。Pickering体系易于通过非常细的固体颗粒稳定并且不溶于水,但可分散于水中,或者不溶且不可分散于水中,但可被亲油性物质润湿。它们的作用方式及其用途描述于EP-A-1 029 018和EP-A-1 321 182中,特别将其公开内容作为参考。
此处Pickering体系可由固体颗粒本身组成,或额外由改进颗粒在水中的分散性或改进颗粒被亲油相润湿的助剂材料组成。
无机固体颗粒可以为金属盐如钙、镁、铁、锌、镍、钛、铝、硅、钡和锰的盐、氧化物和氢氧化物。实例为氢氧化镁、碳酸镁、氧化镁、草酸钙、碳酸钙、碳酸钡、硫酸钡、二氧化钛、氧化铝、氢氧化铝和硫化锌。同样可以提及硅酸盐、膨润土、羟基磷灰石和水滑石。特别优选细碎硅石、焦磷酸镁和磷酸三钙。
可将Pickering体系首先加入水相中,或加入搅拌的水包油乳液中。一些细固体颗粒通过如EP-A 1 029 018和EP-A 1 321 182所述的沉淀制备。
细碎的硅石可作为细固体颗粒分散于水中。然而,也可以使用所谓的硅石的胶态水分散体。这类胶态分散体为碱性的硅石含水混合物。在碱性pH范围中,颗粒溶胀并稳定在水中。为了将这些分散体用作Pickering体系,有利的是用酸将水包油乳液的pH调至2-7。
优选使用有机保护胶体,合适的话使用与无机保护胶体的混合物。
保护胶体的用量基于水相通常为0.1-15重量%,优选0.5-10重量%。无机保护胶体的量基于水相优选为0.5-15重量%。有机保护胶体的用量基于乳液的水相优选为0.1-10重量%。
在一个实施方案中,优选无机保护胶体及其与有机保护胶体的混合物。
另一实施方案中,优选有机中性保护胶体。特别优选带有OH的保护胶体如聚乙烯醇,和部分水解的聚乙酸乙烯酯。
聚乙烯醇和/或部分水解的聚乙酸乙烯酯的总用量基于微胶囊(不含保护胶体)通常为至少3重量%,优选6-8重量%。除了优选量的聚乙烯醇或部分水解的聚乙酸乙烯酯外,还可加入其它上述保护胶体。优选微胶囊仅使用聚乙烯醇和/或部分水解的聚乙酸乙烯酯制备且不含有其它保护胶体。
在另一实施方案中,优选有机保护胶体如聚乙烯醇与纤维素衍生物的混合物。
聚乙烯醇可通过合适的话在共聚单体存在下聚合乙酸乙烯酯并将聚乙酸乙烯酯水解脱去乙酰基形成羟基而得到。聚合物的水解度例如可为1-100%,优选50-100%,特别是65-95%。此处,部分水解的聚乙酸乙烯酯的水解度为<50%,而聚乙烯醇的水解度为≥50%至100%。乙酸乙烯酯的均聚物和共聚物的合成以及将这些聚合物水解形成包含乙烯醇单元的聚合物是公知的常识。包含乙烯醇单元的聚合物例如由Kuraray SpecialitiesEurope(KSE)以牌销售。
优选在20℃在4重量%的水溶液中DIN 53015粘度为3-56mPa*s,优选14-45mPa*s的聚乙烯醇和/或部分水解的聚乙酸乙烯酯。优选水解度为≥65%,优选≥70%,特别是≥75%的聚乙烯醇。
使用聚乙烯醇和/或部分水解的聚乙酸乙烯酯产生稳定乳液,甚至对于小平均粒度如1.5-2.5μm也如此。油滴的尺寸基本等于聚合的微胶囊的尺寸。
通过如下步骤制备微胶囊的方法:
a)制备包含单体、亲油物质和聚乙烯醇和/或部分水解的聚乙酸乙烯酯的水包油乳液,其中油滴的平均尺寸为1.5-2.5μm,和
b)自由基聚合由a)得到的水包油乳液的单体。
可用于自由基聚合反应的自由基引发剂包括常规过氧和偶氮化合物,其量基于单体重量有利地为0.2-5重量%。
取决于自由基引发剂的物理状态及其溶解特性,自由基引发剂可直接加入,但优选作为溶液、乳液或悬浮液加入,因为这样使特别少量的自由基引发剂更精确地计量加入。
优选自由基引发剂为过氧新癸酸叔丁酯、过氧新戊酸叔戊酯、过氧二月桂酰、过氧-2-乙基己酸叔戊酯、2,2’-偶氮二(2,4-二甲基)戊腈、2,2’-偶氮二(2-甲基丁腈)、过氧二苯甲酰、过-2-乙基己酸叔丁酯、过氧二叔丁基、氢过氧化叔丁基、2,5-二甲基-2,5-二(叔丁基过氧)己烷和氢过氧化枯烯。
特别优选自由基引发剂为过氧二(3,5,5-三甲基己酰基)、4,4’-偶氮二异丁腈、过新戊酸叔丁酯和2,2-偶氮二异丁酸二甲酯。它们在30-100℃下的半衰期为10小时。
还可以在聚合中加入常规量的常用调节剂如叔十二烷基硫醇或巯基乙酸乙基己酯。
聚合温度通常为20-100℃,优选40-95℃。取决于所需亲油物质,水包油乳液必须在核材料为液体/油状的温度下形成。因此,所选自由基引发剂的分裂温度必须高于该温度并且聚合同样必须在比该温度高2-50℃的温度下进行,从而合适的话选择分裂温度比亲油物质的熔点高的自由基引发剂。
对于熔点至多约60℃的亲油物质的通用方法变型为,反应温度起始于60℃,在反应过程中升至85℃。有利的是自由基引发剂在45-60℃范围内的半衰期为10小时,如过新戊酸叔丁酯。
对于熔点高于60℃的亲油物质的另一方法变型,选择起始于相应较高地反应温度的温度程序。在70-90℃的范围内的半衰期为10小时的自由基引发剂对于约85℃的引发温度是优选的,如过-2-乙基己酸叔丁酯。
方便的是聚合在大气压力下进行,但也可在减压或略微升高压力下,例如在高于100℃的聚合温度,即在0.5-5巴下进行。
聚合的反应时间通常为1-10小时,常常2-5小时。
利用聚乙烯醇和/或部分水解的聚乙酸乙烯酯的本发明方法变型产生使分散和聚合直接在升高温度下进行的有利工艺方法。
在转化率为90-99重量%的实际聚合反应之后,通常有利的是使微胶囊水分散体基本不含有味载体,如残留单体和其它有机挥发性成分。这可本身已知的方式通过物理手段通过蒸馏除去(尤其是借助蒸汽蒸馏)或通过用惰性气体汽提进行。也可如WO 99/24525所述通过化学手段,有利的是如DE-A 44 35 423、DE-A 44 19 518和DE-A 44 35 422所述通过氧化还原引发聚合而进行。
取决于亲油物质,本发明微胶囊可用于无碳复印纸、化妆品、用于包封粘合剂、粘合剂组分、催化剂或用于作物保护或通常用于包封生物杀伤剂。本发明微胶囊特别可用于潜热储存材料。
根据定义,潜热储存材料为在其中发生传热的温度范围具有相变的物质。优选亲油物质的固/液相变在-20℃至120℃的温度范围。
合适的物质的实例为:
-脂族烃化合物如支化或优选线性的饱和或不饱和的C10-C40烃,如正十四烷、正十五烷、正十六烷、正十七烷、正十八烷、正十九烷、正二十烷、正二十一烷、正二十二烷、正二十三烷、正二十四烷、正二十五烷、正二十六烷、正二十七烷、正二十八以及环状烃如环己烷、环辛烷、环癸烷;-芳烃化合物如苯、萘、联苯、邻三联苯或正三联苯,C1-C40烷基取代的芳烃如十二烷基苯、十四烷基苯、十六烷基苯、己基萘或癸基萘;
-饱和或不饱和的C6-C30脂肪酸如月桂酸、硬脂酸、油酸或山萮酸,优选癸酸与如肉豆寇酸、棕榈酸或月桂酸的低共熔混合物;
-脂肪醇如月桂醇、硬脂醇、油醇、肉豆蔻醇、鲸蜡醇,混合物如椰子油脂肪醇和所谓的羰基合成醇,其中羰基合成醇通过使α-烯烃加氢甲酰化并进一步反应而得到;
-C6-C30脂肪胺如癸胺、十二烷胺、十四烷胺或十六烷胺;
-酯如脂肪酸的C1-C10烷基酯如棕榈酸丙酯、硬脂酸甲酯或棕榈酸甲酯,优选它们的低共熔混合物或肉桂酸甲酯;
-天然和合成蜡如褐煤酸蜡、褐煤酯蜡、巴西棕榈蜡、聚乙烯蜡、氧化蜡、聚乙烯基醚蜡、乙烯乙酸乙烯酯蜡或根据Fischer-Tropsch方法的硬蜡;
-卤代烃如氯代链烷烃、溴十八烷、溴十五烷、溴十九烷、溴二十烷、溴二十二烷。
这些物质的混合物也是合适的,条件是熔点不低出所需范围之外,或者混合物熔化的热对于敏感的应用太低。
例如,有利的是使用纯的正链烷烃、纯度大于80%的正链烷烃或以工业级蒸馏物制备且可直接市购的链烷烃混合物。
此外,有利的是可加入溶于其中的亲油物质的化合物,以防止有时由非极性物质引起的延迟结晶。如US-A 5 456 852中所述,有利的是使用熔点比实际的核物质高20-120K的化合物。适合的化合物为脂肪酸、脂肪醇、脂肪酰胺和脂族烃化合物,其作为上述亲油性物质提及。它们的加入量基于胶囊核为0.1-10重量%。
潜热储存材料的选择根据潜热储存介质所需的温度范围。例如,对于温和气候中的建筑材料的热储存介质,优选使用其固/液相变在0-60℃的温度范围内的潜热储存材料。因此,对于内部应用,通常选择转变温度为15-30℃的单独的材料或混合物。在作为储存介质或避免透明绝热过热的太阳能应用的情况下,如EP-A-333 145中所述,30-60℃的转变温度尤其有利。0-40℃的转变温度对织物领域的应用是有利的,-10℃至120℃的转变温度对于传热流体尤其有利。
优选潜热储存材料为脂族烃,特别优选上述作为举例列出的那些。特别优选具有14-20个碳原子的脂族烃及其混合物。
在一个优选实施方案中,在胶囊壁的外表面额外设置聚电解质。取决于聚电解质的量,排列在表面的聚电解质呈点、斑或圆点,或呈区域形式,该区域可延伸至其中聚电解质形成类似层、夹、壳或封套的均匀排列。
聚电解质的比例基于带有聚电解质的微胶囊的总重量通常为0.1-10重量%。聚电解质的比例基于带有聚电解质的微胶囊的总重量优选为0.5-5重量%,尤其是1-3重量%。
取决于应用领域,不同的壁厚可能是必须的,因此明智的是可基于壁中的单体总量进一步确定聚电解质量。
在一个实施方案中,聚电解质的量基于壁材料中的单体总量因此优选为10-30重量%。
在另一实施方案中,聚电解质的量基于壁材料中的单体总量优选为5-15重量%。
术语聚电解质通常指具有可离子化或可离子化离解的基团的聚合物,其中所述基团可以是聚合物链的成分或取代基。通常而言,聚电解质中的这些可离子化或可离子化离解的基团的数目如此巨大,以至于聚合物以离子形式(也已知为聚离子)为水溶性或可在水中溶胀。优选聚电解质在25℃下在水中的溶解度为≥4g/l,尤其是在水中具有无限溶解度的聚电解质。优选在每个重复单元带有电解质官能团的聚电解质。
与保护胶体不同,聚电解质通常具有小的(如果有的话)乳化作用以及主要具有增稠作用。在本发明范围内,聚电解质的平均分子量为500-10000000g/mol,优选1000-100000g/mol,尤其是1000-10000g/mol。可使用线性或支化聚电解质。与用于本发明的在聚合之前加入以形成水包油乳液的保护胶体不同的是,在本发明范围内的聚电解质为在聚合发生之后与含水介质,优选水中的微胶囊接触的具有可离子化或可离子化离解的基团的聚合物。含水介质是指基于含水基质包含至多10重量%的在25℃和1巴下以所需量与水溶混的水溶混性溶剂的含水混合物。这些溶剂包括醇如甲醇、乙醇、丙醇、异丙醇、乙二醇、甘油和甲氧基乙醇和水溶性醚如四氢呋喃和二噁烷以及非质子添加剂如二甲基甲酰胺或二甲亚砜。
取决于可离解基团的特性,存在阳离子和阴离子聚电解质(也已知为聚离子)。考虑不含抗衡离子的聚离子上的电荷。阳离子聚电解质由包含碱性基团的聚合物(聚碱)通过加入质子或季铵化形成。
阴离子聚电解质由包含酸性基团的聚合物(聚酸)通过脱质子形成。
聚电解质根据聚离子的最终净电荷分类(即不含抗衡离子)。当聚电解质主要带正电荷离解基团,其为阳离子聚电解质。当其主要带负电荷基团,其为阴离子聚电解质。
优选使用一种或多种阳离子或一种或多种阴离子聚电解质。特别优选选择一种或多种阳离子聚电解质。据信依次加入多种带不同电荷的聚电解质会产生多个层构造,条件是在每种情况下聚电解质的量足以构成层。通常而言,基于带有聚电解质的微胶囊的总重量为至少1重量%的聚电解质会产生层涂覆。然而,优选仅施加一层聚电解质。该层可包含一种聚电解质或多种具有相同电荷的聚电解质的混合物。
阴离子聚电解质例如可通过在含水介质中自由基聚合烯属不饱和阴离子单体而得到。有用的烯属不饱和阴离子单体例如包括单烯属不饱和C3-C5羧酸如丙烯酸、甲基丙烯酸、乙基丙烯酸、巴豆酸、马来酸、富马酸和衣康酸,磺酸如乙烯基磺酸、苯乙烯磺酸和丙烯酰胺基甲基丙烷磺酸,以及膦酸如乙烯基膦酸和/或其各自的碱金属盐、碱土金属盐和/或铵盐。
优选阴离子单体包括丙烯酸、甲基丙烯酸、马来酸和丙烯酰胺基-2-甲基丙烷磺酸。特别优选基于丙烯酸的聚合物水分散体。阴离子单体可单独聚合形成均聚物,或者以相互间的混合物聚合以形成共聚物。其实例为丙烯酸的均聚物、甲基丙烯酸的均聚物或丙烯酸与马来酸的共聚物、丙烯酸与甲基丙烯酸的共聚物以及甲基丙烯酸与马来酸的共聚物。
然而,阳离子单体也可在至少一种其它烯属不饱和单体存在下聚合。这些单体可以是非离子的或者带有阳离子电荷。
非离子共聚单体的实例为丙烯酰胺、甲基丙烯酰胺、N-C1-C3烷基丙烯酰胺、N-乙烯基甲酰胺、具有1-20个碳原子的一元醇的丙烯酸酯,尤其是丙烯酸甲酯、丙烯酸乙酯、丙烯酸异丁酯和丙烯酸正丁酯,具有1-20个碳原子的一元醇的甲基丙烯酸酯如甲基丙烯酸甲酯和甲基丙烯酸乙酯以及乙酸乙烯酯和丙酸乙烯酯。
可用于与阴离子单体共聚的阳离子单体包括丙烯酸二烷基氨基乙酯、甲基丙烯酸二烷基氨基乙酯、丙烯酸二烷基氨基丙酯、甲基丙烯酸二烷基氨基丙酯、二烷基氨基乙基丙烯酰胺、二烷基氨基乙基甲基丙烯酰胺、二烷基氨基丙基丙烯酰胺、二烷基氨基丙基甲基丙烯酰胺、二烯丙基二甲基氯化铵、乙烯基咪唑,以及各自用无机酸中和和/或季铵化的阳离子单体。阳离子单体的具体实例为丙烯酸二甲基氨基乙酯、甲基丙烯酸二甲基氨基乙酯、丙烯酸二乙基氨基乙酯、甲基丙烯酸二乙基氨基乙酯、丙烯酸二甲基氨基丙酯、甲基丙烯酸二甲基氨基丙酯、丙烯酸二乙基氨基丙酯和甲基丙烯酸二乙基氨基丙酯、二甲基氨基乙基丙烯酰胺、二甲基氨基乙基甲基丙烯酰胺、二甲基氨基丙基丙烯酰胺、二甲基氨基丙基甲基丙烯酰胺、二乙基氨基乙基丙烯酰胺和二乙基氨基丙基丙烯酰胺。
阳离子单体可完全或仅部分中和或季铵化,例如在每种情况下的程度为1-99%。硫酸二甲酯为阳离子单体的优选季铵化剂。然而,单体也可用硫酸二乙酯季铵化或用烷基化剂,尤其烷基卤如甲基氯、乙基氯或苄基氯季铵化。制备阴离子聚电解质的共聚单体的用量例如使得所得聚合物分散体在高于7.0的pH和在20℃下下用水稀释时为水溶性且具有阴离子电荷。基于用于聚合的全部单体,非离子和/或阳离子共聚单体的量例如为0-99重量%,优选5-75重量%且通常为5-25重量%。阳离子单体的用量至多为使得所得聚电解质在pH<6.0和20℃下具有净阴离子电荷。在所形成的两性聚合物中过量的阴离子电荷例如为至少5mol%,优选至少10mol%,尤其是至少30mol%,最优选至少50mol%。
优选共聚物的实例为包含25-90重量%丙烯酸和75-10重量%丙烯酰胺的共聚物。优选将至少一种烯属不饱和C3-C5羧酸在其它单烯属不饱和单体不存在下聚合。特别优选可通过在其它单体不存在下自由基聚合丙烯酸而得到的丙烯酸均聚物。
可用于制备支化聚电解质的交联剂包括所有在分子中具有至少两个烯属不饱和双键的化合物。这类化合物例如用于制备交联的聚丙烯酸如超吸收剂聚合物,参见EP-A 0 858 478,第4页,第30行至第5页第43行。交联剂的实例为三烯丙基胺、季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、亚甲基双丙烯酰胺、N,N’-二乙烯基亚乙基脲,多元醇如山梨糖醇、1,2-乙二醇、1,4-丁二醇、三羟甲基丙烷、甘油、二甘醇以及糖如蔗糖、葡萄糖、甘露糖的至少二烯丙基醚或至少二乙烯基醚,全丙烯酸酯化或甲基丙烯酸酯化的具有2-4个碳原子的二元醇如乙二醇二甲基丙烯酸酯、乙二醇二丙烯酸酯、丁二醇二甲基丙烯酸酯、丁二醇二丙烯酸酯,分子量为300-600的聚乙二醇的二丙烯酸酯或二甲基丙烯酸酯,乙氧基化三亚甲基丙烷三丙烯酸酯或乙氧基化三亚甲基丙烷三甲基丙烯酸酯,2,2-二(羟基甲基)丁醇三甲基丙烯酸酯、季戊四醇三丙烯酸酯、季戊四醇四丙烯酸酯和三烯丙基甲基氯化铵。当将交联剂用于本发明分散体的制备中时,在每种情况下使用的交联剂的量基于用于聚合的全部单体例如为0.0005-5.0重量%,优选0.001-1.0重量%。优选交联剂为季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、N,N′-二乙烯基亚乙基脲,糖如蔗糖、葡萄糖或甘露糖的至少二烯丙基醚和三烯丙基胺及其混合物。
有用的阴离子聚电解质进一步包括缩聚物如苯酚磺酸树脂。具有适用性的为醛缩合物,特别是基于甲醛、乙醛、异丁醛、丙醛、戊二醛和乙二醛的醛缩合物,非常特别优选基于苯酚磺酸的甲醛缩合物。胺和酰胺,尤其是碳酸的那些,如脲、蜜胺或双氰胺为可一起用于制备苯酚磺酸树脂的其它反应化合物的实例。
苯酚磺酸树脂优选以盐存在。本发明的缩合产物优选的缩合度为1-20且平均分子量为500-10000g/mol。苯酚磺酸树脂优选以类似于EP-A 816 406中所述的方式制备。
有用的阳离子聚电解质例如包括来自下组的聚合物:
(a)包含乙烯基咪唑鎓单元的聚合物,
(b)聚二烯丙基二甲基卤化铵,
(c)包含乙烯基胺单元的聚合物,
(d)包含吖丙啶单元的聚合物,
(e)包含丙烯酸二烷基氨基烷基酯和/或甲基丙烯酸二烷基氨基烷基酯单元的聚合物,和
(f)包含二烷基氨基烷基丙烯酰胺和/或二烷基氨基烷基甲基丙烯酰胺单元的聚合物。
这类聚合物是已知的且可市购。在组(a)-(f)的阳离子聚电解质中存在的单体可以游离碱形式用于聚合,但优选以其与无机酸如盐酸、硫酸或磷酸的盐形式或以季铵化形式用于聚合。有用的季铵化剂例如包括硫酸二甲酯、硫酸二乙酯、甲基氯、乙基氯、鲸蜡基氯或苄基氯。
阳离子聚电解质的实例为:
(a)乙烯基咪唑鎓甲基硫酸盐的均聚物和/或乙烯基咪唑鎓甲基硫酸盐和N-乙烯基吡咯烷酮的共聚物,
(b)聚二烯丙基二甲基氯化铵,
(c)聚乙烯胺以及部分水解的聚乙烯基甲酰胺,
(d)聚乙烯亚胺,
(e)聚丙烯酸二甲基氨基乙酯、聚甲基丙烯酸二甲基氨基乙酯、丙烯酰胺与丙烯酸二甲基氨基乙酯的共聚物以及丙烯酰胺与甲基丙烯酸二甲基氨基乙酯的共聚物,对于它们,碱性单体也可以与无机酸的盐形式或季铵化形式存在,和
(f)聚二甲基氨基乙基丙烯酰胺、聚二甲基氨基乙基甲基丙烯酰胺和丙烯酰胺与二甲基氨基乙基丙烯酰胺的共聚物,对于它们,阳离子单体也可以与无机酸的盐形式或季铵化形式存在。
阳离子聚电解质的平均分子量Mw为至少500g/mol。平均分子量例如为500g/mol至10百万g/mol,优选1000-500000g/mol,通常1000-5000g/mol。
优选将如下聚合物用作阳离子聚合物:
(a)在每种情况下平均分子量Mw为500-10000g/mol的乙烯基咪唑鎓甲基硫酸盐的均聚物和/或乙烯基咪唑鎓甲基硫酸盐和N-乙烯基吡咯烷酮的共聚物,
(b)平均分子量Mw为1000-10000g/mol的聚二烯丙基二甲基氯化铵,
(c)平均分子量Mw为500-10000g/mol的聚乙烯胺以及部分水解的聚乙烯基甲酰胺,和
(d)平均分子量Mw为500-10000g/mol的聚乙烯亚胺。
在(a)下提及的乙烯基咪唑鎓甲基硫酸盐和N-乙烯基吡咯烷酮的共聚物例如以聚合单元形式包含10-90重量%N-乙烯基吡咯烷酮。除了N-乙烯基吡咯烷酮外,作为共聚单体还可使用至少一种选自烯属不饱和C3-C5羧酸,尤其是如丙烯酸或甲基丙烯酸,或者这些羧酸与包含1-18个碳原子的一元醇的酯如丙烯酸甲酯、丙烯酸乙酯、丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸异丁酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯或甲基丙烯酸正丁酯的化合物。
优选(b)组聚合物为聚二烯丙基二甲基氯化铵。还合适的是二烯丙基二甲基氯化铵与丙烯酸二甲基氨基乙酯的共聚物,二烯丙基二甲基氯化铵与甲基丙烯酸二甲基氨基乙酯的共聚物,二烯丙基二甲基氯化铵与丙烯酸二乙基氨基乙酯的共聚物,二烯丙基二甲基氯化铵与丙烯酸二甲基氨基丙酯的共聚物,二烯丙基二甲基氯化铵与二甲基氨基乙基丙烯酰胺的共聚物以及二烯丙基二甲基氯化铵与二甲基氨基丙基丙烯酰胺的共聚物。二烯丙基二甲基氯化铵的共聚物例如包含以聚合单元形式掺入的1-50mol%,通常2-30mol%至少一种所述共聚单体。
包含乙烯基胺单元的聚合物(c)可通过合适的话在共聚单体存在下聚合N-乙烯基甲酰胺,并将聚乙烯基甲酰胺水解以消除甲酰基并形成氨基而得到。聚合物的水解度例如可为1-100%,优选60-100%。对本发明而言,部分水解的聚乙烯基甲酰胺的水解度为≥50%,优选≥90%。N-乙烯基甲酰胺的均聚物和共聚物的制备和这些聚合物水解形成包含乙烯基胺单元的聚合物例如详细描述于US 6,132,558,第2栏第36行至第5栏第25行。此处将其中所做的描述作为参考引入本发明的公开内容。包含乙烯基胺单元的聚合物例如由BASF Aktiengesellschaft以和牌销售。
包含吖丙啶单元的组(d)的聚合物如聚乙烯基亚胺同样为市售产品。它们例如由BASF Aktiengesellschaft以如SK销售。这些阳离子聚合物为吖丙啶的聚合物,其通过在含水介质中在少量酸或形成酸的化合物如卤代烃如氯仿、四氯化碳、四氯乙烷或乙基氯存在下聚合而制备,或者这些阳离子聚合物为表氯醇和包含氨基的化合物如单胺和多胺如二甲胺、二乙胺、乙二胺、二亚乙基三胺和三亚乙基四胺或氨的缩合物。它们的分子量Mw例如为500g/mol至1百万g/mol,优选1000-500000g/mol。
该组阳离子聚合物也包括吖丙啶在具有伯氨基或仲氨基的化合物如二羧酸和多胺的聚酰胺型胺上的接枝聚合物。用吖丙啶接枝的聚酰胺型胺合适的话也可与双官能交联剂如与表氯醇或聚亚烷基二醇的二表氯醇醚反应。
组(e)的合适的阳离子聚合物为包含丙烯酸二烷基氨基烷基酯和/或甲基丙烯酸二烷基氨基烷基酯单元的聚合物。这些单体可以游离碱形式,但优选以与无机酸如盐酸、硫酸或磷酸的盐形式以及以季铵化形式用于聚合。合适的季铵化剂例如为硫酸二甲酯、硫酸二乙酯、甲基氯、乙基氯、鲸蜡基氯或苄基氯。均聚物和共聚物均可由这些单体制备。合适的共聚单体例如为丙烯酰胺、甲基丙烯酰胺、N-乙烯基甲酰胺、N-乙烯基吡咯烷酮、丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯以及所述单体的混合物。
组(f)的阳离子聚合物为包含二甲基氨基乙基丙烯酰胺或二甲基氨基乙基甲基丙烯酰胺单元和包含优选以与无机酸的盐形式或以季铵化形式的阳离子单体的聚合物。它们可以为均聚物和共聚物。实例为用硫酸二甲酯或苄基氯完全季铵化的二甲基氨基乙基丙烯酰胺的均聚物,用硫酸二甲酯、甲基氯、乙基氯或苄基氯完全季铵化的二甲基氨基乙基甲基丙烯酰胺的均聚物,以及用硫酸二甲酯季铵化的丙烯酰胺和二甲基氨基乙基丙烯酰胺的共聚物。
除了仅包含阳离子单体的那些聚阳离子外,也可将两性聚合物用作阳离子聚合物,条件是它们总体上带有阳离子电荷。两性聚合物中阳离子电荷例如过量至少5mol%,优选至少10mol%且通常为15-95mol%。具有过量阳离子电荷的两性聚合物的实例为:
-丙烯酰胺、丙烯酸二甲基氨基乙酯和丙烯酸的共聚物,其包含比以聚合单元形式掺入的丙烯酸多至少5mol%的丙烯酸二甲基氨基乙酯,
-乙烯基咪唑鎓甲基硫酸盐、N-乙烯基吡咯烷酮和丙烯酸的共聚物,其包含比以聚合单元形式掺入的丙烯酸多至少5mol%乙烯基咪唑鎓甲基硫酸盐,
-N-乙烯基甲酰胺和烯属不饱和C3-C5羧酸,优选丙烯酸或甲基丙烯酸的水解共聚物,其乙烯基胺单元的含量比烯属不饱和羧酸的单元高至少5mol%,
-乙烯基咪唑、丙烯酰胺和丙烯酸的共聚物,其中选择pH,以使比以聚合单元形式掺入的丙烯酸多至少5mol%的乙烯基咪唑带阳离子电荷。
对本发明而言,有用的聚电解质进一步包括生物聚合物,如海藻酸、阿拉伯树胶、核酸、果胶、蛋白质,以及化学改性的生物聚合物如离子或可离子化的多糖,实例为羧甲基纤维素、壳聚糖、壳聚糖硫酸盐和木素磺酸盐。
优选聚电解质选自聚丙烯酸、苯酚磺酸预缩合物、聚二烯丙基二甲基氯化铵、聚乙烯基胺、部分水解的聚乙烯基甲酰胺和聚乙烯亚胺。
在一个实施方案中,优选阴离子聚电解质,尤其是聚丙烯酸和苯酚磺酸树脂。
在一个实施方案中,优选阳离子聚电解质,尤其是组(b)、(c)和(d)的阳离子聚电解质,即聚二烯丙基二甲基氯化铵、聚乙烯胺和部分水解的聚乙烯基甲酰胺和聚乙烯亚胺。特别优选使用聚二烯丙基二甲基氯化铵作为阳离子聚电解质。
聚电解质改性的微胶囊通过使微胶囊或优选微胶囊分散体与一种或多种聚电解质合适的话在水或含水介质中接触而得到。
优选平均粒度为1.5-2.5μm且其中90%的颗粒的粒度≤4μm的聚电解质改性的微胶囊以及优选实施方案的组合。它们通过使包含胶囊核和胶囊壁的微胶囊与一种或多种聚电解质在水或含水介质中接触而得到,其中基于单体总重量,胶囊壁由如下单体构成:
30-90重量%的一种或多种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸,优选一种或多种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯(单体I),
10-70重量%二乙烯基和多乙烯基单体的混合物(单体II),其中多乙烯基单体的比例基于单体II为2-90重量%,以及
0-30重量%其它单体(单体III),
其中微胶囊的平均粒度为1.5-2.5μm且90%的颗粒具有≤4μm的粒度。优选使微胶囊分散体与一种或多种聚电解质接触。
它们优选通过如下步骤得到:
a)制备包含单体、亲油物质和聚乙烯醇和/或部分水解的聚乙酸乙烯酯的水包油乳液,其中油滴的平均尺寸为1.5-2.5μm,和
b)自由基聚合由a)得到的水包油乳液的单体以及合适的话分离微胶囊,
c)使b)中得到的微胶囊或微胶囊分散体与一种或多种聚电解质合适的话在水或含水介质中接触。
将聚电解质在不含溶剂下或以溶液,优选作为水溶液加入起始微胶囊分散体中。聚电解质的量基于起始微胶囊的量为0.1-5重量%,优选0.25-1.5重量%。
合适的话,随后可将本发明微胶囊通过喷雾干燥分离。自由基聚合b)的方法步骤产生作为中间产物的起始微胶囊分散体,将该分散体在步骤c)中与聚电解质接触。聚电解质改性的微胶囊分散体的粒度分布相对于起始微胶囊分散体没有变化。优选将方法步骤b)中得到的微胶囊分散体与一种或多种聚电解质接触,即不进行微胶囊的中间分离。因此此时存在水分散体,其中使微胶囊和聚电解质接触的所需介质已经可供使用。接触例如应理解为指用常规搅拌器或混合器混合。
本发明微胶囊可直接作为微胶囊水分散体加工或以粉末形式加工。当用于织物领域中时,微胶囊对干洗具有良好耐久性以及良好的蒸发率。它们也具有良好的雾化值。
本发明微胶囊粉末具有多种用途。对于改性纤维和制备的织物制品,例如织造织物和非织造物(例如毡)非常有用。此处,有用的应用形式尤其包括微胶囊涂层、具有微胶囊的泡沫和微胶囊改性的织物纤维。对于涂层,将微胶囊与聚合物粘合剂以及合适的话其它助剂材料通常作为分散体一起施加至制备的织物制品。常规的织物粘合剂为玻璃化转变温度为-45℃至45℃,优选-30℃至12℃的成膜聚合物。这类微胶囊涂层的制备例如描述于WO 95/34609中,此处完全引入作为参考。用微胶囊改性泡沫以类似于DE 981576T和US 5,955,188中所述的方式进行。用含粘合剂的微胶囊分散体表面处理预发泡的基材,优选聚氨酯或聚醚。随后通过施加减压使粘合剂-微胶囊混合物与开孔泡沫结构接触,其中粘合剂固化并将微胶囊与基材连接。另一加工可能性为改性织物纤维本身,如US 2002/0054964所述通过由熔体或水分散体纺丝而进行。熔体纺丝方法用于尼龙纤维、聚酯纤维、聚丙烯纤维和类似的纤维,而湿法纺丝方法尤其用于制备丙烯酸类纤维。
另一宽的应用领域为粘合包含矿物、硅酸盐或聚合物粘合剂的建筑材料。在成型制品和涂覆组合物之间加以区别。它们的显著之处在于它们对含水材料和常见的碱性含水材料的水解稳定性。
术语矿物成型制品是指由矿物粘合剂、水、集料以及合适的话助剂在成型后通过在升高温度或不在升高温度的作用下随时间固化矿物粘合剂/水混合物形成的成型制品。矿物粘合剂是公知的常识。它们包括细碎无机物质如石灰、石膏、粘土、壤土和/或水泥,通过与水搅拌将它们转化为即用形式,并且在空气或甚至在水下以及在升高温度或不在升高温度的作用下随时间使其自身固化为石头状物质。
集料通常由颗粒状或纤维状天然或合成岩石(颗粒、沙、玻璃纤维或矿物纤维)组成,或者在特定情况下由金属或有机集料或其混合物组成,将其粒度或纤维长度在每种情况下以常规方式与意欲用途匹配。在许多情况下,也将彩色颜料用作集料以用于着色目的。
有用的助剂尤其包括促进或延迟固化或影响固化矿物成型制品弹性或空隙率的物质。它们尤其为例如由US-A 4 340 510、GB专利1 505 558、US-A 3 196 122、US-A 3 043 790、US-A 3 239 479、DE-A 43 17 035、DE-A 43 17 036、JP-A 91/131 533和其它参考文献已知的聚合物。
本发明微胶囊适用于改性包含矿物粘合剂的矿物粘合建筑材料(砂浆类制剂),该矿物粘合剂由70-100重量%水泥和0-30重量%石膏组成。这在水泥为仅有的矿物粘合剂时尤其如此。本发明的效果与水泥类型基本无关。因此,取决于手边的产品,可以使用高炉水泥、油页岩水泥、波特兰水泥、疏水化波特兰水泥、快凝水泥、高膨胀水泥或高铝水泥,使用波特兰水泥证明是特别有利的。对于进一步的细节可参考DE-A 196 23 413。矿物粘合建筑材料的干组合物通常基于矿物粘合剂的量包含0.1-20重量%微胶囊。
优选将本发明微胶囊掺入矿物涂覆组合物如打底中。用于内部区域的这类打底通常包含石膏粘合剂。石膏/微胶囊的重量比通常为95∶5-70∶30。更高的微胶囊比例当然也是可以的。
用于外部区域如外表面或潮湿环境的涂料可包含作为粘合剂的水泥(水泥类打底)、石灰或水玻璃(矿物或硅酸盐打底)或聚合物分散体(合成树脂打底)和填料以及合适的话用于着色的颜料。微胶囊占的总固体比例对应于石膏打底的重量比。
本发明微胶囊还可用于聚合物成型制品或聚合物涂料组合物。这是指其加工不能破坏微胶囊的热塑性和热固性塑料材料。实例为环氧树脂、脲、蜜胺、聚氨酯和硅树脂以及涂料材料-溶剂性、高固体、粉末涂料或水性-和分散膜。微胶囊粉末也适用于掺入聚合物泡沫和纤维中。泡沫的实例为聚氨酯泡沫、聚苯乙烯泡沫、乳胶泡沫和蜜胺树脂泡沫。
本发明微胶囊可进一步用于木素纤维素成型制品如粗纸板。
如果在经受发泡的矿物成型制品中加工本发明微胶囊,则可进一步实现有利效果。
本发明微胶囊可进一步用于改性石膏板。微胶囊粉末以基于石膏板的总重量(干物质)优选为5-40重量%,尤其是20-35重量%的量掺入石膏板。包含微胶囊化潜热储存介质的石膏板的制备是常识且描述于EP-A 1 421243中,此处引入作为参考。除了基于纤维素的板之外,也可使用替代的纤维结构体作为两面覆盖物用于“石膏板”。替代材料为例如包含聚丙烯、聚酯、聚酰胺、聚丙烯酸酯、聚丙烯腈等的聚合物纤维。玻璃纤维同样合适。替代材料可以织造物或非织造物使用。合适的建筑板例如由US 4,810,569、US 4,195,110和US 4,394,411已知。
本发明微胶囊可进一步用于制备传热流体。此处,传热流体不仅指用于传输热量的流体而且指用于冷却传输的流体,即冷却流体。在两种情况下,热能传输的原理是相同的且仅在传输方向方面不同。
如下实施例阐述本发明。除非另有说明,实施例中的百分数为重量百分数。
微胶囊粉末的粒度使用3600E Malvern粒度仪根据文献中记录的标准测量方法测定。D(0.1)值说明10%的颗粒的粒度(体积平均)至多为该值。因此,D(0.5)是指50%的颗粒的粒度(体积平均)不超过该值。跨度值为差(D(0.9)-D(0.1))与D(0.5)的商。
测定蒸发率
对于预处理,将2g微胶囊分散体在金属盘中在105℃下干燥2小时以除去任何残留水。然后,测定重量(mo)。在180℃下加热1小时并冷却之后,再测定重量(m1)。基于m0的(m0-m1)重量差并乘以100为蒸发率百分数。值越小,微胶囊的致密度越好。应考虑到的是,对于蒸发率的比较总是应对相当的胶囊尺寸和稳定剂体系进行。
制备微胶囊分散体
实施例1a和1b:通过无机Pickering体系稳定的胶囊
实施例1a(非本发明)
水相
630g 水
110g 50% pH为9.2的SiO2的胶态水分散体(粒度约80-100nm)
2.1g 2.5重量%亚硝酸钠水溶液
油相
431g 工业级石蜡馏分C16-C18(约92%C18)
9g 沙索蜡(Sasol wax)6805(高熔点石蜡)
82.5g 甲基丙烯酸甲酯(MMA)
27.5g 丁二醇二丙烯酸酯(BDA2)
0.76g 巯基乙酸乙基己酯
0.92g 75重量%的过新戊酸叔丁酯在脂族烃中的溶液
加料1
7.65g 10重量%氢过氧化叔丁基水溶液
进料流1
28.34g 1.1重量%抗坏血酸水溶液
a)将水相作为起始装料引入并用20重量%的硫酸将pH调节至2.5。在40℃下,加入油相并用高速溶解器在3500rpm下将混合物分散40分钟,得到稳定乳液。
b)将用锚式搅拌器搅拌的乳液经60分钟加热至67℃,经另一60分钟加热至85℃并在85℃下维持1小时。加入加料1并将所得微胶囊分散体经30分钟在搅拌下冷却至20℃,同时经80分钟加入进料流1。
这得到固含量为43.8重量%且平均粒度为D[4,3]=8.34μm、跨度=0.98的微胶囊分散体。蒸发率为70.6%且雾化值为1.3mg/g。
实施例1b
重复实施例1a,不同之处在于用季戊四醇四丙烯酸酯(PETIA)代替50重量%丁二醇二丙烯酸酯。
这得到固含量为39.3重量%且平均粒度为D[4,3]=5.82μm、跨度=1.01的微胶囊分散体。蒸发率为64.6%。
实施例2a-2e
水相
380g 水
47.5g 10重量%聚乙烯醇水溶液(Mowiol 15-79)
2.1g 2.5重量%亚硝酸钠水溶液
油相
431g 工业级十八烷(纯度为95重量%)
9g 沙索蜡6805(高熔点石蜡)
19.6g 甲基丙烯酸甲酯
19.6g 交联剂混合物,参见表1
9.8g 甲基丙烯酸
0.7g 75重量%的过新戊酸叔丁酯在脂族烃中的溶液
加料1
5.38g 10重量%氢过氧化叔丁基水溶液
进料流1
28.3g 1.1重量%抗坏血酸水溶液
a)在40℃下,将上述水相作为起始装料引入,并在加入油相之后,用高速溶解器在3500rpm下分散混合物。在分散40分钟后得到稳定乳液。
b)将用锚式搅拌器搅拌的乳液经60分钟加热至70℃,经另一60分钟加热至85℃并在85℃下维持1小时。加入加料1并将所得微胶囊分散体经30分钟在搅拌下冷却至20℃,同时加入进料流1。
所得微胶囊分散体的特征示于表1。微胶囊的平均粒度D[4,3]=3-5μm。
表1:来自不同交联剂混合物的微胶囊
BDA2:丁二醇二丙烯酸酯
PETIA:季戊四醇四丙烯酸酯
实施例2a和2e为非本发明的。
实施例3a-3h
水相
425g 水
412g 10重量%聚乙烯醇水溶液Mowiol 40-88)
2.1g 2.5重量%亚硝酸钠水溶液
油相
431g 工业级石蜡馏分C16-C18(约92%C18)
9g 沙索蜡6805(高熔点石蜡)
77.6g 单体混合物,按照表2
0.76g 巯基乙酸乙基己酯
0.7g 75重量%的过新戊酸叔丁酯在脂族烃中的溶液
加料1
5.38g 10重量%氢过氧化叔丁基水溶液,
进料流1
28.3g 1.1重量%抗坏血酸水溶液
加料2
1.00g 25%氢氧化钠水溶液
1.43g 水
a)在70℃下,将上述水相作为起始装料引入,并在加入油相之后,用高速溶解器在6000rpm下分散混合物。在分散40分钟后得到平均粒度D[4,3]=2.3μm直径的稳定乳液。
b)将用锚式搅拌器搅拌的乳液经60分钟加热至70℃,经另一60分钟加热至85℃并在85℃下维持1小时。加入加料1并将所得微胶囊分散体经30分钟在搅拌下冷却至20℃,同时加入进料流1。加入加料2将pH调节至7。
所得微胶囊分散体的特征描述于表2。
Claims (13)
1.包含胶囊核和胶囊壁的微胶囊,其中基于单体总重量,胶囊壁由如下单体构成:
30-80重量%的一种或多种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸,即单体I,
20-60重量%二乙烯基和多乙烯基单体的混合物,即单体II,其中多乙烯基单体的比例基于单体II为5-80重量%,以及
0-30重量%一种或多种其它单体,即单体III;
其中所述二乙烯基单体选自二醇与丙烯酸或甲基丙烯酸的二酯以及这些二醇的二烯丙基醚和二乙烯基醚、二乙烯基苯和二乙烯基环己烷;
所述多乙烯基单体选自多元醇与丙烯酸和/或甲基丙烯酸的聚酯以及这些多元醇的多烯丙基醚和多乙烯基醚;
所述其它单体选自乙酸乙烯酯、丙酸乙烯酯、乙烯基吡啶、苯乙烯、α-甲基苯乙烯、衣康酸、马来酸酐、丙烯酸2-羟基乙酯、甲基丙烯酸2-羟基乙酯、丙烯酰胺基-2-甲基丙烷磺酸、甲基丙烯腈、丙烯腈、甲基丙烯酰胺、N-乙烯基吡咯烷酮、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、甲基丙烯酸二甲基氨基乙酯和甲基丙烯酸二乙基氨基乙酯。
2.根据权利要求1的微胶囊,其中微胶囊的平均粒度为1.5-2.5μm且90%的颗粒的粒度≤4μm。
3.根据权利要求1的微胶囊,其中所述多乙烯基单体选自三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、季戊四醇三丙烯酸酯和季戊四醇四丙烯酸酯。
4.根据权利要求1的微胶囊,其中所述胶囊核为固/液相变在-20℃至120℃的温度范围的亲油物质。
5.根据权利要求1的微胶囊,其中在胶囊壁的外表面额外设置平均分子量为500g/mol至10百万g/mol的聚电解质。
6.根据权利要求1的微胶囊,其中聚电解质量基于带有聚电解质的微胶囊的总重量为0.1-10重量%。
7.根据权利要求1的微胶囊,其呈水分散体形式。
8.一种制备根据权利要求1的包含胶囊核和胶囊壁的微胶囊的方法,其中基于单体总重量,胶囊壁由如下单体构成:
30-80重量%的一种或多种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸,即单体I,
20-60重量%二乙烯基和多乙烯基单体的混合物,即单体II,其中多乙烯基单体的比例基于单体II为5-80重量%,以及
0-30重量%其它单体,即单体III,该方法通过加热其中单体、自由基引发剂和亲油物质作为分散相存在的水包油乳液而进行。
9.根据权利要求8的制备微胶囊的方法,其通过如下步骤进行:
a)制备包含单体、亲油物质和聚乙烯醇和/或部分水解的聚乙酸乙烯酯的水包油乳液,其中油滴的平均尺寸为1.5-2.5μm,和
b)自由基聚合由a)得到的水包油乳液的单体。
10.根据权利要求8的制备微胶囊的方法,其中使微胶囊分散体与一种或多种聚电解质接触。
11.根据权利要求1的微胶囊在掺入织物中的使用方法。
12.根据权利要求1的微胶囊在粘合建筑材料中的使用方法。
13.根据权利要求1的微胶囊的分散体在传热流体中的使用方法。
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US20130225717A1 (en) | 2013-08-29 |
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JP5096486B2 (ja) | 2012-12-12 |
JP2010512986A (ja) | 2010-04-30 |
WO2008071649A2 (de) | 2008-06-19 |
EP2099557A2 (de) | 2009-09-16 |
US9217080B2 (en) | 2015-12-22 |
CN101547736A (zh) | 2009-09-30 |
EP2099557B1 (de) | 2016-03-23 |
WO2008071649A3 (de) | 2008-09-12 |
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