JP2023113992A - paste vinyl chloride resin - Google Patents
paste vinyl chloride resin Download PDFInfo
- Publication number
- JP2023113992A JP2023113992A JP2022016012A JP2022016012A JP2023113992A JP 2023113992 A JP2023113992 A JP 2023113992A JP 2022016012 A JP2022016012 A JP 2022016012A JP 2022016012 A JP2022016012 A JP 2022016012A JP 2023113992 A JP2023113992 A JP 2023113992A
- Authority
- JP
- Japan
- Prior art keywords
- vinyl chloride
- weight
- parts
- chloride resin
- paste
- 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.)
- Pending
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- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 title claims abstract description 180
- 229920005989 resin Polymers 0.000 title claims abstract description 112
- 239000011347 resin Substances 0.000 title claims abstract description 112
- 239000002245 particle Substances 0.000 claims abstract description 76
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 64
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000009826 distribution Methods 0.000 claims abstract description 16
- 238000010022 rotary screen printing Methods 0.000 claims abstract description 12
- 150000008051 alkyl sulfates Chemical class 0.000 claims abstract description 9
- 239000004816 latex Substances 0.000 claims description 38
- 229920000126 latex Polymers 0.000 claims description 38
- -1 alkylbenzene sulfonate Chemical class 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 16
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 13
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 13
- 239000004014 plasticizer Substances 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 8
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-O triethanolammonium Chemical compound OCC[NH+](CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-O 0.000 claims description 5
- 238000000790 scattering method Methods 0.000 claims description 4
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 claims description 3
- 229940063953 ammonium lauryl sulfate Drugs 0.000 claims description 3
- 229940043264 dodecyl sulfate Drugs 0.000 claims description 3
- 238000007561 laser diffraction method Methods 0.000 claims description 3
- YFVGRULMIQXYNE-UHFFFAOYSA-M lithium;dodecyl sulfate Chemical compound [Li+].CCCCCCCCCCCCOS([O-])(=O)=O YFVGRULMIQXYNE-UHFFFAOYSA-M 0.000 claims description 2
- 159000000000 sodium salts Chemical group 0.000 claims 1
- 238000005187 foaming Methods 0.000 abstract description 15
- 238000007639 printing Methods 0.000 abstract description 6
- 239000000178 monomer Substances 0.000 description 47
- 239000006260 foam Substances 0.000 description 29
- 239000007864 aqueous solution Substances 0.000 description 15
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 15
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 14
- 238000003786 synthesis reaction Methods 0.000 description 14
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000002156 mixing Methods 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 239000003995 emulsifying agent Substances 0.000 description 8
- 239000003381 stabilizer Substances 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 239000003085 diluting agent Substances 0.000 description 7
- 239000004088 foaming agent Substances 0.000 description 7
- 239000000049 pigment Substances 0.000 description 7
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 description 6
- 239000003063 flame retardant Substances 0.000 description 6
- 239000011541 reaction mixture Substances 0.000 description 6
- 229920006395 saturated elastomer Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 3
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 3
- ZUBJEHHGZYTRPH-KTKRTIGZSA-N [(z)-octadec-9-enyl] hydrogen sulfate Chemical compound CCCCCCCC\C=C/CCCCCCCCOS(O)(=O)=O ZUBJEHHGZYTRPH-KTKRTIGZSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003505 polymerization initiator Substances 0.000 description 3
- URLJMZWTXZTZRR-UHFFFAOYSA-N sodium myristyl sulfate Chemical class CCCCCCCCCCCCCCOS(O)(=O)=O URLJMZWTXZTZRR-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000007720 emulsion polymerization reaction Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000001530 fumaric acid Substances 0.000 description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229950005425 sodium myristyl sulfate Drugs 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical class OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- KAKVFSYQVNHFBS-UHFFFAOYSA-N (5-hydroxycyclopenten-1-yl)-phenylmethanone Chemical compound OC1CCC=C1C(=O)C1=CC=CC=C1 KAKVFSYQVNHFBS-UHFFFAOYSA-N 0.000 description 1
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- IOSXLUZXMXORMX-UHFFFAOYSA-N 1-ethenoxypentane Chemical compound CCCCCOC=C IOSXLUZXMXORMX-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- MKTOIPPVFPJEQO-UHFFFAOYSA-N 4-(3-carboxypropanoylperoxy)-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OOC(=O)CCC(O)=O MKTOIPPVFPJEQO-UHFFFAOYSA-N 0.000 description 1
- JHWLWOYSFJIYQV-UHFFFAOYSA-N 4-dodecylbenzenesulfonate;tris(2-hydroxyethyl)azanium Chemical compound OCC[NH+](CCO)CCO.CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHWLWOYSFJIYQV-UHFFFAOYSA-N 0.000 description 1
- FVAIEHAPKZFAGH-UHFFFAOYSA-N 6,6-dimethylheptanoyl 6,6-dimethylheptaneperoxoate Chemical compound CC(CCCCC(=O)OOC(CCCCC(C)(C)C)=O)(C)C FVAIEHAPKZFAGH-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- ATMLPEJAVWINOF-UHFFFAOYSA-N acrylic acid acrylic acid Chemical class OC(=O)C=C.OC(=O)C=C ATMLPEJAVWINOF-UHFFFAOYSA-N 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 239000012615 aggregate Substances 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- PLUHAVSIMCXBEX-UHFFFAOYSA-N azane;dodecyl benzenesulfonate Chemical compound N.CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 PLUHAVSIMCXBEX-UHFFFAOYSA-N 0.000 description 1
- AHVCYVORAAEAKW-UHFFFAOYSA-N azanium;tetradecyl sulfate Chemical compound N.CCCCCCCCCCCCCCOS(O)(=O)=O AHVCYVORAAEAKW-UHFFFAOYSA-N 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 229960000541 cetyl alcohol Drugs 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229930016911 cinnamic acid Natural products 0.000 description 1
- 235000013985 cinnamic acid Nutrition 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000012933 diacyl peroxide Substances 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 description 1
- RZMWTGFSAMRLQH-UHFFFAOYSA-L disodium;2,2-dihexyl-3-sulfobutanedioate Chemical compound [Na+].[Na+].CCCCCCC(C([O-])=O)(C(C([O-])=O)S(O)(=O)=O)CCCCCC RZMWTGFSAMRLQH-UHFFFAOYSA-L 0.000 description 1
- YHAIUSTWZPMYGG-UHFFFAOYSA-L disodium;2,2-dioctyl-3-sulfobutanedioate Chemical compound [Na+].[Na+].CCCCCCCCC(C([O-])=O)(C(C([O-])=O)S(O)(=O)=O)CCCCCCCC YHAIUSTWZPMYGG-UHFFFAOYSA-L 0.000 description 1
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- NHOGGUYTANYCGQ-UHFFFAOYSA-N ethenoxybenzene Chemical compound C=COC1=CC=CC=C1 NHOGGUYTANYCGQ-UHFFFAOYSA-N 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- ZQZUENMXBZVXIZ-UHFFFAOYSA-N ethenyl tetradecanoate Chemical compound CCCCCCCCCCCCCC(=O)OC=C ZQZUENMXBZVXIZ-UHFFFAOYSA-N 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009408 flooring Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- MLDSWUBFGPXMOM-UHFFFAOYSA-M lithium;tetradecyl sulfate Chemical compound [Li+].CCCCCCCCCCCCCCOS([O-])(=O)=O MLDSWUBFGPXMOM-UHFFFAOYSA-M 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 125000005397 methacrylic acid ester group Chemical group 0.000 description 1
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- 150000005673 monoalkenes Chemical class 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- XNTUJOTWIMFEQS-UHFFFAOYSA-N octadecanoyl octadecaneperoxoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCCCCCCCC XNTUJOTWIMFEQS-UHFFFAOYSA-N 0.000 description 1
- SRSFOMHQIATOFV-UHFFFAOYSA-N octanoyl octaneperoxoate Chemical compound CCCCCCCC(=O)OOC(=O)CCCCCCC SRSFOMHQIATOFV-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 1
- ONQDVAFWWYYXHM-UHFFFAOYSA-M potassium lauryl sulfate Chemical compound [K+].CCCCCCCCCCCCOS([O-])(=O)=O ONQDVAFWWYYXHM-UHFFFAOYSA-M 0.000 description 1
- 229940116985 potassium lauryl sulfate Drugs 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- HSJXWMZKBLUOLQ-UHFFFAOYSA-M potassium;2-dodecylbenzenesulfonate Chemical compound [K+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HSJXWMZKBLUOLQ-UHFFFAOYSA-M 0.000 description 1
- DQFWABVCOIFBPO-UHFFFAOYSA-M potassium;tetradecyl sulfate Chemical compound [K+].CCCCCCCCCCCCCCOS([O-])(=O)=O DQFWABVCOIFBPO-UHFFFAOYSA-M 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- MWZFQMUXPSUDJQ-KVVVOXFISA-M sodium;[(z)-octadec-9-enyl] sulfate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCCOS([O-])(=O)=O MWZFQMUXPSUDJQ-KVVVOXFISA-M 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
Description
本発明は、ペースト加工に適した塩化ビニル系樹脂に関するものであり、特に発泡印刷層がシャープな立体感を有し、ロータリースクリーン印刷壁紙用として優れた特性を有するペースト加工用として優れるペースト塩化ビニル系樹脂に関するものである。 The present invention relates to a vinyl chloride resin suitable for paste processing, and in particular, the foamed printed layer has a sharp three-dimensional effect, and has excellent properties for rotary screen printing wallpaper. Paste vinyl chloride excellent for paste processing. It relates to system resins.
ペースト塩化ビニル系樹脂（以下、ペースト塩ビと略記する場合もある。）は、一般に可塑剤、充填剤、安定剤又はその他の配合剤などと共に混練することにより、ペースト塩ビゾルを調製し、該ペースト塩ビゾルを使用し種々の成形加工法により壁紙、タイルカーペット、手袋などの様々な成形加工品に用いられている。 Paste vinyl chloride resin (hereinafter sometimes abbreviated as paste vinyl chloride) is generally kneaded with a plasticizer, a filler, a stabilizer or other compounding agents to prepare a paste vinyl chloride sol, and the paste It is used for various molded products such as wallpaper, tile carpet, and gloves by various molding methods using vinyl chloride sol.
特に壁紙等の意匠性を要求される分野においては、塩化ビニル系のペースト樹脂を用いたロータリースクリーン印刷法が種々検討されている。しかしながら、この塩化ビニル系のペースト樹脂、その組成物は、例えば、柄保型性等の点で不十分な場合があるなど、かならずしも充分満足し得るロータリー印刷特性を有するものではなく、例えば、特定のせん断粘度においてレベリング性、印刷模様のシャープ性、保形性、高速印刷性等の印刷用組成物としての基本性能に優れるロータリースクリーン印刷用ペーストゾル組成物が提案されている（例えば特許文献１参照。）。 In particular, in fields such as wall paper, which require designability, various rotary screen printing methods using vinyl chloride-based paste resins have been studied. However, this vinyl chloride-based paste resin and its composition do not necessarily have sufficiently satisfactory rotary printing characteristics, for example, in some cases, such as insufficient pattern retention. There has been proposed a paste-sol composition for rotary screen printing which is excellent in basic performance as a printing composition such as leveling property, sharpness of printed pattern, shape retention property, and high-speed printing property at shear viscosity of reference.).
しかし、特許文献１の提案においては、塩化ビニル系のペースト用樹脂とブレンディング樹脂のペーストゾル組成物を提案するものであり、壁紙用、特にロータリースクリーン印刷壁紙用としてのペースト塩ビについては何ら検討のなされていないものであった。 However, in the proposal of Patent Document 1, a paste sol composition of a vinyl chloride-based paste resin and a blending resin is proposed, and paste vinyl chloride for wallpaper, especially for rotary screen printing wallpaper, has not been studied at all. It had not been done.
そこで、本発明は、発泡印刷層として適用した際にシャープな立体感を発現し、特にロータリースクリーン印刷壁紙用として優れた性能を発揮するペースト塩化ビニル系樹脂を提供することにある。 Accordingly, it is an object of the present invention to provide a paste vinyl chloride resin that exhibits a sharp three-dimensional effect when applied as a foamed printed layer, and exhibits particularly excellent performance as a wallpaper for rotary screen printing.
本発明者は、上記の課題について鋭意検討を重ねた結果、特定の特性を有し、特定の配合を有するペースト塩化ビニル系樹脂が、ペースト塩ビゾルとして発泡壁紙に適用した際に発泡印刷層がシャープな立体感を有し、ロータリースクリーン印刷壁紙用として優れた特性を有することを見出し、本発明を完成させるに至った。 As a result of intensive studies on the above problems, the inventors of the present invention have found that when a paste vinyl chloride-based resin having specific properties and a specific formulation is applied as a paste vinyl chloride sol to a foamed wallpaper, the foamed printed layer is formed. The inventors have found that it has a sharp three-dimensional effect and excellent properties for rotary screen printing wallpaper, and have completed the present invention.
以下、本発明に関し詳細に説明する。 The present invention will be described in detail below.
本発明は、平均重合度７００～１５００の塩化ビニル系樹脂１００重量部に対して、アルキル硫酸エステル塩０．５～２重量部、アルキルベンゼンスルホン酸塩０．０５～０．５重量部を含み、下記条件１にて測定した際の平均粒子径が２～１００μｍ、粒子径０．０１～５μｍの範囲の粒子成分が２０～６０ｖｏｌ％、５～２００μｍの粒子成分が４０～８０ｖｏｌ％である、ことを特徴とするペースト塩化ビニル系樹脂及びその製造方法に関するものである。
条件１；ペースト塩化ビニル系樹脂１００重量部に対し、フタル酸ジイソノニル６０重量部を配合し、ペースト塩化ビニル系樹脂ゾルを調製し、２３℃、２時間保管後にレーザー回折・散乱法にて粒子径分布を測定。
The present invention contains 0.5 to 2 parts by weight of an alkyl sulfate and 0.05 to 0.5 parts by weight of an alkylbenzenesulfonate with respect to 100 parts by weight of a vinyl chloride resin having an average degree of polymerization of 700 to 1500, The average particle size when measured under condition 1 below is 2 to 100 μm, the particle component with a particle size of 0.01 to 5 μm is 20 to 60 vol%, and the particle component with a particle size of 5 to 200 μm is 40 to 80 vol%. It relates to a paste vinyl chloride resin characterized by and a method for producing the same.
Condition 1: 60 parts by weight of diisononyl phthalate is blended with 100 parts by weight of paste vinyl chloride resin to prepare a paste vinyl chloride resin sol, which is stored at 23° C. for 2 hours, and then the particle size is determined by laser diffraction/scattering method. Measure distribution.
本発明のペースト塩化ビニル系樹脂における塩化ビニル系樹脂は、平均重合度が７００～１５００のものであり、特に艶消しと表面平滑性に優れるとの効果を奏するものとなることから平均重合度９００～１４００のものであることが好ましく、更に１０００～１３００のものであることが好ましい。ここで、平均重合度が７００未満である場合、艶消し性に劣るものとなる。一方、重合度が１５００を越えるものである場合、表面平滑性、発泡シャープ性に劣るものとなる。なお、塩化ビニル系樹脂の平均重合度の測定方法としては、例えばＪＩＳ Ｋ６７２１のウベローデ粘度計を用いて、溶液粘度測定法により重合度として算出する方法を挙げることができる。 The vinyl chloride-based resin in the paste vinyl chloride-based resin of the present invention has an average degree of polymerization of 700 to 1,500. It is preferably from 1,400 to 1,400, more preferably from 1,000 to 1,300. Here, when the average degree of polymerization is less than 700, the matting property is inferior. On the other hand, if the degree of polymerization exceeds 1500, the surface smoothness and foaming sharpness will be inferior. As a method for measuring the average degree of polymerization of the vinyl chloride resin, for example, a method of calculating the degree of polymerization by a solution viscosity measurement method using an Ubbelohde viscometer according to JIS K6721 can be mentioned.
本発明のペースト塩化ビニル系樹脂はアルキルベンゼンスルホン酸塩を含有するものであり、その際のアルキルベンゼンスルホン酸塩としてはその範疇に属するものであれば如何なるものであってもよく、例えばドデシルベンゼンスルホン酸ナトリウム、ドデシルベンゼンスルホン酸カリウム、ドデシルベンゼンスルホン酸アンモニウム、ドデシルベンゼンスルホン酸トリエタノールアンモニウム等を挙げることができ、中でも特に表面平滑性に優れるペースト塩化ビニル系樹脂となることからドデシルベンゼンスルホン酸ナトリウムであることが好ましい。 The paste vinyl chloride resin of the present invention contains an alkylbenzenesulfonate, and the alkylbenzenesulfonate in this case may be any one that belongs to that category, such as dodecylbenzenesulfonic acid. sodium, potassium dodecylbenzenesulfonate, ammonium dodecylbenzenesulfonate, triethanolammonium dodecylbenzenesulfonate, and the like. Preferably.
アルキルベンゼンスルホン酸塩の配合量としては、塩化ビニル系樹脂１００重量部に対して０．０５～０．５重量部であり、特に表面平滑性に優れるものとなることから０．０７～０．３重量部であることが好ましく、更に０．０９～０．２重量部を含むものであることが好ましい。そして、該アルキルベンゼンスルホン酸塩は、塩化ビニル系樹脂を得る際の乳化剤であってもよく、塩化ビニル系樹脂の調製時の乳化剤をそのまま、または別途添加・減量することにより添加量を調整したものであってもよい。ここで、アルキルベンゼンスルホン酸塩が０．０５重量部未満である場合、表面平滑性に劣るものとなる。一方、０．５重量部を越える場合、発泡シャープ性に劣るものとなる。 The amount of the alkylbenzene sulfonate compounded is 0.05 to 0.5 parts by weight with respect to 100 parts by weight of the vinyl chloride resin, and is 0.07 to 0.3 because the surface smoothness is particularly excellent. It is preferably part by weight, more preferably 0.09 to 0.2 part by weight. The alkyl benzene sulfonate may be an emulsifier used in obtaining the vinyl chloride resin, or the emulsifier used in the preparation of the vinyl chloride resin may be used as it is, or the added amount may be adjusted by adding or reducing the amount. may be Here, when the alkylbenzenesulfonate is less than 0.05 parts by weight, the surface smoothness is poor. On the other hand, if the amount exceeds 0.5 parts by weight, the foaming sharpness will be poor.
本発明のペースト塩化ビニル系樹脂はアルキル硫酸エステル塩を含有するものであり、その際のアルキル硫酸エステル塩としてはその範疇に属するものであればよく、中でも、全炭素数が１０～１４のアルキル硫酸エステル塩であることが好ましく、例えば、ラウリル硫酸リチウム、ラウリル硫酸カリウム、ラウリル硫酸ナトリウム、ラウリル硫酸アンモニウム、ラウリル硫酸トリエタノールアンモニウム等のラウリル硫酸塩；オレイル硫酸リチウム、オレイル硫酸カリウム、オレイル硫酸ナトリウム、オレイル硫酸アンモニウム、オレイル硫酸トリエタノールアンモニウム等のオレイル硫酸塩；ミリスチル硫酸リチウム、ミリスチル硫酸カリウム、ミリスチル硫酸ナトリウム、ミリスチル硫酸アンモニウム、ミリスチル硫酸トリエタノールアンモニウム等のミリスチル硫酸塩、等が挙げられ、特にラウリル硫酸リチウム、ラウリル硫酸カリウム、ラウリル硫酸ナトリウム、ラウリル硫酸アンモニウム、ラウリル硫酸トリエタノールアンモニウム等のラウリル硫酸エステル塩であることが好ましい。 The paste vinyl chloride-based resin of the present invention contains an alkyl sulfate ester salt. Sulfuric ester salts are preferred, for example, lauryl sulfates such as lithium lauryl sulfate, potassium lauryl sulfate, sodium lauryl sulfate, ammonium lauryl sulfate, and triethanolammonium lauryl sulfate; lithium oleyl sulfate, potassium oleyl sulfate, sodium oleyl sulfate, oleyl oleyl sulfates such as ammonium sulfate and triethanolammonium oleyl sulfate; myristyl sulfates such as lithium myristyl sulfate, potassium myristyl sulfate, sodium myristyl sulfate, ammonium myristyl sulfate, and triethanolammonium myristyl sulfate; Lauryl sulfate salts such as potassium sulfate, sodium lauryl sulfate, ammonium lauryl sulfate and triethanolammonium lauryl sulfate are preferred.
アルキル硫酸エステル塩の配合量としては、塩化ビニル系樹脂１００重量部に対して、０．５～２重量部を含むものであり、特に表面平滑性、発泡シャープ性に優れるものとなることから０．６～１．５重量部であることが好ましく、更に０．６～１重量部を含むものであることが好ましい。そして、該アルキル硫酸エステル塩は、塩化ビニル系樹脂を得る際の乳化剤であってもよく、塩化ビニル系樹脂の調製時の乳化剤をそのまま、または別途添加・減量することにより添加量を調整したものであってもよい。ここで、アルキル硫酸エステル塩が０．５重量部未満である場合、表面平滑性に劣るものとなる。一方、２重量部を越える場合、表面平滑性、発泡シャープ性に劣るものとなる。 The amount of the alkyl sulfate ester salt to be blended is 0.5 to 2 parts by weight per 100 parts by weight of the vinyl chloride resin. .6 to 1.5 parts by weight, preferably 0.6 to 1 part by weight. The alkyl sulfate ester salt may be an emulsifier used in obtaining the vinyl chloride resin, or the emulsifier used in the preparation of the vinyl chloride resin may be used as it is, or the amount added may be adjusted by adding or reducing the amount. may be Here, if the amount of the alkyl sulfate is less than 0.5 parts by weight, the surface smoothness is poor. On the other hand, if it exceeds 2 parts by weight, the surface smoothness and foaming sharpness will be inferior.
本発明のペースト塩化ビニル系樹脂は、該ペースト塩化ビニル系樹脂１００重量部に対し、可塑剤としてフタル酸ジイソノニル６０重量部を配合し、ペースト塩ビゾルを調製し、２３℃、２時間保管後にレーザー回折・散乱法により粒子径分布を測定した際に、該ペースト塩ビゾル中の平均粒子径が２～１００μｍであり、特に２～５０μｍ、更に３～２０μｍであることが好ましい。ここで、ペースト塩ビゾル中の平均粒子径が２μｍ未満である場合、経時のゾル粘度が上昇し加工性が低下するものとなる。一方、１００μｍを超えるものであるとスクリーンメッシュに詰まりを生じるものとなる。また、ペースト塩ビゾルにおける粒子径分布として、粒子径０．０１～５μｍの範囲内の粒子成分（以下、Ａ成分と記す場合がある。）が２０～６０ｖｏｌ％、５～２００μｍの粒子成分（以下、Ｂ成分と記す場合がある。）が４０～８０ｖｏｌ％となるものである。ここで、A成分又はB成分がこれらの範囲外である場合、発泡シャープ性に劣るものとなる。なお、ペースト塩ビゾル中の粒子径分布を測定する際のレーザー回折・散乱法粒度分布測定装置は、粒子径分布の測定が可能であればいかなるものを用いることも可能である。 The paste vinyl chloride resin of the present invention is prepared by blending 60 parts by weight of diisononyl phthalate as a plasticizer with 100 parts by weight of the paste vinyl chloride resin to prepare a paste vinyl chloride sol. When the particle size distribution is measured by a diffraction/scattering method, the paste vinyl chloride sol has an average particle size of 2 to 100 μm, preferably 2 to 50 μm, more preferably 3 to 20 μm. Here, if the average particle size in the paste vinyl chloride sol is less than 2 μm, the sol viscosity increases over time and the workability decreases. On the other hand, if it exceeds 100 μm, the screen mesh will be clogged. In addition, as the particle size distribution in the paste vinyl chloride sol, the particle component with a particle size of 0.01 to 5 μm (hereinafter sometimes referred to as component A) is 20 to 60 vol%, and the particle component with a particle size of 5 to 200 μm (hereinafter , sometimes referred to as B component.) is 40 to 80 vol%. Here, if the A component or the B component is out of these ranges, the foaming sharpness will be inferior. Any laser diffraction/scattering particle size distribution measuring apparatus for measuring the particle size distribution in the paste vinyl chloride sol can be used as long as the particle size distribution can be measured.
本発明のペースト塩化ビニル系樹脂を構成する塩化ビニル系樹脂としては、塩化ビニル単独重合体はもとより、共重合体であってもよくその際の共重合可能な単量体としては、例えば酢酸ビニル、プロピオン酸ビニル、ミリスチン酸ビニル、安息香酸ビニル等のビニルエステル類；アクリル酸、メタクリル酸、マレイン酸、フマル酸等の不飽和カルボン酸またはその無水物；アクリル酸メチル、アクリル酸エチル、アクリル酸ブチル等のアクリル酸エステル類；メタクリル酸メチル、メタクリル酸エチル、メタクリル酸ブチル等のメタクリル酸エステル類；マレイン酸エステル、フマル酸エステル、桂皮酸エステル類等の不飽和カルボン酸エステル類；ビニルメチルエーテル、ビニルアミルエーテル、ビニルフェニルエーテル等のビニルエーテル類；エチレン、プロピレン、ブテン、ペンテン等のモノオレフィン類；塩化ビニリデン、スチレン及びその誘導体、アクリロニトリル、メタクリロニトリル等を挙げることができる。 The vinyl chloride-based resin constituting the paste vinyl chloride-based resin of the present invention may be not only a vinyl chloride homopolymer but also a copolymer. , vinyl propionate, vinyl myristate, vinyl esters such as vinyl benzoate; unsaturated carboxylic acids such as acrylic acid, methacrylic acid, maleic acid, fumaric acid or their anhydrides; methyl acrylate, ethyl acrylate, acrylic acid Acrylic acid esters such as butyl; Methacrylic acid esters such as methyl methacrylate, ethyl methacrylate and butyl methacrylate; Unsaturated carboxylic acid esters such as maleic acid ester, fumaric acid ester and cinnamic acid ester; Vinyl methyl ether , vinyl amyl ether and vinyl phenyl ether; monoolefins such as ethylene, propylene, butene and pentene; vinylidene chloride, styrene and derivatives thereof, acrylonitrile and methacrylonitrile.
塩化ビニル系樹脂は、ペースト塩化ビニル系樹脂の一般的な重合法として知られている乳化重合法、ミクロ懸濁重合法、シード乳化重合法、シードミクロ懸濁重合法等により得られる塩化ビニル系樹脂であってもよく、これら重合法により塩化ビニル系樹脂ラテックスを得て、得られたラテックスの水分を除去することにより樹脂又はその粒子として得ることができる。その際に、塩化ビニル系樹脂ラテックスから水分を除去する方法としては、例えば噴霧乾燥、流動層乾燥、通気乾燥、回転乾燥、伝導加熱乾燥による方法等が挙げられ、中でも、効率よく水分を除去できることから、噴霧乾燥による方法が好ましい。 Vinyl chloride resins are vinyl chloride resins obtained by emulsion polymerization, microsuspension polymerization, seed emulsion polymerization, seed microsuspension polymerization, etc., which are known as general polymerization methods for paste vinyl chloride resins. It may be a resin, and it can be obtained as a resin or particles thereof by obtaining a vinyl chloride resin latex by these polymerization methods and removing water from the obtained latex. At that time, the method for removing water from the vinyl chloride resin latex includes, for example, spray drying, fluidized bed drying, aeration drying, rotary drying, conduction heating drying, etc. Among them, water should be efficiently removed. Therefore, the spray drying method is preferred.
以下に、該塩化ビニル系樹脂、塩化ビニル系樹脂ラテックスを製造する際の一例として、シードミクロ懸濁重合法による方法を示す。 As an example of the production of the vinyl chloride resin and vinyl chloride resin latex, a seed microsuspension polymerization method is shown below.
シードミクロ懸濁重合法とは、１）ミクロ懸濁重合法により油溶性重合開始剤を含む塩化ビニル系樹脂を含有する塩化ビニル系樹脂シードラテックスを得る第一段階、２）得られたシードラテックスを塩化ビニルモノマー、又は塩化ビニルモノマーとこれと共重合可能な単量体を、脱イオン水、乳化剤、緩衝剤、必要に応じて高級アルコール等の乳化助剤の存在下で緩やかな攪拌で重合を行い、シードラテックスを肥大化させて塩化ビニル系樹脂ラテックスを得る第二段階からなる重合方法である。 The seed microsuspension polymerization method includes 1) the first step of obtaining a vinyl chloride resin seed latex containing a vinyl chloride resin containing an oil-soluble polymerization initiator by the microsuspension polymerization method, and 2) the obtained seed latex. A vinyl chloride monomer, or a vinyl chloride monomer and a monomer copolymerizable therewith, are polymerized with gentle stirring in the presence of deionized water, an emulsifier, a buffer, and, if necessary, an emulsifying aid such as a higher alcohol. and enlarging the seed latex to obtain a vinyl chloride resin latex.
ここで、塩化ビニルモノマーと共重合可能な単量体としては、上記した単量体を例示することができる。また、乳化剤としては、上記したアルキルベンゼンスルホン酸塩、アルキル硫酸エステル塩以外に、例えばジオクチルスルホコハク酸ナトリウム塩、ジヘキシルスルホコハク酸ナトリウム塩等のスルホコハク酸塩類；ポリオキシエチレンアルキル硫酸エステル塩類、ポリオキシエチレンアルキルアリール硫酸エステル塩類等のアニオン系乳化剤，ソルビタンモノオレート、ポリオキシエチレンソルビタンモノステアレート等のソルビタンエステル類；ポリオキシエチレンアルキルフェニルエーテル類、ポリオキシエチレンアルキルエステル類等のノニオン系乳化剤等の従来より知られているものを１種類又は２種類以上用いることができる。緩衝剤としては、例えばリン酸一水素アルカリ金属塩、リン酸二水素アルカリ金属塩、フタル酸水素カリウム、炭酸水素ナトリウム、ホウ酸－苛性カリウム溶液等が挙げられる。 Here, the above-described monomers can be exemplified as the monomer copolymerizable with the vinyl chloride monomer. As emulsifiers, in addition to the alkylbenzenesulfonates and alkyl sulfates mentioned above, sulfosuccinates such as sodium dioctylsulfosuccinate and sodium dihexylsulfosuccinate; polyoxyethylene alkyl sulfates, polyoxyethylene alkyl Anionic emulsifiers such as aryl sulfate ester salts, sorbitan esters such as sorbitan monooleate and polyoxyethylene sorbitan monostearate; nonionic emulsifiers such as polyoxyethylene alkylphenyl ethers and polyoxyethylene alkyl esters. One type or two or more types of known materials can be used. Examples of buffering agents include alkali metal monohydrogen phosphate, alkali metal dihydrogen phosphate, potassium hydrogen phthalate, sodium hydrogen carbonate, boric acid-caustic potassium solution and the like.
さらに、必要に応じて用いられる乳化助剤としては、例えばセチルアルコール、ラウリルアルコール等の高級アルコール；ラウリン酸、パルミチン酸、ステアリン酸等の高級脂肪酸、そのエステル；芳香族炭化水素、高級脂肪酸炭化水素、塩素化パラフィンのようなハロゲン化炭化水素等が挙げられる。 Furthermore, emulsifying aids used as necessary include, for example, higher alcohols such as cetyl alcohol and lauryl alcohol; higher fatty acids such as lauric acid, palmitic acid and stearic acid, esters thereof; aromatic hydrocarbons and higher fatty acid hydrocarbons. , halogenated hydrocarbons such as chlorinated paraffins, and the like.
また、シードミクロ懸濁重合法に用いられる塩化ビニル系樹脂シードラテックスは、以下のようなミクロ懸濁重合法で調製することが可能である。まず、塩化ビニルモノマー、油溶性重合開始剤、界面活性剤、緩衝剤、高級アルコール、高級脂肪酸、高級脂肪酸エステル、塩素化パラフィン等の分散助剤、必要に応じて重合度調整剤を添加してプレミックスし、ホモジナイザーにより均質化処理して油滴の調整を行なう。この際のホモジナイザーとしては、例えば、コロイドミル、振動攪拌機、二段式高圧ポンプ等を用いることができる。そして、均質化処理した液を重合器に送り、緩やかに攪拌しながら重合器内の温度を上げて重合反応を開始し、所定の転化率に達するまで重合を行なうことにより油溶性重合開始剤を含有する塩化ビニル系樹脂シードラテックスを調製することが可能である。 Also, the vinyl chloride resin seed latex used in the seed microsuspension polymerization method can be prepared by the following microsuspension polymerization method. First, vinyl chloride monomers, oil-soluble polymerization initiators, surfactants, buffers, higher alcohols, higher fatty acids, higher fatty acid esters, dispersing aids such as chlorinated paraffin, and, if necessary, polymerization degree adjusters are added. The oil droplets are adjusted by premixing and homogenizing with a homogenizer. As a homogenizer at this time, for example, a colloid mill, a vibration stirrer, a two-stage high-pressure pump, or the like can be used. Then, the homogenized liquid is sent to the polymerization vessel, and the temperature inside the polymerization vessel is raised while gently stirring to initiate the polymerization reaction. It is possible to prepare a vinyl chloride-based resin seed latex containing.
その際の油溶性重合開始剤としては、１０時間半減期温度３０～７０℃のジアシルパーオキサイドが好ましく、そのような油溶性重合開始剤としては、例えばイソブチリルパーオキサイド、３，３，５－トリメチルヘキサノイルパーオキサイド、オクタノイルパーオキサイド、ラウロイルパーオキサイド、ステアロイルパーオキサイド、コハク酸パーオキサイド等が挙げられる。 As the oil-soluble polymerization initiator at that time, diacyl peroxide having a 10-hour half-life temperature of 30 to 70° C. is preferable. trimethylhexanoyl peroxide, octanoyl peroxide, lauroyl peroxide, stearoyl peroxide, succinic acid peroxide and the like.
そして、該塩化ビニル系樹脂ラテックスを噴霧乾燥することにより、場合によっては１次粒子又はその集合体である粒子をペースト塩化ビニル系樹脂として得ることができる。また、集合体である粒子は、必要に応じて粉砕したものであってもよい。ペースト塩化ビニル系樹脂とする際に用いる乾燥機は一般的に使用されているものでよく、例えば、「ＳＰＲＡＹ ＤＲＹＩＮＧ ＨＡＮＤＢＯＯＫ」（Ｋ．Ｍａｓｔｅｒｓ著、３版、１９７９年、ＧｅｏｒｇｅｇｏｄｗｉｎＬｉｍｉｔｅｄより出版）の１２１頁第４．１０図に記載されている各種の噴霧乾燥機を挙げることができる。その際の乾燥用空気入口温度、乾燥用空気出口温度に特に制限はなく、中でも、ペースト塩化ビニル系樹脂を効率的に製造することが可能となると共にロータリースクリーン印刷壁紙用として優れた特性、発泡シャープ性を有するものとなることから、乾燥用空気入口温度は１６０～２３０℃、乾燥用空気出口温度は６０～７０℃であることが好ましい。 By spray-drying the vinyl chloride resin latex, primary particles or aggregate particles thereof can be obtained as paste vinyl chloride resin in some cases. Moreover, the aggregated particles may be pulverized as necessary. A commonly used dryer may be used for the paste vinyl chloride-based resin. The various spray dryers described in Figure 4.10 may be mentioned. At that time, there are no particular restrictions on the drying air inlet temperature and the drying air outlet temperature. It is preferable that the drying air inlet temperature is 160 to 230° C. and the drying air outlet temperature is 60 to 70° C., since sharpness is obtained.
本発明のペースト塩化ビニル系樹脂は、可塑剤、充填剤、顔料、発泡剤、希釈剤、安定剤等を配合することにより、成形加工性に優れるペースト塩ビゾルとすることが可能となり、フィルム、シート、壁紙、床材、発泡シート等の各種用途に適用可能であり、表面平滑性、表面強度、発泡性等の要求される発泡壁紙用、特にロータリースクリーン印刷壁紙用として適したものとなる。 The paste vinyl chloride resin of the present invention can be made into a paste vinyl chloride sol having excellent molding processability by blending a plasticizer, a filler, a pigment, a foaming agent, a diluent, a stabilizer, and the like. It can be applied to various uses such as sheets, wallpapers, flooring materials, and foamed sheets, and is suitable for foamed wallpapers that require surface smoothness, surface strength, foamability, etc., especially for rotary screen printing wallpapers.
本発明のペースト塩化ビニル系樹脂は、表面平滑性、発泡印刷シャープ性に優れる発泡体を提供することが可能であり、発泡壁紙用、特にロータリースクリーン印刷壁紙用として適しており、その工業的価値は非常に高いものである。 INDUSTRIAL APPLICABILITY The paste vinyl chloride-based resin of the present invention can provide a foam having excellent surface smoothness and foam printing sharpness, and is suitable for foam wallpaper, particularly for rotary screen printing wallpaper, and its industrial value. is very high.
以下に、実施例より得られたペースト塩化ビニル系樹脂の評価方法を示す。 Methods for evaluating paste vinyl chloride resins obtained in Examples are shown below.
＜塩化ビニル系樹脂の重合度＞
ＪＩＳ Ｋ６７２１のウベローデ粘度計を用いて、溶液粘度測定法により重合度を算出した。
<Polymerization degree of vinyl chloride resin>
The degree of polymerization was calculated by the solution viscosity measuring method using an Ubbelohde viscometer of JIS K6721.
＜ペースト塩ビゾル中の粒子径分布の測定＞
ペースト塩化ビニル系樹脂１００重量部に対し、フタル酸ジイソノニル６０重量部を配合し、ペースト塩ビゾルを調製し、２３℃、２時間保管した。その後、ＰＩＤＳ濃度が４０～５０％となるように濃度調整を行い、レーザー回析／散乱法 粒径測定装置（（商品名）ＬＳ１３３２０、ベックマン・コールター（株）製）にて、粒子径分布測定を行うと共に平均粒子径を算出した。
<Measurement of particle size distribution in paste vinyl chloride sol>
A paste vinyl chloride sol was prepared by blending 60 parts by weight of diisononyl phthalate with 100 parts by weight of paste vinyl chloride resin, and stored at 23° C. for 2 hours. After that, the concentration is adjusted so that the PIDS concentration is 40 to 50%, and the particle size distribution is measured with a laser diffraction/scattering method particle size measuring device ((trade name) LS13320, manufactured by Beckman Coulter, Inc.). and calculated the average particle size.
＜発泡倍率＞
得られたペースト塩化ビニル系樹脂を発泡体として以下の（１）式により算出した。
発泡倍率＝（発泡体の厚み－原反の厚み）／原反の厚み （１）
＜表面平滑性＞
得られた発泡体の表面を観察し評価した
○：表面が平滑。
×：表面が粗い。
<Expansion ratio>
The resulting paste vinyl chloride-based resin was used as a foam and calculated according to the following formula (1).
Foaming ratio = (thickness of foam - thickness of original fabric) / thickness of original fabric (1)
<Surface smoothness>
The surface of the obtained foam was observed and evaluated. Good: The surface is smooth.
x: The surface is rough.
＜発泡シャープ性＞
得られた発泡体のエンボス性を観察し評価した。
エンボス性の評価基準を以下に示す。
○：互いに接する凹凸面の角度が５０度以上９０度未満。
×：互いに接する凹凸面の角度が５０度未満又は９０度以上。
<Foam sharpness>
The embossability of the resulting foam was observed and evaluated.
Embossability evaluation criteria are shown below.
○: The angle of the uneven surfaces in contact with each other is 50 degrees or more and less than 90 degrees.
x: The angle of the uneven surfaces in contact with each other is less than 50 degrees or 90 degrees or more.
合成例１
１ｍ３ステンレス製オートクレーブに脱イオン水３６０ｋｇ、塩化ビニルモノマー３００ｋｇ、過酸化ラウロイル５．７ｋｇ及び１５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液３０ｋｇを仕込み、ホモジナイザーを用いて３時間循環し均質化処理を行なった後、反応系の温度を４５℃に上げて重合を開始した。重合系の圧力が低下した後、未反応塩化ビニルモノマーを回収し、固形分含有率３５重量％、平均粒子径０．５５μｍ、塩化ビニル系樹脂に対して２重量％の過酸化ラウロイルを含有する塩化ビニル系樹脂シードラテックス（ａ）を得た。
Synthesis example 1
A 1 m 3 stainless steel autoclave was charged with 360 kg of deionized water, 300 kg of vinyl chloride monomer, 5.7 kg of lauroyl peroxide, and 30 kg of a 15% by weight sodium dodecylbenzenesulfonate aqueous solution, and homogenized by circulating for 3 hours using a homogenizer. After that, the temperature of the reaction system was raised to 45° C. to initiate polymerization. After the pressure of the polymerization system is lowered, the unreacted vinyl chloride monomer is recovered, and the solid content is 35% by weight, the average particle size is 0.55 μm, and lauroyl peroxide is contained in an amount of 2% by weight based on the vinyl chloride resin. A vinyl chloride resin seed latex (a) was obtained.
合成例２
１ｍ３ステンレス製オートクレーブに脱イオン水４００ｋｇ、塩化ビニルモノマー３５０ｋｇ、１６重量％ラウリン酸カリウム水溶液２ｋｇ及び１６重量％ドデシルベンゼンスルホン酸ナトリウム水溶液５ｋｇを仕込み、反応系の温度を６０℃に上げて重合を開始した。重合系の圧力が低下した後、未反応塩化ビニルモノマーを回収し、固形分含有率４０重量％、平均粒子径０．１５μｍである塩化ビニル系樹脂シードラテックス（ｂ）を得た。
Synthesis example 2
400 kg of deionized water, 350 kg of vinyl chloride monomer, 2 kg of 16% by weight potassium laurate aqueous solution and 5 kg of 16% by weight sodium dodecylbenzenesulfonate aqueous solution were charged in a 1 m 3 stainless steel autoclave, and the temperature of the reaction system was raised to 60°C to initiate polymerization. started. After the pressure of the polymerization system was lowered, the unreacted vinyl chloride monomer was recovered to obtain a vinyl chloride resin seed latex (b) having a solid content of 40% by weight and an average particle size of 0.15 μm.
実施例１
２．５Ｌステンレス製オートクレーブに脱イオン水６１０ｇ、塩化ビニルモノマー７３０ｇ、５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液１５ｇ、合成例１により得られた平均粒子径０．５５μｍのシードラテックス（ａ）を塩化ビニルモノマー１００重量部に対し４重量部、合成例２により得られた平均粒子径０．１５μｍのシードラテックス（ｂ）を塩化ビニルモノマー１００重量部に対し５重量部仕込み、この反応混合物の温度を５４℃に上げて重合を開始した。重合を開始してから重合を終了までの間、塩化ビニルモノマーに対し０．７重量部の５重量％ラウリル硫酸ナトリウム水溶液を連続的に添加した。重合圧が５４℃における塩化ビニルモノマーの飽和蒸気圧から０．３７ＭＰａまで降下したときに重合を停止し、未反応塩化ビニルモノマーを回収し、塩化ビニル系樹脂ラテックスを得た。
Example 1
610 g of deionized water, 730 g of a vinyl chloride monomer, 15 g of a 5% by weight sodium dodecylbenzenesulfonate aqueous solution, seed latex (a) having an average particle size of 0.55 μm obtained in Synthesis Example 1 was added to a 2.5 L stainless steel autoclave. 4 parts by weight per 100 parts by weight of the monomer, and 5 parts by weight of the seed latex (b) having an average particle size of 0.15 μm obtained in Synthesis Example 2 were charged per 100 parts by weight of the vinyl chloride monomer, and the reaction mixture was heated to 54 parts by weight. °C to initiate polymerization. From the start of polymerization to the end of polymerization, 0.7 parts by weight of a 5% by weight sodium lauryl sulfate aqueous solution was continuously added to the vinyl chloride monomer. When the polymerization pressure dropped from the saturated vapor pressure of the vinyl chloride monomer at 54° C. to 0.37 MPa, the polymerization was stopped and the unreacted vinyl chloride monomer was recovered to obtain a vinyl chloride resin latex.
得られた塩化ビニル系樹脂ラテックス１ｋｇを、回転円盤式のスプレードライヤーを用い、熱風温度２１０℃、出口温度６５℃で噴霧乾燥し、ペースト塩化ビニル系樹脂を得た。得られたペースト塩化ビニル系樹脂は、塩化ビニル系樹脂１００重量部に対しドデシルベンゼンスルホン酸ナトリウム０．１重量部、ラウリル硫酸ナトリウム０．８重量部を含むものであった。また、塩化ビニル樹脂の重合度は１１００であり、フタル酸ジイソノニル６０重量部を配合し、調製したペースト塩ビゾルの粒子径分布における平均粒子径は９．９μｍであり、粒子径０．０１～５μｍの範囲の粒子成分４０ｖｏｌ％、５～２００μｍの粒子成分６０ｖｏｌ％のものであった。 1 kg of the obtained vinyl chloride resin latex was spray-dried using a rotating disk type spray dryer at a hot air temperature of 210°C and an outlet temperature of 65°C to obtain a paste vinyl chloride resin. The resulting paste vinyl chloride resin contained 0.1 parts by weight of sodium dodecylbenzenesulfonate and 0.8 parts by weight of sodium lauryl sulfate with respect to 100 parts by weight of the vinyl chloride resin. The vinyl chloride resin has a polymerization degree of 1100, and the paste vinyl chloride sol prepared by blending 60 parts by weight of diisononyl phthalate has an average particle size of 9.9 μm in the particle size distribution, and a particle size of 0.01 to 5 μm. 40 vol % of the particle component in the range of 200 μm and 60 vol % of the particle component of 5 to 200 μm.
得られたペースト塩化ビニル系樹脂１００重量部に対し、可塑剤としてジイソノニルフタレート（（株）ジェイ・プラス、グレード工業用）５０重量部、充填剤として炭酸カルシウム（三共精粉（株）、グレード一級）４０重量部、顔料として酸化チタン（テイカ（株）、（商品名）ＪＲ６００Ａ）１０重量部、発泡剤（大塚化学（株）、（商品名）ＡＺウルトラ１０５０）３重量部、希釈剤（ＪＸ日鉱日石（株）、（商品名）Ｎ１０）１０重量部、安定剤（（株）アデカ、（商品名）ＦＬ－１０３Ｎ）３重量部を用い、ディゾルバーを用いて混練し、ペースト塩ビゾルを得た。 To 100 parts by weight of the resulting paste vinyl chloride resin, 50 parts by weight of diisononyl phthalate (J-Plus Co., Ltd., grade industrial use) as a plasticizer, and calcium carbonate (Sankyo Seifun Co., Ltd., grade 1 grade) as a filler. ) 40 parts by weight, 10 parts by weight of titanium oxide (Tayca Co., Ltd., (trade name) JR600A) as a pigment, foaming agent (Otsuka Chemical Co., Ltd., (trade name) AZ Ultra 1050) 3 parts by weight, diluent (JX Nikko Nisseki Co., Ltd., (trade name) N10) 10 parts by weight, stabilizer (Adeka Co., Ltd., (trade name) FL-103N) 3 parts by weight, kneaded using a dissolver to form a paste vinyl chloride sol Obtained.
得られたペースト塩ビゾルを、予め１８０℃で５秒加熱した難燃紙上に０．１４ｍｍの厚みでコーティングし、１９０℃で１０秒加熱することにより、原反を得た。 The resulting paste vinyl chloride sol was coated in a thickness of 0.14 mm on a flame-retardant paper heated at 180° C. for 5 seconds, and heated at 190° C. for 10 seconds to obtain a raw sheet.
得られた原反の厚みを測定した後、２１０℃で３５秒加熱することにより発泡体を得た。その後、得られた発泡体の厚みを測定し、発泡倍率、表面平滑性、発泡シャープ性を評価した。試験結果を表１に示す。発泡倍率は４．８倍であり、表面平滑性、発泡シャープ性に優れるものであった。 After measuring the thickness of the obtained original sheet, it was heated at 210° C. for 35 seconds to obtain a foam. After that, the thickness of the obtained foam was measured, and the expansion ratio, surface smoothness and foam sharpness were evaluated. Table 1 shows the test results. The foaming ratio was 4.8 times, and the surface smoothness and sharpness of foaming were excellent.
実施例２
２．５Ｌステンレス製オートクレーブに脱イオン水６１０ｇ、塩化ビニルモノマー７３０ｇ、５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液１５ｇ、合成例１により得られた平均粒子径０．５５μｍのシードラテックス（ａ）を塩化ビニルモノマー１００重量部に対し４重量部、合成例２により得られた平均粒子径０．１５μｍのシードラテックス（ｂ）を塩化ビニルモノマー１００重量部に対し５重量部仕込み、この反応混合物の温度を５４℃に上げて重合を開始した。重合を開始してから重合を終了までの間、塩化ビニルモノマーに対し０．７重量部の５重量％ラウリル硫酸ナトリウム水溶液を連続的に添加した。重合圧が５４℃における塩化ビニルモノマーの飽和蒸気圧から０．３７ＭＰａまで降下したときに重合を停止し、未反応塩化ビニルモノマーを回収し、塩化ビニル系樹脂ラテックスを得た。
Example 2
610 g of deionized water, 730 g of a vinyl chloride monomer, 15 g of a 5% by weight sodium dodecylbenzenesulfonate aqueous solution, seed latex (a) having an average particle size of 0.55 μm obtained in Synthesis Example 1 was added to a 2.5 L stainless steel autoclave. 4 parts by weight per 100 parts by weight of the monomer, and 5 parts by weight of the seed latex (b) having an average particle size of 0.15 μm obtained in Synthesis Example 2 were charged per 100 parts by weight of the vinyl chloride monomer, and the reaction mixture was heated to 54 parts by weight. °C to initiate polymerization. From the start of polymerization to the end of polymerization, 0.7 parts by weight of a 5% by weight sodium lauryl sulfate aqueous solution was continuously added to the vinyl chloride monomer. When the polymerization pressure dropped from the saturated vapor pressure of the vinyl chloride monomer at 54° C. to 0.37 MPa, the polymerization was stopped and the unreacted vinyl chloride monomer was recovered to obtain a vinyl chloride resin latex.
得られた塩化ビニル系樹脂ラテックス１ｋｇを、回転円盤式のスプレードライヤーを用い、熱風温度１９０℃、出口温度６０℃で噴霧乾燥し、ペースト塩化ビニル系樹脂を得た。得られたペースト塩化ビニル系樹脂は、塩化ビニル系樹脂１００重量部に対しドデシルベンゼンスルホン酸ナトリウム０．１重量部、ラウリル硫酸ナトリウム０．８重量部を含むものであった。また、塩化ビニル樹脂の重合度は１１００であり、フタル酸ジイソノニル６０重量部を配合し、調製したペースト塩ビゾルの粒子径分布における平均粒子径は５．０μｍであり、粒子径０．０１～５μｍの範囲の粒子成分５０ｖｏｌ％、５～２００μｍの粒子成分５０ｖｏｌ％のものであった。 1 kg of the obtained vinyl chloride resin latex was spray-dried using a rotating disc type spray dryer at a hot air temperature of 190°C and an outlet temperature of 60°C to obtain a paste vinyl chloride resin. The resulting paste vinyl chloride resin contained 0.1 parts by weight of sodium dodecylbenzenesulfonate and 0.8 parts by weight of sodium lauryl sulfate with respect to 100 parts by weight of the vinyl chloride resin. The vinyl chloride resin has a polymerization degree of 1100, and the paste vinyl chloride sol prepared by blending 60 parts by weight of diisononyl phthalate has an average particle size of 5.0 μm in the particle size distribution, and a particle size of 0.01 to 5 μm. 50 vol % of the particle component in the range of 50 vol % and 50 vol % of the particle component of 5 to 200 μm.
得られたペースト塩化ビニル系樹脂１００重量部に対し、可塑剤としてジイソノニルフタレート（（株）ジェイ・プラス、グレード工業用）５０重量部、充填剤として炭酸カルシウム（三共精粉（株）、グレード一級）４０重量部、顔料として酸化チタン（テイカ（株）、（商品名）ＪＲ６００Ａ）１０重量部、発泡剤（大塚化学（株）、（商品名）ＡＺウルトラ１０５０）３重量部、希釈剤（ＪＸ日鉱日石（株）、（商品名）Ｎ１０）１０重量部、安定剤（（株）アデカ、（商品名）ＦＬ－１０３Ｎ）３重量部を用い、ディゾルバーを用いて混練し、ペースト塩ビゾルを得た。 To 100 parts by weight of the resulting paste vinyl chloride resin, 50 parts by weight of diisononyl phthalate (J-Plus Co., Ltd., grade industrial use) as a plasticizer, and calcium carbonate (Sankyo Seifun Co., Ltd., grade 1 grade) as a filler. ) 40 parts by weight, 10 parts by weight of titanium oxide (Tayca Co., Ltd., (trade name) JR600A) as a pigment, foaming agent (Otsuka Chemical Co., Ltd., (trade name) AZ Ultra 1050) 3 parts by weight, diluent (JX Nikko Nisseki Co., Ltd., (trade name) N10) 10 parts by weight, stabilizer (Adeka Co., Ltd., (trade name) FL-103N) 3 parts by weight, kneaded using a dissolver to form a paste vinyl chloride sol Obtained.
得られたペースト塩ビゾルを、予め１８０℃で５秒加熱した難燃紙上に０．１４ｍｍの厚みでコーティングし、１９０℃で１０秒加熱することにより、原反を得た。 The resulting paste vinyl chloride sol was coated in a thickness of 0.14 mm on a flame-retardant paper heated at 180° C. for 5 seconds, and heated at 190° C. for 10 seconds to obtain a raw sheet.
得られた原反の厚みを測定した後、２１０℃で３５秒加熱することにより発泡体を得た。その後、得られた発泡体の厚みを測定し、発泡倍率、表面平滑性、発泡シャープ性を評価した。試験結果を表１に示す。発泡倍率は４．７倍であり、表面平滑性、発泡シャープ性に優れるものであった。 After measuring the thickness of the obtained original sheet, it was heated at 210° C. for 35 seconds to obtain a foam. After that, the thickness of the obtained foam was measured, and the expansion ratio, surface smoothness and foam sharpness were evaluated. Table 1 shows the test results. The foaming ratio was 4.7 times, and the surface smoothness and sharpness of foaming were excellent.
実施例３
２．５Ｌステンレス製オートクレーブに脱イオン水５００ｇ、塩化ビニルモノマー８００ｇ、５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液１５ｇ、合成例１により得られた平均粒子径０．５５μｍのシードラテックス（ａ）を塩化ビニルモノマー１００重量部に対し４重量部、合成例２により得られた平均粒子径０．１５μｍのシードラテックス（ｂ）を塩化ビニルモノマー１００重量部に対し５重量部仕込み、この反応混合物の温度を６４℃に上げて重合を開始した。重合を開始してから重合を終了までの間、塩化ビニルモノマーに対し０．７重量部の５重量％ラウリル硫酸ナトリウム水溶液を連続的に添加した。重合圧が６４℃における塩化ビニルモノマーの飽和蒸気圧から０．３８ＭＰａまで降下したときに重合を停止し、未反応塩化ビニルモノマーを回収し、塩化ビニル系樹脂ラテックスを得た。
Example 3
500 g of deionized water, 800 g of a vinyl chloride monomer, 15 g of a 5% by weight aqueous solution of sodium dodecylbenzenesulfonate, seed latex (a) having an average particle size of 0.55 μm obtained in Synthesis Example 1 was added to a 2.5 L stainless steel autoclave. 4 parts by weight per 100 parts by weight of the monomer, and 5 parts by weight of the seed latex (b) having an average particle size of 0.15 μm obtained in Synthesis Example 2 were charged per 100 parts by weight of the vinyl chloride monomer, and the reaction mixture was heated to 64 parts by weight. °C to initiate polymerization. From the start of polymerization to the end of polymerization, 0.7 parts by weight of a 5% by weight sodium lauryl sulfate aqueous solution was continuously added to the vinyl chloride monomer. When the polymerization pressure dropped from the saturated vapor pressure of the vinyl chloride monomer at 64° C. to 0.38 MPa, the polymerization was stopped and the unreacted vinyl chloride monomer was recovered to obtain a vinyl chloride resin latex.
得られた塩化ビニル系樹脂ラテックス１ｋｇを、回転円盤式のスプレードライヤーを用い、熱風温度１９０℃、出口温度６０℃で噴霧乾燥し、ペースト塩化ビニル系樹脂を得た。得られたペースト塩化ビニル系樹脂は、塩化ビニル系樹脂１００重量部に対しドデシルベンゼンスルホン酸ナトリウム０．１重量部、ラウリル硫酸ナトリウム０．８重量部を含むものであった。また、塩化ビニル樹脂の重合度は８５０であり、フタル酸ジイソノニル６０重量部を配合し、調製したペースト塩ビゾルの粒子径分布における平均粒子径は３．０μｍであり、粒子径０．０１～５μｍの範囲の粒子成分５８ｖｏｌ％、５～２００μｍの粒子成分４２ｖｏｌ％のものであった。 1 kg of the obtained vinyl chloride resin latex was spray-dried using a rotating disc type spray dryer at a hot air temperature of 190°C and an outlet temperature of 60°C to obtain a paste vinyl chloride resin. The resulting paste vinyl chloride resin contained 0.1 parts by weight of sodium dodecylbenzenesulfonate and 0.8 parts by weight of sodium lauryl sulfate with respect to 100 parts by weight of the vinyl chloride resin. The vinyl chloride resin has a polymerization degree of 850, and the paste vinyl chloride sol prepared by blending 60 parts by weight of diisononyl phthalate has an average particle size of 3.0 μm in the particle size distribution, and a particle size of 0.01 to 5 μm. 58 vol% of the particle content in the range of 200 μm and 42 vol% of the particle content of 5 to 200 μm.
得られたペースト塩化ビニル系樹脂１００重量部に対し、可塑剤としてジイソノニルフタレート（（株）ジェイ・プラス、グレード工業用）５０重量部、充填剤として炭酸カルシウム（三共精粉（株）、グレード一級）４０重量部、顔料として酸化チタン（テイカ（株）、（商品名）ＪＲ６００Ａ）１０重量部、発泡剤（大塚化学（株）、（商品名）ＡＺウルトラ１０５０）３重量部、希釈剤（ＪＸ日鉱日石（株）、（商品名）Ｎ１０）１０重量部、安定剤（（株）アデカ、（商品名）ＦＬ－１０３Ｎ）３重量部を用い、ディゾルバーを用いて混練し、ペースト塩ビゾルを得た。 To 100 parts by weight of the resulting paste vinyl chloride resin, 50 parts by weight of diisononyl phthalate (J-Plus Co., Ltd., grade industrial use) as a plasticizer, and calcium carbonate (Sankyo Seifun Co., Ltd., grade 1 grade) as a filler. ) 40 parts by weight, 10 parts by weight of titanium oxide (Tayca Co., Ltd., (trade name) JR600A) as a pigment, foaming agent (Otsuka Chemical Co., Ltd., (trade name) AZ Ultra 1050) 3 parts by weight, diluent (JX Nikko Nisseki Co., Ltd., (trade name) N10) 10 parts by weight, stabilizer (Adeka Co., Ltd., (trade name) FL-103N) 3 parts by weight, kneaded using a dissolver to form a paste vinyl chloride sol Obtained.
得られたペースト塩ビゾルを、予め１８０℃で５秒加熱した難燃紙上に０．１４ｍｍの厚みでコーティングし、１９０℃で１０秒加熱することにより、原反を得た。 The resulting paste vinyl chloride sol was coated in a thickness of 0.14 mm on a flame-retardant paper heated at 180° C. for 5 seconds, and heated at 190° C. for 10 seconds to obtain a raw sheet.
得られた原反の厚みを測定した後、２１０℃で３５秒加熱することにより発泡体を得た。その後、得られた発泡体の厚みを測定し、発泡倍率、表面平滑性、発泡シャープ性を評価した。試験結果を表１に示す。発泡倍率は４．４倍であり、表面平滑性、発泡シャープ性に優れるものであった。 After measuring the thickness of the obtained original sheet, it was heated at 210° C. for 35 seconds to obtain a foam. After that, the thickness of the obtained foam was measured, and the expansion ratio, surface smoothness and foam sharpness were evaluated. Table 1 shows the test results. The expansion ratio was 4.4 times, and the surface smoothness and sharpness of foaming were excellent.
比較例１
２．５Ｌステンレス製オートクレーブに脱イオン水６１０ｇ、塩化ビニルモノマー７３０ｇ、５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液１５ｇ、合成例１により得られた平均粒子径０．５５μｍのシードラテックス（ａ）を塩化ビニルモノマー１００重量部に対し４重量部、合成例２により得られた平均粒子径０．１５μｍのシードラテックス（ｂ）を塩化ビニルモノマー１００重量部に対し５重量部仕込み、この反応混合物の温度を５４℃に上げて重合を開始した。重合を開始してから重合を終了までの間、塩化ビニルモノマーに対し０．７重量部の５重量％ラウリル硫酸ナトリウム水溶液を連続的に添加した。重合圧が５４℃における塩化ビニルモノマーの飽和蒸気圧から０．３７ＭＰａまで降下したときに重合を停止し、未反応塩化ビニルモノマーを回収し、塩化ビニル系樹脂ラテックスを得た。
Comparative example 1
610 g of deionized water, 730 g of a vinyl chloride monomer, 15 g of a 5% by weight sodium dodecylbenzenesulfonate aqueous solution, seed latex (a) having an average particle size of 0.55 μm obtained in Synthesis Example 1 was added to a 2.5 L stainless steel autoclave. 4 parts by weight per 100 parts by weight of the monomer, and 5 parts by weight of the seed latex (b) having an average particle size of 0.15 μm obtained in Synthesis Example 2 were charged per 100 parts by weight of the vinyl chloride monomer, and the reaction mixture was heated to 54 parts by weight. °C to initiate polymerization. From the start of polymerization to the end of polymerization, 0.7 parts by weight of a 5% by weight sodium lauryl sulfate aqueous solution was continuously added to the vinyl chloride monomer. When the polymerization pressure dropped from the saturated vapor pressure of the vinyl chloride monomer at 54° C. to 0.37 MPa, the polymerization was stopped and the unreacted vinyl chloride monomer was recovered to obtain a vinyl chloride resin latex.
得られた塩化ビニル系樹脂ラテックス１ｋｇを、回転円盤式のスプレードライヤーを用い、熱風温度１６０℃、出口温度５５℃で噴霧乾燥し、ペースト塩化ビニル系樹脂を得た。得られたペースト塩化ビニル系樹脂は、塩化ビニル系樹脂１００重量部に対しドデシルベンゼンスルホン酸ナトリウム０．１重量部、ラウリル硫酸ナトリウム０．８重量部を含むものであった。また、塩化ビニル樹脂の重合度は１１００であり、フタル酸ジイソノニル６０重量部を配合し、調製したペースト塩ビゾルの粒子径分布における平均粒子径は１．９μｍであり、粒子径０．０１～５μｍの範囲の粒子成分６７ｖｏｌ％、５～２００μｍの粒子成分３３ｖｏｌ％のものであった。 1 kg of the obtained vinyl chloride resin latex was spray-dried using a rotating disc type spray dryer at a hot air temperature of 160°C and an outlet temperature of 55°C to obtain a paste vinyl chloride resin. The resulting paste vinyl chloride resin contained 0.1 parts by weight of sodium dodecylbenzenesulfonate and 0.8 parts by weight of sodium lauryl sulfate with respect to 100 parts by weight of the vinyl chloride resin. The vinyl chloride resin has a polymerization degree of 1100, and the paste vinyl chloride sol prepared by blending 60 parts by weight of diisononyl phthalate has an average particle size of 1.9 μm in the particle size distribution, and a particle size of 0.01 to 5 μm. 67 vol % of the particle content in the range of 200 μm and 33 vol % of the particle content of 5 to 200 μm.
得られたペースト塩化ビニル系樹脂１００重量部に対し、可塑剤としてジイソノニルフタレート（（株）ジェイ・プラス、グレード工業用）５０重量部、充填剤として炭酸カルシウム（三共精粉（株）、グレード一級）４０重量部、顔料として酸化チタン（テイカ（株）、（商品名）ＪＲ６００Ａ）１０重量部、発泡剤（大塚化学（株）、（商品名）ＡＺウルトラ１０５０）３重量部、希釈剤（ＪＸ日鉱日石（株）、（商品名）Ｎ１０）１０重量部、安定剤（（株）アデカ、（商品名）ＦＬ－１０３Ｎ）３重量部を用い、ディゾルバーを用いて混練し、ペースト塩ビゾルを得た。 To 100 parts by weight of the resulting paste vinyl chloride resin, 50 parts by weight of diisononyl phthalate (J-Plus Co., Ltd., grade industrial use) as a plasticizer, and calcium carbonate (Sankyo Seifun Co., Ltd., grade 1 grade) as a filler. ) 40 parts by weight, 10 parts by weight of titanium oxide (Tayca Co., Ltd., (trade name) JR600A) as a pigment, foaming agent (Otsuka Chemical Co., Ltd., (trade name) AZ Ultra 1050) 3 parts by weight, diluent (JX Nikko Nisseki Co., Ltd., (trade name) N10) 10 parts by weight, stabilizer (Adeka Co., Ltd., (trade name) FL-103N) 3 parts by weight, kneaded using a dissolver to form a paste vinyl chloride sol Obtained.
得られたペースト塩ビゾルを、予め１８０℃で５秒加熱した難燃紙上に０．１４ｍｍの厚みでコーティングし、１９０℃で１０秒加熱することにより、原反を得た。 The resulting paste vinyl chloride sol was coated in a thickness of 0.14 mm on a flame-retardant paper heated at 180° C. for 5 seconds, and heated at 190° C. for 10 seconds to obtain a raw sheet.
得られた原反の厚みを測定した後、２１０℃で３５秒加熱することにより発泡体を得た。その後、得られた発泡体の厚みを測定し、発泡倍率、表面平滑性、発泡シャープ性を評価した。試験結果を表２に示す。発泡倍率は４．４倍であり、表面平滑性は優れるものの、発泡シャープ性は劣る結果であった。 After measuring the thickness of the obtained original sheet, it was heated at 210° C. for 35 seconds to obtain a foam. After that, the thickness of the obtained foam was measured, and the expansion ratio, surface smoothness and foam sharpness were evaluated. Table 2 shows the test results. The expansion ratio was 4.4 times, and although the surface smoothness was excellent, the foaming sharpness was inferior.
比較例２
２．５Ｌステンレス製オートクレーブに脱イオン水６１０ｇ、塩化ビニルモノマー７３０ｇ、５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液１５ｇ、合成例１により得られた平均粒子径０．５５μｍのシードラテックス（ａ）を塩化ビニルモノマー１００重量部に対し４重量部、合成例２により得られた平均粒子径０．１５μｍのシードラテックス（ｂ）を塩化ビニルモノマー１００重量部に対し５重量部仕込み、この反応混合物の温度を５４℃に上げて重合を開始した。重合を開始してから重合を終了までの間、塩化ビニルモノマーに対し０．７重量部の５重量％ラウリル硫酸ナトリウム水溶液を連続的に添加した。重合圧が５４℃における塩化ビニルモノマーの飽和蒸気圧から０．３７ＭＰａまで降下したときに重合を停止し、未反応塩化ビニルモノマーを回収し、塩化ビニル系樹脂ラテックスを得た。
Comparative example 2
610 g of deionized water, 730 g of a vinyl chloride monomer, 15 g of a 5% by weight sodium dodecylbenzenesulfonate aqueous solution, seed latex (a) having an average particle size of 0.55 μm obtained in Synthesis Example 1 was added to a 2.5 L stainless steel autoclave. 4 parts by weight per 100 parts by weight of the monomer, and 5 parts by weight of the seed latex (b) having an average particle size of 0.15 μm obtained in Synthesis Example 2 were charged per 100 parts by weight of the vinyl chloride monomer, and the reaction mixture was heated to 54 parts by weight. °C to initiate polymerization. From the start of polymerization to the end of polymerization, 0.7 parts by weight of a 5% by weight sodium lauryl sulfate aqueous solution was continuously added to the vinyl chloride monomer. When the polymerization pressure dropped from the saturated vapor pressure of the vinyl chloride monomer at 54° C. to 0.37 MPa, the polymerization was stopped and the unreacted vinyl chloride monomer was recovered to obtain a vinyl chloride resin latex.
得られた塩化ビニル系樹脂ラテックス１ｋｇを、回転円盤式のスプレードライヤーを用い、熱風温度１１０℃、出口温度５０℃で噴霧乾燥し、ペースト塩化ビニル系樹脂を得た。得られたペースト塩化ビニル系樹脂は、塩化ビニル系樹脂１００重量部に対しドデシルベンゼンスルホン酸ナトリウム０．１重量部、ラウリル硫酸ナトリウム０．８重量部を含むものであった。また、塩化ビニル樹脂の重合度は１１００であり、フタル酸ジイソノニル６０重量部を配合し、調製したペースト塩ビゾルの粒子径分布における平均粒子径は１．３μｍであり、粒子径０．０１～５μｍの範囲の粒子成分９５ｖｏｌ％、５～２００μｍの粒子成分５ｖｏｌ％のものであった。 1 kg of the obtained vinyl chloride resin latex was spray-dried using a rotary disk type spray dryer at a hot air temperature of 110°C and an outlet temperature of 50°C to obtain a paste vinyl chloride resin. The resulting paste vinyl chloride resin contained 0.1 parts by weight of sodium dodecylbenzenesulfonate and 0.8 parts by weight of sodium lauryl sulfate with respect to 100 parts by weight of the vinyl chloride resin. The vinyl chloride resin has a polymerization degree of 1100, and the paste vinyl chloride sol prepared by blending 60 parts by weight of diisononyl phthalate has an average particle size of 1.3 μm in the particle size distribution, and a particle size of 0.01 to 5 μm. 95 vol% of the particle content in the range of 100 μm and 5 vol% of the particle content of 5 to 200 μm.
得られたペースト塩化ビニル系樹脂１００重量部に対し、可塑剤としてジイソノニルフタレート（（株）ジェイ・プラス、グレード工業用）５０重量部、充填剤として炭酸カルシウム（三共精粉（株）、グレード一級）４０重量部、顔料として酸化チタン（テイカ（株）、（商品名）ＪＲ６００Ａ）１０重量部、発泡剤（大塚化学（株）、（商品名）ＡＺウルトラ１０５０）３重量部、希釈剤（ＪＸ日鉱日石（株）、（商品名）Ｎ１０）１０重量部、安定剤（（株）アデカ、（商品名）ＦＬ－１０３Ｎ）３重量部を用い、ディゾルバーを用いて混練し、ペースト塩ビゾルを得た。 To 100 parts by weight of the resulting paste vinyl chloride resin, 50 parts by weight of diisononyl phthalate (J-Plus Co., Ltd., grade industrial use) as a plasticizer, and calcium carbonate (Sankyo Seifun Co., Ltd., grade 1 grade) as a filler. ) 40 parts by weight, 10 parts by weight of titanium oxide (Tayca Co., Ltd., (trade name) JR600A) as a pigment, foaming agent (Otsuka Chemical Co., Ltd., (trade name) AZ Ultra 1050) 3 parts by weight, diluent (JX Nikko Nisseki Co., Ltd., (trade name) N10) 10 parts by weight, stabilizer (Adeka Co., Ltd., (trade name) FL-103N) 3 parts by weight, kneaded using a dissolver to form a paste vinyl chloride sol Obtained.
得られたペースト塩ビゾルを、予め１８０℃で５秒加熱した難燃紙上に０．１４ｍｍの厚みでコーティングし、１９０℃で１０秒加熱することにより、原反を得た。 The resulting paste vinyl chloride sol was coated in a thickness of 0.14 mm on a flame-retardant paper heated at 180° C. for 5 seconds, and heated at 190° C. for 10 seconds to obtain a raw sheet.
得られた原反の厚みを測定した後、２１０℃で３５秒加熱することにより発泡体を得た。その後、得られた発泡体の厚みを測定し、発泡倍率、表面平滑性、発泡シャープ性を評価した。試験結果を表２に示す。発泡倍率は４．２倍であり、表面平滑性、発泡シャープ性は劣る結果であった。 After measuring the thickness of the obtained original sheet, it was heated at 210° C. for 35 seconds to obtain a foam. After that, the thickness of the obtained foam was measured, and the expansion ratio, surface smoothness and foam sharpness were evaluated. Table 2 shows the test results. The foaming ratio was 4.2 times, and the surface smoothness and foaming sharpness were inferior.
比較例３
２．５Ｌステンレス製オートクレーブに脱イオン水６１０ｇ、塩化ビニルモノマー７３０ｇ、５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液１５ｇ、２重量％過硫酸カリウム２ｇ、合成例１により得られた平均粒子径０．５５μｍのシードラテックス（ａ）を塩化ビニルモノマー１００重量部に対し４重量部、合成例２により得られた平均粒子径０．１５μｍのシードラテックス（ｂ）を塩化ビニルモノマー１００重量部に対し７重量部仕込み、この反応混合物の温度を５１℃に上げて重合を開始した。重合を開始してから重合を終了までの間、塩化ビニルモノマーに対し０．７重量部の５重量％ドデシルベンゼンスルホン酸ナトリウム水溶液を連続的に添加した。重合圧が５１℃における塩化ビニルモノマーの飽和蒸気圧から０．３３ＭＰａまで降下したときに重合を停止し、未反応塩化ビニルモノマーを回収し、塩化ビニル系樹脂ラテックスを得た。
Comparative example 3
610 g of deionized water, 730 g of vinyl chloride monomer, 15 g of 5% by weight sodium dodecylbenzenesulfonate aqueous solution, 2 g of 2% by weight potassium persulfate, and the average particle size of 0.55 μm obtained in Synthesis Example 1 were placed in a 2.5 L stainless steel autoclave. 4 parts by weight of seed latex (a) per 100 parts by weight of vinyl chloride monomer, and 7 parts by weight of seed latex (b) having an average particle size of 0.15 μm obtained in Synthesis Example 2 per 100 parts by weight of vinyl chloride monomer. , the temperature of the reaction mixture was raised to 51°C to initiate polymerization. 0.7 parts by weight of a 5% by weight sodium dodecylbenzenesulfonate aqueous solution was continuously added to the vinyl chloride monomer from the start of the polymerization to the end of the polymerization. When the polymerization pressure dropped from the saturated vapor pressure of the vinyl chloride monomer at 51° C. to 0.33 MPa, the polymerization was stopped and the unreacted vinyl chloride monomer was recovered to obtain a vinyl chloride resin latex.
得られた塩化ビニル系樹脂ラテックス１ｋｇを、回転円盤式のスプレードライヤーを用い、熱風温度１６０℃、出口温度５５℃で噴霧乾燥し、ペースト塩化ビニル系樹脂を得た。得られたペースト塩化ビニル系樹脂は、塩化ビニル系樹脂１００重量部に対しドデシルベンゼンスルホン酸ナトリウム０．９重量部を含むものであった。また、塩化ビニル樹脂の重合度は１３００であり、フタル酸ジイソノニル６０重量部を配合し、調製したペースト塩ビゾルの粒子径分布における平均粒子径は３．２μｍであり、粒子径０．０１～５μｍの範囲の粒子成分５５ｖｏｌ％、５～２００μｍの粒子成分４５ｖｏｌ％のものであった。 1 kg of the obtained vinyl chloride resin latex was spray-dried using a rotating disc type spray dryer at a hot air temperature of 160°C and an outlet temperature of 55°C to obtain a paste vinyl chloride resin. The resulting paste vinyl chloride resin contained 0.9 parts by weight of sodium dodecylbenzenesulfonate per 100 parts by weight of the vinyl chloride resin. The vinyl chloride resin has a polymerization degree of 1300, and the paste vinyl chloride sol prepared by blending 60 parts by weight of diisononyl phthalate has an average particle size of 3.2 μm in the particle size distribution, and a particle size of 0.01 to 5 μm. 55 vol% of the particle component in the range of 200 µm and 45 vol% of the particle component in the range of 5 to 200 µm.
得られたペースト塩化ビニル系樹脂１００重量部に対し、可塑剤としてジイソノニルフタレート（（株）ジェイ・プラス、グレード工業用）５０重量部、充填剤として炭酸カルシウム（三共精粉（株）、グレード一級）４０重量部、顔料として酸化チタン（テイカ（株）、（商品名）ＪＲ６００Ａ）１０重量部、発泡剤（大塚化学（株）、（商品名）ＡＺウルトラ１０５０）３重量部、希釈剤（ＪＸ日鉱日石（株）、（商品名）Ｎ１０）１０重量部、安定剤（（株）アデカ、（商品名）ＦＬ－１０３Ｎ）３重量部を用い、ディゾルバーを用いて混練し、ペースト塩ビゾルを得た。 To 100 parts by weight of the resulting paste vinyl chloride resin, 50 parts by weight of diisononyl phthalate (J-Plus Co., Ltd., grade industrial use) as a plasticizer, and calcium carbonate (Sankyo Seifun Co., Ltd., grade 1 grade) as a filler. ) 40 parts by weight, 10 parts by weight of titanium oxide (Tayca Co., Ltd., (trade name) JR600A) as a pigment, foaming agent (Otsuka Chemical Co., Ltd., (trade name) AZ Ultra 1050) 3 parts by weight, diluent (JX Nikko Nisseki Co., Ltd., (trade name) N10) 10 parts by weight, stabilizer (Adeka Co., Ltd., (trade name) FL-103N) 3 parts by weight, kneaded using a dissolver to form a paste vinyl chloride sol Obtained.
得られたペースト塩ビゾルを、予め１８０℃で５秒加熱した難燃紙上に０．１４ｍｍの厚みでコーティングし、１９０℃で１０秒加熱することにより、原反を得た。 The resulting paste vinyl chloride sol was coated in a thickness of 0.14 mm on a flame-retardant paper heated at 180° C. for 5 seconds, and heated at 190° C. for 10 seconds to obtain a raw sheet.
得られた原反の厚みを測定した後、２１０℃で３５秒加熱することにより発泡体を得た。その後、得られた発泡体の厚みを測定し、発泡倍率、表面平滑性、発泡シャープ性を評価した。試験結果を表２に示す。発泡倍率は４．９倍であり、表面平滑性は優れるものの、発泡シャープ性は劣る結果であった。 After measuring the thickness of the obtained original sheet, it was heated at 210° C. for 35 seconds to obtain a foam. After that, the thickness of the obtained foam was measured, and the expansion ratio, surface smoothness and foam sharpness were evaluated. Table 2 shows the test results. The expansion ratio was 4.9 times, and although the surface smoothness was excellent, the foaming sharpness was inferior.
本発明のペースト塩化ビニル系樹脂は、表面平滑性、発泡印刷シャープ性に優れる発泡体を提供することが可能であり、発泡壁紙用、特にロータリースクリーン印刷壁紙用として適したものである。 The paste vinyl chloride resin of the present invention can provide a foam having excellent surface smoothness and foam printing sharpness, and is suitable for foam wallpaper, particularly for rotary screen printing wallpaper.
Claims (5)
条件１；ペースト塩化ビニル系樹脂１００重量部に対し、フタル酸ジイソノニル６０重量部を配合し、ペースト塩化ビニル系樹脂ゾルを調製し、２３℃、２時間保管後にレーザー回折・散乱法にて粒子径分布を測定。 Contains 0.5 to 2 parts by weight of alkyl sulfate and 0.05 to 0.5 parts by weight of alkylbenzene sulfonate for 100 parts by weight of vinyl chloride resin having an average degree of polymerization of 700 to 1500, and meets the following condition 1 It is characterized in that the average particle diameter when measured by the Paste vinyl chloride resin.
Condition 1: 60 parts by weight of diisononyl phthalate is blended with 100 parts by weight of paste vinyl chloride resin to prepare a paste vinyl chloride resin sol, which is stored at 23° C. for 2 hours, and then the particle size is determined by laser diffraction/scattering method. Measure distribution.
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