NO762540L - - Google Patents
Info
- Publication number
- NO762540L NO762540L NO762540A NO762540A NO762540L NO 762540 L NO762540 L NO 762540L NO 762540 A NO762540 A NO 762540A NO 762540 A NO762540 A NO 762540A NO 762540 L NO762540 L NO 762540L
- Authority
- NO
- Norway
- Prior art keywords
- dyes
- compounds
- polymerization
- group
- acid
- Prior art date
Links
- 150000001875 compounds Chemical class 0.000 claims description 67
- 238000006116 polymerization reaction Methods 0.000 claims description 64
- 238000000034 method Methods 0.000 claims description 44
- 239000000178 monomer Substances 0.000 claims description 43
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims description 34
- 239000000975 dye Substances 0.000 claims description 33
- -1 oxides Chemical class 0.000 claims description 32
- 239000006185 dispersion Substances 0.000 claims description 25
- 238000000576 coating method Methods 0.000 claims description 23
- 239000011248 coating agent Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000654 additive Substances 0.000 claims description 18
- 150000003839 salts Chemical class 0.000 claims description 18
- 150000002894 organic compounds Chemical class 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 150000002148 esters Chemical class 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 150000004715 keto acids Chemical class 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 7
- 239000000987 azo dye Substances 0.000 claims description 7
- 239000004800 polyvinyl chloride Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 239000000314 lubricant Substances 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000001993 wax Substances 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000004014 plasticizer Substances 0.000 claims description 4
- 239000011342 resin composition Substances 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000001000 anthraquinone dye Substances 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 239000002216 antistatic agent Substances 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 150000001735 carboxylic acids Chemical class 0.000 claims description 3
- 150000004820 halides Chemical class 0.000 claims description 3
- 150000004679 hydroxides Chemical class 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- 239000003505 polymerization initiator Substances 0.000 claims description 3
- 150000004053 quinones Chemical class 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 150000003568 thioethers Chemical class 0.000 claims description 3
- QGKMIGUHVLGJBR-UHFFFAOYSA-M (4z)-1-(3-methylbutyl)-4-[[1-(3-methylbutyl)quinolin-1-ium-4-yl]methylidene]quinoline;iodide Chemical compound [I-].C12=CC=CC=C2N(CCC(C)C)C=CC1=CC1=CC=[N+](CCC(C)C)C2=CC=CC=C12 QGKMIGUHVLGJBR-UHFFFAOYSA-M 0.000 claims description 2
- RTLULCVBFCRQKI-UHFFFAOYSA-N 1-amino-4-[3-[(4,6-dichloro-1,3,5-triazin-2-yl)amino]-4-sulfoanilino]-9,10-dioxoanthracene-2-sulfonic acid Chemical compound C1=2C(=O)C3=CC=CC=C3C(=O)C=2C(N)=C(S(O)(=O)=O)C=C1NC(C=1)=CC=C(S(O)(=O)=O)C=1NC1=NC(Cl)=NC(Cl)=N1 RTLULCVBFCRQKI-UHFFFAOYSA-N 0.000 claims description 2
- QAMCXJOYXRSXDU-UHFFFAOYSA-N 2,4-dimethoxy-n-[2-(1,3,3-trimethylindol-1-ium-2-yl)ethenyl]aniline;chloride Chemical compound [Cl-].COC1=CC(OC)=CC=C1NC=CC1=[N+](C)C2=CC=CC=C2C1(C)C QAMCXJOYXRSXDU-UHFFFAOYSA-N 0.000 claims description 2
- BCHZICNRHXRCHY-UHFFFAOYSA-N 2h-oxazine Chemical compound N1OC=CC=C1 BCHZICNRHXRCHY-UHFFFAOYSA-N 0.000 claims description 2
- MCTQNEBFZMBRSQ-GEEYTBSJSA-N Chrysoidine Chemical compound Cl.NC1=CC(N)=CC=C1\N=N\C1=CC=CC=C1 MCTQNEBFZMBRSQ-GEEYTBSJSA-N 0.000 claims description 2
- JQYMGXZJTCOARG-UHFFFAOYSA-N Reactive blue 2 Chemical compound C1=2C(=O)C3=CC=CC=C3C(=O)C=2C(N)=C(S(O)(=O)=O)C=C1NC(C=C1S(O)(=O)=O)=CC=C1NC(N=1)=NC(Cl)=NC=1NC1=CC=CC(S(O)(=O)=O)=C1 JQYMGXZJTCOARG-UHFFFAOYSA-N 0.000 claims description 2
- WLKAMFOFXYCYDK-UHFFFAOYSA-N [5-amino-4-[[3-[(2-amino-4-azaniumyl-5-methylphenyl)diazenyl]-4-methylphenyl]diazenyl]-2-methylphenyl]azanium;dichloride Chemical compound [Cl-].[Cl-].CC1=CC=C(N=NC=2C(=CC([NH3+])=C(C)C=2)N)C=C1N=NC1=CC(C)=C([NH3+])C=C1N WLKAMFOFXYCYDK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000999 acridine dye Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 150000001299 aldehydes Chemical class 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- JPIYZTWMUGTEHX-UHFFFAOYSA-N auramine O free base Chemical compound C1=CC(N(C)C)=CC=C1C(=N)C1=CC=C(N(C)C)C=C1 JPIYZTWMUGTEHX-UHFFFAOYSA-N 0.000 claims description 2
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical group OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 claims description 2
- FCCOTXHFDDRSDO-UHFFFAOYSA-L disodium 5-[[4-[[4-[(3-carboxylato-4-hydroxyphenyl)diazenyl]phenyl]carbamoylamino]phenyl]diazenyl]-2-hydroxybenzoate Chemical compound [Na+].[Na+].Oc1ccc(cc1C([O-])=O)N=Nc1ccc(NC(=O)Nc2ccc(cc2)N=Nc2ccc(O)c(c2)C([O-])=O)cc1 FCCOTXHFDDRSDO-UHFFFAOYSA-L 0.000 claims description 2
- NDHOYLRUTRKFBM-UHFFFAOYSA-L disodium 6-amino-5-[[4-[4-[(1-amino-4-sulfonatonaphthalen-2-yl)diazenyl]phenyl]phenyl]diazenyl]-4-hydroxynaphthalene-2-sulfonate Chemical compound NC1=CC=C2C=C(C=C(O)C2=C1N=NC1=CC=C(C=C1)C1=CC=C(C=C1)N=NC1=C(N)C2=CC=CC=C2C(=C1)S(=O)(=O)O[Na])S(=O)(=O)O[Na] NDHOYLRUTRKFBM-UHFFFAOYSA-L 0.000 claims description 2
- FTZLWXQKVFFWLY-UHFFFAOYSA-L disodium;2,5-dichloro-4-[3-methyl-5-oxo-4-[(4-sulfonatophenyl)diazenyl]-4h-pyrazol-1-yl]benzenesulfonate Chemical compound [Na+].[Na+].CC1=NN(C=2C(=CC(=C(Cl)C=2)S([O-])(=O)=O)Cl)C(=O)C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 FTZLWXQKVFFWLY-UHFFFAOYSA-L 0.000 claims description 2
- YUZILKLGVPUFOT-YHPRVSEPSA-L disodium;5-[(6-anilino-4-oxo-1h-1,3,5-triazin-2-yl)amino]-2-[(e)-2-[4-[(6-anilino-4-oxo-1h-1,3,5-triazin-2-yl)amino]-2-sulfonatophenyl]ethenyl]benzenesulfonate Chemical compound [Na+].[Na+].C=1C=C(\C=C\C=2C(=CC(NC=3NC(NC=4C=CC=CC=4)=NC(=O)N=3)=CC=2)S([O-])(=O)=O)C(S(=O)(=O)[O-])=CC=1NC(N1)=NC(=O)N=C1NC1=CC=CC=C1 YUZILKLGVPUFOT-YHPRVSEPSA-L 0.000 claims description 2
- SEACYXSIPDVVMV-UHFFFAOYSA-L eosin Y Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C([O-])=C(Br)C=C21 SEACYXSIPDVVMV-UHFFFAOYSA-L 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 239000012760 heat stabilizer Substances 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 239000001005 nitro dye Substances 0.000 claims description 2
- 239000001006 nitroso dye Substances 0.000 claims description 2
- 150000002923 oximes Chemical class 0.000 claims description 2
- 239000001007 phthalocyanine dye Substances 0.000 claims description 2
- 239000011295 pitch Substances 0.000 claims description 2
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 2
- 235000012731 ponceau 4R Nutrition 0.000 claims description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 claims description 2
- OARRHUQTFTUEOS-UHFFFAOYSA-N safranin Chemical compound [Cl-].C=12C=C(N)C(C)=CC2=NC2=CC(C)=C(N)C=C2[N+]=1C1=CC=CC=C1 OARRHUQTFTUEOS-UHFFFAOYSA-N 0.000 claims description 2
- LYZQCTRTDQFROA-UHFFFAOYSA-N sodium 4-hydroxy-7-[[5-hydroxy-7-sulfo-6-[(6-sulfonaphthalen-2-yl)diazenyl]naphthalen-2-yl]carbamoylamino]-3-phenyldiazenylnaphthalene-2-sulfonic acid Chemical compound C1=CC=C(C=C1)N=NC2=C(C=C3C=C(C=CC3=C2O)NC(=O)NC4=CC5=CC(=C(C(=C5C=C4)O)N=NC6=CC7=C(C=C6)C=C(C=C7)S(=O)(=O)O)S(=O)(=O)O)S(=O)(=O)O.[Na+] LYZQCTRTDQFROA-UHFFFAOYSA-N 0.000 claims description 2
- CQNXJSVLKPHNRI-OXEZCZPGSA-N sodium 5-[(4-hydroxyphenyl)diazenyl]-2-[(E)-2-[4-[(4-hydroxyphenyl)diazenyl]-2-sulfophenyl]ethenyl]benzenesulfonic acid Chemical compound C1=CC(=CC=C1N=NC2=CC(=C(C=C2)/C=C/C3=C(C=C(C=C3)N=NC4=CC=C(C=C4)O)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] CQNXJSVLKPHNRI-OXEZCZPGSA-N 0.000 claims description 2
- 239000011269 tar Substances 0.000 claims description 2
- 239000001017 thiazole dye Substances 0.000 claims description 2
- RBKBGHZMNFTKRE-UHFFFAOYSA-K trisodium 2-[(2-oxido-3-sulfo-6-sulfonatonaphthalen-1-yl)diazenyl]benzoate Chemical compound C1=CC=C(C(=C1)C(=O)[O-])N=NC2=C3C=CC(=CC3=CC(=C2[O-])S(=O)(=O)O)S(=O)(=O)[O-].[Na+].[Na+].[Na+] RBKBGHZMNFTKRE-UHFFFAOYSA-K 0.000 claims description 2
- 239000001018 xanthene dye Substances 0.000 claims description 2
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims 1
- AUNGANRZJHBGPY-SCRDCRAPSA-N Riboflavin Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-SCRDCRAPSA-N 0.000 claims 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims 1
- 239000006096 absorbing agent Substances 0.000 claims 1
- YOCIQNIEQYCORH-UHFFFAOYSA-M chembl2028361 Chemical compound [Na+].OC1=CC=C2C=C(S([O-])(=O)=O)C=CC2=C1N=NC1=CC=CC=C1 YOCIQNIEQYCORH-UHFFFAOYSA-M 0.000 claims 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 claims 1
- 229940097275 indigo Drugs 0.000 claims 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- 238000005728 strengthening Methods 0.000 claims 1
- 150000003462 sulfoxides Chemical class 0.000 claims 1
- 239000001016 thiazine dye Substances 0.000 claims 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 claims 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 claims 1
- 229920000642 polymer Polymers 0.000 description 24
- 230000008021 deposition Effects 0.000 description 22
- 239000000243 solution Substances 0.000 description 22
- 239000002253 acid Substances 0.000 description 14
- 239000002184 metal Substances 0.000 description 13
- 238000013019 agitation Methods 0.000 description 10
- 238000010557 suspension polymerization reaction Methods 0.000 description 10
- 239000000981 basic dye Substances 0.000 description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 150000002739 metals Chemical class 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 239000000982 direct dye Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000004115 Sodium Silicate Substances 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000007334 copolymerization reaction Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 6
- 229910052911 sodium silicate Inorganic materials 0.000 description 6
- 229940126062 Compound A Drugs 0.000 description 5
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 5
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 239000000980 acid dye Substances 0.000 description 5
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 238000012662 bulk polymerization Methods 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 4
- 239000008116 calcium stearate Substances 0.000 description 4
- 235000013539 calcium stearate Nutrition 0.000 description 4
- 238000007720 emulsion polymerization reaction Methods 0.000 description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- TZJQCUDHKUWEFU-UHFFFAOYSA-N 2,2-dimethylpentanenitrile Chemical compound CCCC(C)(C)C#N TZJQCUDHKUWEFU-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical group [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000012736 aqueous medium Substances 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 150000002118 epoxides Chemical class 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- 235000011007 phosphoric acid Nutrition 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 239000000985 reactive dye Substances 0.000 description 3
- 239000003549 soybean oil Substances 0.000 description 3
- 235000012424 soybean oil Nutrition 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 description 2
- HXVNBWAKAOHACI-UHFFFAOYSA-N 2,4-dimethyl-3-pentanone Chemical compound CC(C)C(=O)C(C)C HXVNBWAKAOHACI-UHFFFAOYSA-N 0.000 description 2
- NXQMCAOPTPLPRL-UHFFFAOYSA-N 2-(2-benzoyloxyethoxy)ethyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCCOCCOC(=O)C1=CC=CC=C1 NXQMCAOPTPLPRL-UHFFFAOYSA-N 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
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- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- 235000011178 triphosphate Nutrition 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 229940124543 ultraviolet light absorber Drugs 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
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/002—Scale prevention in a polymerisation reactor or its auxiliary parts
- C08F2/004—Scale prevention in a polymerisation reactor or its auxiliary parts by a prior coating on the reactor walls
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
Nærværende oppfinnelse vedrører en fremgangsmåte for fremstillingThe present invention relates to a method for production
av polyvinylkloridharpikser som er forblandet med foskjellige additiver såsom stabilisatorer, smøremidler, fyllstoffer, fargestoffer og lignende, hvorved man foretar polymerisasjon av vinylkloridmonomer eller en blanding av vinylkloridmonomer med en annen monomer eller monomerer, som er kopolymeriserbar resp. kopolymeriserbare med vinylklorid, i nærvær av forannevnte additiver i en polymerisasjonsreaktor, hvis innervegger og andre overflater, som kommer i kontakt med rnonomeren eller monomerene, er overtrukket eller behandlet med spesielle kjemikalier. of polyvinyl chloride resins which are premixed with various additives such as stabilizers, lubricants, fillers, dyes and the like, whereby polymerization of vinyl chloride monomer or a mixture of vinyl chloride monomer with another monomer or monomers, which is copolymerisable resp. copolymerizable with vinyl chloride, in the presence of the aforementioned additives in a polymerization reactor, whose inner walls and other surfaces, which come into contact with the monomer or monomers, are coated or treated with special chemicals.
Det er fra tidligere kjent forskjellige typer polymerisasjon, hvilke omfatter suspensjonspolymerisasjon, emulsjonspolymerisasjon, løsningspolymerisasjon, gassfasepolymerisasjon og massepolymerisasjon. Alle tidligere kjente metoder lider av problemet med polymerskallavsetning på innerveggene til polymerisasjonsreaktoren, agitatorbladene og andre overflater som kommer i kontakt med monomer. Dette har ugunstige konsekvenser med hensyn til redusert polymerutbytte og redusert kjølekapasitet i polymerisasjonsreaktoren, og dessuten foreligger fare for at polymerskall løsner fra overflatene og således havner i slutt-produktene, som derved blir av dårligere kvalitet. I tillegg til disse ulemper kommer rensearbeidet med polymerisasjonsreaktoren, hvorved fjerningen av polymerskall krever meget tid og arbeid. Arbeidet byr forøvrig på alvorlige helsemessige problemer for arbeiderne på grunn av giftigheten av den i polymerskallet aborberte og ureagerte vinylkloridmonomeren. There are previously known different types of polymerization, which include suspension polymerization, emulsion polymerization, solution polymerization, gas phase polymerization and mass polymerization. All previously known methods suffer from the problem of polymer scale deposition on the inner walls of the polymerization reactor, the agitator blades, and other surfaces that come into contact with monomer. This has unfavorable consequences with regard to reduced polymer yield and reduced cooling capacity in the polymerization reactor, and there is also a risk of polymer shells detaching from the surfaces and thus ending up in the end products, which are therefore of poorer quality. In addition to these disadvantages comes the cleaning work with the polymerization reactor, whereby the removal of polymer shell requires a lot of time and work. The work also presents serious health problems for the workers due to the toxicity of the vinyl chloride monomer absorbed and unreacted in the polymer shell.
Når polyvinyiklorldharplksér ahvéri^ av ' f orskjellige artikler vil, på den anrién :tside: polyyir^lk^ '• harpiksene vanligvis blandes med forskjellige, typer additiver^ '.såsom stabilisatorer, smøremidler, fyllstoffer, fargestoffer. / , og lignende, og de erholdte.sammensetninger, som foreligger i f orm'av pulver eller pellet,, er klare 'f or støping -tidl artikler av ønsket form ved hjelp' av ekstrudere teller .sprøytestøpemas'kinér. Denne fremgangsmåte er imidlertid noe vanskelig og problemfylt på grunn av emisjonen; av skadelig ureågert vinylkloridmonomer. ved blandingsoperas joneri,.samt så vel som'vanskeligheter med å, sikre Jevn fordeling av additivene i forbindelsen.,Det er for nærværende derfor eh tendens til'å' sløyfe blandingsoperasjbnén ved å forblande vinylkloridmonomeren med de 'nevnte additiver under eller før polymerisasjonsproséssen, for således å fremstille de såkalte polyvinylkloridharpiks-sammensetningene. Denne fremstillingsprosess. for forblandede polyyinylkloridharpiks-sammensetninger.er imidlertid ikke fri for problemet med polymerskallavsetning.'When polyvinyl chloride resins are made of different articles, on the other hand, the polyvinyl resins are usually mixed with different types of additives, such as stabilizers, lubricants, fillers, dyes. / , and the like, and the compositions obtained, which are in the form of powder or pellet, are ready for molding - tidl articles of the desired shape by means of extruders and injection molding machines. However, this method is somewhat difficult and problematic due to the emission; of harmful unreacted vinyl chloride monomer. in the mixing operation, as well as difficulties in ensuring even distribution of the additives in the compound. There is currently therefore a tendency to skip the mixing operation by premixing the vinyl chloride monomer with the aforementioned additives during or before the polymerization process, in order to thus produce the so-called polyvinyl chloride resin compositions. This manufacturing process. for premixed polyyinyl chloride resin compositions, however, are not free from the problem of polymer shell deposition.'
Det er kjent en fremgangsmåte for å hindre pqlymerskallavsetning på innerveggene til .polymerisasjonsreaktoren og øvrige overflater. Ifølge denne fremgangsmåte overtrekkes overflatene,'som kommer A method is known to prevent polymer scale deposition on the inner walls of the polymerization reactor and other surfaces. According to this method, the surfaces, which come, are coated
i kontakt med monomeréri, med visse'polare organiske forbindelser såsom aminforbindelser, kinonforbindelser, aldehydforbindelser og lignende (jfr.- f.eks. U.S. patent nr. 3669.946). Denne fremgangsmåte er effektiv med hensyn til å,.hindre polymerskallavsetning ved suspensjonspolymerisasjon av vinylklorid, eller spesielt av vinylklorid alene, i et vandig medium, men fremgangsmåten er mindre effektiv når polymerisasjonen utføres 1 nærvær av additiver såsom stabilisatorer, smøremidler, fyllstoffer, fargestoffer og lignende, hvor effekten for å hindre polymerskallavsetning går tapt på relativt kort tid ved kontinuerlig polymerisasjon.. in contact with monomers, with certain polar organic compounds such as amine compounds, quinone compounds, aldehyde compounds and the like (cf., e.g., U.S. patent no. 3669,946). This method is effective in preventing polymer shell deposition by suspension polymerization of vinyl chloride, or especially of vinyl chloride alone, in an aqueous medium, but the method is less effective when the polymerization is carried out in the presence of additives such as stabilizers, lubricants, fillers, dyes and the like , where the effect to prevent polymer shell deposition is lost in a relatively short time with continuous polymerisation.
Formålet ved nærværende oppfinnelse har vært å fremskaffe en nyThe purpose of the present invention has been to provide a new
og forbedret fremgangsmåte for fremstilling av forblandede and improved method for the preparation of premixes
polyvinylkloridharpiks-sammensetninger.ved polymerisasJonen av vinylkloridmonomer eller ved kopolymerisasjon av vinylklorid med en annen koplymeriserbar monomer eller kopo lymer i serbar e monomer er, i nærvær av additiver, hvorved avsetning av polymerskall på overflatene minimaliseres uavhengig av polymerisasjons-typen. polyvinyl chloride resin compositions. by polymerization of vinyl chloride monomer or by copolymerization of vinyl chloride with another copolymerizable monomer or copolymers in severable monomers, in the presence of additives, whereby the deposition of polymer shell on the surfaces is minimized regardless of the type of polymerization.
Fremgangsmåten ifølge nærværende oppfinnelse omfatter utførelseThe method according to the present invention includes execution
av polymerisasjonen av vinylkloridmonomer alene for seg eller kopolymerisasjon av en, blanding av vinylklorid med noen annen monomer eller andre monomerer, som er kopolymeriserbar resp. kopolymeriserbare med vinylklorid, i nærvær av en polymerisasjonsinitiator og et flertall additiver i en polymerisasjonsreaktor. Herved blir innerveggene og andre overflater i polymerisasJonsreaktoren, hvilke kommer i kontakt med monomeren, resp. menomeréne, overtrukket eller behandlet før polymerisasjonen med (a) i det minste en organisk forbindelse utvalgt,fra gruppen bestående av' polare organiske forbindelser og organiske fargestoffer'og (b) of the polymerization of vinyl chloride monomer alone or copolymerization of a mixture of vinyl chloride with some other monomer or other monomers, which is copolymerizable or copolymerizable with vinyl chloride, in the presence of a polymerization initiator and a plurality of additives in a polymerization reactor. In this way, the inner walls and other surfaces in the polymerization reactor, which come into contact with the monomer, resp. menomerenes, coated or treated before polymerization with (a) at least one organic compound selected from the group consisting of 'polar organic compounds and organic dyes' and (b)
i det minste en forbindelse utvalgt fra gruppen bestående av hydroksyder, oksyder, halogenider og karboksylater av metallelementer samt oksosyrer av elementene tilhørende den andre til den sjette perioden, og da gruppene IIB og III til VII; i det periodiske system, samt saltene til okssyrene. Den ved nærværende fremgangsmåte oppnådde effekt kan ytterligere forbedres ved å'tilsette reaksjonsproduktet av de ovennevnte forbindelsene (a) at least one compound selected from the group consisting of hydroxides, oxides, halides and carboxylates of metal elements as well as oxoacids of the elements belonging to the second to the sixth period, and then groups IIB and III to VII; in the periodic table, as well as the salts of the oxic acids. The effect achieved by the present method can be further improved by adding the reaction product of the above-mentioned compounds (a)
og (b) i en mengde fra 5 til iOO vekts-p.p.m., beregnet på monomeren eller monomerene som er gjenstand for polymerisasjon, til polymerisasjonsreaktoren, som har overflater som er overtrukket eller behandlet på ovenfor beskrevne måte. and (b) in an amount of from 5 to 100 wt.p.m., calculated on the monomer or monomers subject to polymerization, to the polymerization reactor, which has surfaces coated or treated in the manner described above.
Av de ovenfor nevnte forbindelser (a) kan følgende nevnes: (1) Nitrogenholdige organiske forbindelser utvalgt fra f orbindelsene med en amlno-, imino-, azo-, nitro-, nitroso- eller azometingruppe eller en azlnring samt amin-, imin-, og kvaternære ammoniumforbindelser, f.eks. azometan, azobenzen,, nitrobenzen, nitrosobenzen, monoaminomononltroazobenzen, pyrazin, pyridin, tiaziner, anilin. oksaziner (morf olin etc. ), benzalanilin, EDTA,c<- og'j3-na f ty laminer, etanolamin, dietanolamin; ,toluidiner, rnetylenblått, "Nigrosine Black", "Oil Black", "Spirit Black"/ diamindnaftalener, difenyl-amin, hydrazinderivater, N,N-dimetylamin,■-. urea, laurylamin,.cetyl-trimetylammonlumklorid, polyamider og poiyetyléniminér. (2) Svovelholdige organiske forbindelser.utvalgt fra•forbindelsene med en tiokarbqnyl-, tioeter- eller tioalkoholgruppe, f.eks. tioglykolsyre, tiourea, tiokarbanilsyre, tiokarbaminsyre, tiobenzo-syre, tioetere ifølge den generelle formelen R-S-R', hvor R. og R', som kan ha samme eller forrskjellig betydning, hver står for en alkylgruppe såsom dimetylsulfid og etylmetylsulfid, merkaptaner såsom propylmerkaptan og butylmerkaptan, polysulfider, polysulfoner, sulfonsyrer såsom p-toluensulfonsyre, cykloheksylsulfonsyre, .. , antrakinonsulfonsyre, metanilsyre; dodecylbenzensulfonsyre samt salter derav med alkalimetaller såsom natrium og kalium. (3) Oksygenholdige organiske forbindelser utvalgt fra kinoner, Of the above-mentioned compounds (a), the following can be mentioned: (1) Nitrogen-containing organic compounds selected from the compounds with an amino-, imino-, azo-, nitro-, nitroso- or azomethine group or an azln ring as well as amine-, imine-, and quaternary ammonium compounds, e.g. azomethane, azobenzene,, nitrobenzene, nitrosobenzene, monoaminomononltroazobenzene, pyrazine, pyridine, thiazines, aniline. oxazines (morpholine etc. ), benzalaniline, EDTA, c<- and'j3-na f ty lamins, ethanolamine, diethanolamine; ,toluidines, rnethylene blue, "Nigrosine Black", "Oil Black", "Spirit Black"/ diamine naphthalenes, diphenyl-amine, hydrazine derivatives, N,N-dimethylamine,■-. urea, laurylamine, cetyl-trimethylammonium chloride, polyamides and polyethyleneimine. (2) Sulphur-containing organic compounds selected from the compounds having a thiocarbynyl, thioether or thioalcohol group, e.g. thioglycolic acid, thiourea, thiocarbanilic acid, thiocarbamic acid, thiobenzoic acid, thioethers according to the general formula R-S-R', where R. and R', which may have the same or different meaning, each stand for an alkyl group such as dimethyl sulphide and ethyl methyl sulphide, mercaptans such as propyl mercaptan and butyl mercaptan, polysulfides, polysulfones, sulfonic acids such as p-toluenesulfonic acid, cyclohexylsulfonic acid, .. , anthraquinonesulfonic acid, methanilic acid; dodecylbenzenesulfonic acid and salts thereof with alkali metals such as sodium and potassium. (3) Oxygenated organic compounds selected from quinones,
ketoner, aldehyder, etere, alkoholer, estere,.. karboksyl syrer og salter derav, sulfoksyder og oksimer, f.eks. p-benzokinon,rantra-kinon, benzofenon, acetofehon, diisopropylketon,formaldehyd, acet-aldehyd, benzaldehyd, oktylalkohol, cetylalkohol, benzylalkohol, fenol, kresol, hematein, propargylalkohol, hydrokinon, fluorescein, etylenglykol, pentaeritritol, glykose, sakkarose, polyvinylalkohol, diisopropyleter, difenyleter, celluloseetere, amylacetat, étyl-benzoat, stearinsyre, benzosyre, salisylsyre, maleinsyre, oksal-syre, tartarsyre, Rochelle-salt eller seignettesalt, ravsyre, isonikotinsyre, fenylglycin, 3-oksy-2-naftosyre, gallussyre, polyacetaler og polyakrylsyrer. ketones, aldehydes, ethers, alcohols, esters,... carboxylic acids and their salts, sulphoxides and oximes, e.g. p-benzoquinone, rantra-quinone, benzophenone, acetopheone, diisopropyl ketone, formaldehyde, acet-aldehyde, benzaldehyde, octyl alcohol, cetyl alcohol, benzyl alcohol, phenol, cresol, hematein, propargyl alcohol, hydroquinone, fluorescein, ethylene glycol, pentaerythritol, glucose, sucrose, polyvinyl alcohol, diisopropyl ether, diphenyl ether, cellulose ethers, amyl acetate, ethyl benzoate, stearic acid, benzoic acid, salicylic acid, maleic acid, oxalic acid, tartaric acid, Rochelle salt or Seignette salt, succinic acid, isonicotinic acid, phenylglycine, 3-oxy-2-naphthoic acid, gallic acid, polyacetals and polyacrylic acids.
(4) Fosforholdige organiske forbindelser utvalgt fra fosfor-(4) Phosphorus-containing organic compounds selected from phosphorus-
og polyfosforsyreestere og alkalimetall- eller ammoniumsalter derav, f.eks. monolaurylfosfat, sorbitanheksametafosfat, poly-oksyetylensorbitantrifosfat og fytinsyre. (5) Tjære, bek, harpikser og vokser med vanskelig definerbar kjemisk struktur. and polyphosphoric acid esters and alkali metal or ammonium salts thereof, e.g. monolauryl phosphate, sorbitan hexametaphosphate, polyoxyethylene sorbitan triphosphate and phytic acid. (5) Tar, pitch, resins and waxes with a difficult to define chemical structure.
Av fargestoffer ifølge forbindelse (a) kan følgende nevnes: Azofargestoffer såsom monoazo-fargestoffer, polyazo-fargestoffer, metallholdige azofargestoffer, naftol-fargestoffer ( azoiske fargestoffer, eng. "azoio dyes" hvor "azolc" står for varinuløslige azo-fargestoffer, sanfå^åzofske fargestoffer) og dispergerte azo-fargestoffer; antrakinon-fargestoffer såsom antrakinonsure fargestoffer, antrakinonkypefargestoff,alizarinfargestoffer; indigoid-fargestoffer såsom "Brilliant Indigo B", "Indanthrene Red Violet RH" og "indanthrene Printing Black B"; svovelfargestoffer såsom "Sulfur Blue FBB" og "Sulfur Black B"; ftalocyaninfargestoffer såsom kobberftalocyanin og metallfrie ftalocyaninforbindelser; nitro- og nitrosofargestoffer; tiazolfargestoffer; xantenfargestoffer; akridinfargestoffer; azinfargestoffer; oksazinfargestoffer; tiazln-fargestoffer; benzokinon- og naftokinonfargestoffer; cyaninfargestoffer; og vannløslige organiske fargestoffer tilhørende alkalimetall-salter av organiske sulfonsyrer såsom "Direct Brilliant Yellow G" (direkte fargestoff), "Acid Light Yellow 2G" Of the dyes according to compound (a), the following can be mentioned: Azo dyes such as monoazo dyes, polyazo dyes, metal-containing azo dyes, naphthol dyes (azo dyes, eng. "azoio dyes" where "azolc" stands for water-insoluble azo dyes, sanfå^ azo dyes) and dispersed azo dyes; anthraquinone dyes such as anthraquinone acid dyes, anthraquinone dye, alizarin dyes; indigoid dyes such as "Brilliant Indigo B", "Indanthrene Red Violet RH" and "indanthrene Printing Black B"; sulfur dyes such as "Sulfur Blue FBB" and "Sulfur Black B"; phthalocyanine dyes such as copper phthalocyanine and metal-free phthalocyanine compounds; nitro and nitroso dyes; thiazole dyes; xanthene dyes; acridine dyes; azine dyes; oxazine dyes; thiazln dyes; benzoquinone and naphthoquinone dyes; cyanine dyes; and water-soluble organic dyes belonging to alkali metal salts of organic sulfonic acids such as "Direct Brilliant Yellow G" (direct dye), "Acid Light Yellow 2G"
(surt fargestoff), "Levafix Yellow 4<g>" (reaktivt fargestoff), "Procion Brilliant Orange G" (reaktivt fargestoff), "Direct Fast Scarlet GS" (direkte fargestoff), "Direct Bordeaux NS" (direkte fargestoff), "Brilliant Scarlet 3R" (surt fargestoff), "Acid Alizarin Red B" ( surt beisefargestoff), "Direct Turkish Blue GL" (acid dye), "Levafix Yellow 4<g>" (reactive dye), "Procion Brilliant Orange G" (reactive dye), "Direct Fast Scarlet GS" (direct dye), "Direct Bordeaux NS" (direct dye), "Brilliant Scarlet 3R" (acid dye), "Acid Alizarin Red B" (acid mordant), "Direct Turkish Blue GL"
(direkte fargestoff), "Cibacron Blue 3G" (reaktivt fargestoff), "Blankophor B" (surt fargestoff), "Nigrosine" (surt fargestoff) (direct dye), "Cibacron Blue 3G" (reactive dye), "Blankophor B" (acid dye), "Nigrosine" (acid dye)
og "Sirius Gray G" (direkte fargestoff); alkalimetallsalter av karboksylsyrer såsom "Chrysamine G" (direkte fargestoff), "Direct Fast Yellow GG" (direkte fargestoff), "Chrome Yellow G" and "Sirius Gray G" (direct dye); alkali metal salts of carboxylic acids such as "Chrysamine G" (direct dye), "Direct Fast Yellow GG" (direct dye), "Chrome Yellow G"
(surt beisefargestoff), "Chrome Yellow ME" (surt beisefargestoff) og "Eosine G" (surt fargestoff); kvaternære ammoniumsalter såsom "Basic Flavln 8g" (basisk fargestoff), "Astrazon Yellow 3G" (acid mordant dye), "Chrome Yellow ME" (acid mordant dye) and "Eosine G" (acid mordant); quaternary ammonium salts such as "Basic Flavln 8g" (basic dye), "Astrazon Yellow 3G"
(basisk-fargestoff), "Rhodåmirie 6GCP" (basisk fargestoff), "Safranine T" (basisk fargestoff), "(Rhodamine B" (basisk fargestoff),, og "Daltophor AN" (basisk fargestoff); og hydroklorider såsom "Auramine Conc" (basisk fargestoff),. "Chrysoidine" (basisk fargestoff) og "Bismarck Brown BG" (basisk fargestoff). (basic dye), "Rhodåmirie 6GCP" (basic dye), "Safranine T" (basic dye), "(Rhodamine B" (basic dye), and "Daltophor AN" (basic dye); and hydrochlorides such as "Auramine Conc" (basic dye), "Chrysoidine" (basic dye) and "Bismarck Brown BG" (basic dye).
De ovenfor nevnte organiske polare forbindelsene og organiske , fargestoffene kan anvendes hver for seg.eller i kombinasjon med; -.; The above-mentioned organic polar compounds and organic dyes can be used separately or in combination with; -.;
hverandre.- ■■■■ l':;,-.;. ■•' ^ ■ '" ''■'■' each other.- ■■■■ l':;,-.;. ■•' ^ ■ '" ''■'■'
Dernest kan på den ene; side forbindelsene, som betegnés som ■ forbindelser (b) og som er anvendbare ved- fremgangsmåten ifølge nærværende•oppfinnelse, utvelges fra halogenidene., oksydene, hydroksydene,og lavere karboksylater med 1 til 8 karbonatomer av metall-elemehter. De kan eksemplifiseres ved hjelp av: alkaII-metåller såsom .natrium og kalium; jordalkalimetaller såsom magnesium, kalsium'og barium; metaller fra sinkgrupperi såsom sink; metaller fra alumihiumgruppen såsom aluminium; metaller fra tinngruppen såsom' titan og tinnj metaller frå Jerngruppen såsom Jern og nikkel; metaller fra kromgruppen:såsom krom og molybden; metaller fra rna riga ngruppe n:såsom mangan;.metaller, fra kobbergruppen såsom kobber og sølv; og metaller fra platina- \ gruppen såsom platina.^Illustrative eksempler på disse forbindelser er natriumfluorid, natriumacetat, jern-rll-klorld, kalsiumklorid,' kaliumklorid,. natriumtartrat, natriumklorid,. kalsiumacétat., Secondly can on the one; on the other hand, the compounds, which are designated as ■ compounds (b) and which are usable in the method according to the present • invention, are selected from the halides, the oxides, the hydroxides, and lower carboxylates with 1 to 8 carbon atoms of metal elements. They can be exemplified by: alkali metals such as sodium and potassium; alkaline earth metals such as magnesium, calcium and barium; metals from the zinc group such as zinc; metals from the aluminum group such as aluminium; metals from the tin group such as titanium and tin; metals from the iron group such as iron and nickel; metals from the chromium group: such as chromium and molybdenum; metals from the rna riga ngroup n:such as manganese;.metals, from the copper group such as copper and silver; and metals from the platinum group such as platinum. Illustrative examples of these compounds are sodium fluoride, sodium acetate, ferric chloride, calcium chloride, potassium chloride. sodium tartrate, sodium chloride,. calcium acetate.,
natriumoksalat, aluminiumklorid, kobber-II-klorid, jernoktoat og tlnn-IV-klorid.. '•■ sodium oxalate, aluminum chloride, copper II chloride, ferric octoate and tlnn IV chloride.. '•■
På den annen side utvelges forbindelsene (b) fra oksosyrer av elementene tilhørende den 2.e til 6.e perioden, og da gruppene IIB og III til VII i det periodiske system samt uorganiske salter av oksosyrene. Eksempler på elementene . er: sink, bor, aluminium,, karbon, silisium, tinn, titan, nitrogen, fosfor, svovel, .'krom, molybden, wolfram, klor og mangan. On the other hand, the compounds (b) are selected from oxoacids of the elements belonging to the 2nd to 6th period, and then groups IIB and III to VII in the periodic table as well as inorganic salts of the oxoacids. Examples of the elements. are: zinc, boron, aluminium,, carbon, silicon, tin, titanium, nitrogen, phosphorus, sulphur, chromium, molybdenum, tungsten, chlorine and manganese.
Illustrative oksosyrer og salter derav ertsinksyre, borsyre, aluminiumsyre, karbonsyre,.kiselsyre, tinnsyre, titansyre, fosforsyrer omfattende, ortosyre samt dehydratiserte og kondenserte fosforsyrer såsom metafosforsyre,. pyrofosforsyre og tripolyfosfor-syre, salpetersyre, svovelsyre, kromsyre, molybdensyre, wolfram-syre, mangansyre, saltsyre så vel sOm permangansyre og bikrom-syre med høyere oksydas joirstrinn, salpetersyrling', hy po salpeter-syrling, fosforsyrling, hypofosforsyre og hypofosforsyrlinger med lavere oksydasjonstrinn samt salter av de ovenfor nevnte oksosyrer med ammonium, alkalimetaller eller jordålkalimetaller. Illustrative oxo acids and salts thereof ore zinc acid, boric acid, aluminum acid, carbonic acid, silicic acid, stannous acid, titanic acid, phosphoric acids including, ortho acid as well as dehydrated and condensed phosphoric acids such as metaphosphoric acid. pyrophosphoric acid and tripolyphosphoric acid, nitric acid, sulfuric acid, chromic acid, molybdic acid, tungstic acid, manganic acid, hydrochloric acid as well as permanganic acid and bichromic acid with a higher degree of oxidation, nitric acid, hypo nitric acid, phosphoric acid, hypophosphoric acid and hypophosphoric acid with a lower oxidation step as well as salts of the above-mentioned oxo acids with ammonium, alkali metals or alkaline earth metals.
Ved utførelse av fremgangsmåten ifølge nærværende oppfinnelse erWhen carrying out the method according to the present invention is
det fordelaktig at forbindelsene (a) og (b) blir oppløst eller dispergert separat eller i kombinasjon i et egnet løsningsmiddel eller egnede løsningsmidler før man forétar oyertrekkingen eller behandlingen. Som løsningsmiddel anvendes vanligvis vann, alkoholiske løsningsmidler, ester-løsningsmidler, keton-løsnings-midler, hydrokarbon-løsningsmidler og klorerte hydrokarbon-løsningsmidler i henhold til forbindelsenes løslighet eller dispergerbarhet. it is advantageous that the compounds (a) and (b) are dissolved or dispersed separately or in combination in a suitable solvent or suitable solvents before carrying out the oyer extraction or the treatment. Water, alcoholic solvents, ester solvents, ketone solvents, hydrocarbon solvents and chlorinated hydrocarbon solvents are usually used as solvents according to the solubility or dispersibility of the compounds.
I det følgende skal tre foretrukkede utførelsesformer for overtrekking eller behandling av overflatene med forbindelsene (a) og (b) i henhold til fremgangsmåten ifølge oppfinnelsen beskrives: 1. Forbindelse (a) oppløses eller.dispergeres 1 ett av.de ovenfor nevnte' løsningsmidlene, og den. erholdte løsning eller dispersjon påføres overflatene til reaktorens innervegger og andre deler som kommer i kontakt med monomeren eller monomerene. Deretter blir de således overtrukkede overflatene brakt I kontakt eller behandlet med forbindelse (b) ved å tilsette dens løsning eller dispersjon til reaktoren, oppvarme løsningen eller dispersjonen fortrinnsvis ved .50 til 100°C i 10 minutter eller mer, hvoretter man fjerner løsningen eller dispersjonen fra reaktoren, og hvoretter man foretar polymerisasjon i den samme reaktoren under tilsetning av additiver før og under polymerisasjonen. , I tilfelle , polymerisasjonsmedlet er vandig,som ved suspensjonspolymerisasJon eller emulsjonspolymerisasjon, og når løsningsmidlet som anvendes for å danne løsningen eller dispersjonen av forbindelsen (b) er vann, er det ikke alltid nødvendig å.fjerne den vandige løsningen eller dispersjonen etter'oppvarmingen. ' 2. Forbindelse (a) oppløses eller dispergeres' i et egnet løsnings-middel, mens forbindelse (b) .oppløses eller dispergeres separat i det samme eller et annet løsningsmiddel. Løsningen eller. In the following, three preferred embodiments for coating or treating the surfaces with compounds (a) and (b) according to the method according to the invention will be described: 1. Compound (a) is dissolved or dispersed in one of the above-mentioned solvents, and that one. obtained solution or dispersion is applied to the surfaces of the inner walls of the reactor and other parts that come into contact with the monomer or monomers. Then the surfaces thus coated are contacted or treated with compound (b) by adding its solution or dispersion to the reactor, heating the solution or dispersion preferably at .50 to 100°C for 10 minutes or more, after which the solution or dispersion is removed from the reactor, after which polymerization is carried out in the same reactor with the addition of additives before and during the polymerization. In the event that the polymerization agent is aqueous, as in suspension polymerization or emulsion polymerization, and when the solvent used to form the solution or dispersion of compound (b) is water, it is not always necessary to remove the aqueous solution or dispersion after heating. 2. Compound (a) is dissolved or dispersed in a suitable solvent, while compound (b) is dissolved or dispersed separately in the same or another solvent. The solution or.
dispersjonen av forbindelse (b) tilsettes til løsningen eller dispersjonen av. forbindelse (a) eller omvendt, etterfulgt av oppvarming til fortrinnsvis 50 til 100°C. Den erholdte.blandingen påføres overflatene til innerveggene og andre deler i reaktoren som kommer i kontakt med monomeren eller monomerene. Hvis nødvendig, vaskes de således overtrukkede overflatene med vann. Deretter foretas polymerisasjon ved hjelp av fremgangsmåten som er beskrevet tidligere. the dispersion of compound (b) is added to the solution or dispersion of. compound (a) or vice versa, followed by heating to preferably 50 to 100°C. The resulting mixture is applied to the surfaces of the inner walls and other parts of the reactor which come into contact with the monomer or monomers. If necessary, the thus coated surfaces are washed with water. Polymerization is then carried out using the method described earlier.
3. Separate løsninger eller dispersjoner av forbindelsene (a) og (b) fremstilles i samme eller forskjellige løsningsmidler. Løsningen eller dispersjonen av forbindelse (a) og løsningen eller dispersjonen av forbindelse (b) påføres vekselvis en eller flere ganger overflatene som kommer i kontakt med monomeren eller monomerene. De således overtrukkede overflatene blir gjenstand for varmebehandling ved at vann eller vanndamp sendes gjennom reaktorens mantel eller ved at varm luft blåses inn i reaktoren. En foretrukket utførelses-form for påføring av belegg-løsriingen eller -dispersjonen er at man under arbeidsprosessen holder innerveggens temperatur ved 50 til 100°C ved å sende varmt vann eller vanndamp gjennom mantelen. Ennå mer foretrukket er det å fullføre påføringen av løsningen 3. Separate solutions or dispersions of compounds (a) and (b) are prepared in the same or different solvents. The solution or dispersion of compound (a) and the solution or dispersion of compound (b) are alternately applied one or more times to the surfaces that come into contact with the monomer or monomers. The thus coated surfaces are subjected to heat treatment by sending water or steam through the reactor's mantle or by blowing hot air into the reactor. A preferred embodiment for applying the coating release or dispersion is that during the work process the temperature of the inner wall is kept at 50 to 100°C by sending hot water or steam through the mantle. Even more preferred is to complete the application of the solution
eller dispersjonen ved samtidig å sende varmt vann eller vanndamp gjennom mantelen samt blåse varm,luft inn i reaktoren under den tid påføringen av overtrekket pågår..'or the dispersion by simultaneously sending hot water or water vapor through the mantle and blowing hot air into the reactor during the time the coating is being applied..'
Det er naturligvis mulig å utføre to eller tre av de ovennevnte arbeidsoperasjoner i kombinasjon. Når to eller flere av forbindelsene (a) anvendes i kombinasjon er det tilrådlig at minst en av ,dem er en vannløslig organisk forbindelse eller et vannløslig organisk fargestoff og minst en av dem vannuløsllg. Herved fås, som vist I eksemplene, bedre resultater. It is naturally possible to carry out two or three of the above work operations in combination. When two or more of the compounds (a) are used in combination, it is advisable that at least one of them is a water-soluble organic compound or a water-soluble organic dye and at least one of them is water-insoluble. In this way, as shown in the examples, better results are obtained.
I hvert av de ovennevnte utførelsesformer er. det viktig at fobindelsene (a) og (b) bringes.i,kontakt med hverandre ved en høyere temperatur, som overstiger 50°C, i l time. Hvis temperaturen er lavere enn 5.0°C, når" kontakt finner sted,. vil man ikke oppnå tilfredsstillende resultater, eller man må anvende 10 timer 'eller mer på behandlingen. In each of the above embodiments is. it is important that the fob parts (a) and (b) are brought into contact with each other at a higher temperature, exceeding 50°C, for 1 hour. If the temperature is lower than 5.0°C when contact takes place, satisfactory results will not be obtained, or 10 hours or more will have to be applied to the treatment.
Ifølge nærværende oppfinnelse vil mengdene av forbindelsene (a)According to the present invention, the amounts of the compounds (a)
og (b) eller en blanding åy disse, og som anvendes for belegging av overflatene av innerveggene og andre deler tilhørende polymerisasjonsreaktoren, kunne variere avhengig av forbindelsene, polymerisasjonstyper, overtrekkingsmetode eller behandlingsmåte samt andre faktorer. Mengden av de nevnte.forbindelser er imidlertid vanligvis minst 0,0001 g/m , eller fortrinnsvis fra 0,005 til 1,0 g/m<2>, hvilket er tilstrekkelig for å oppnå tilfredsstillende effekt med hensyn til å hindre polymerskallavsetning. and (b) or a mixture of these, and which is used for coating the surfaces of the inner walls and other parts belonging to the polymerization reactor, could vary depending on the compounds, polymerization types, coating method or treatment method and other factors. However, the amount of the said compounds is usually at least 0.0001 g/m, or preferably from 0.005 to 1.0 g/m<2>, which is sufficient to achieve a satisfactory effect with respect to preventing polymer scale deposition.
Mengdeforholdene av forbindelse (b) til (a) varierer avhengig av overtrekkingsmetode eller behandlingsmetode. Ved den ovenfor beskrevne første utførelsesformen hvor konsentrasjonen av forbindelse (b) i løsningen, som fyller polymerisasjonsreaktoren som har overflater overtrukket med forbindelse (a), vanligvis er meget lav, bør f.eks. mengden av forbindelse (b) nødvendigvis være stor, og vektsforholdet av forbindelsene (b) til (a) ligger, fortrinnsvis i området fra 0,1 til 500. På den annen side vil The quantity ratios of compound (b) to (a) vary depending on the coating method or treatment method. In the above-described first embodiment where the concentration of compound (b) in the solution, which fills the polymerization reactor which has surfaces coated with compound (a), is usually very low, e.g. the amount of compound (b) must necessarily be large, and the weight ratio of the compounds (b) to (a) lies, preferably in the range from 0.1 to 500. On the other hand,
ved den andre utførelsesformen, hvor en blanding eller et reaksjonsprodukt av forbindelsene (a) og (b) anvendes som overtrekkingsmateriale, vektsforholdet mellom forbindelsene (b) in the second embodiment, where a mixture or a reaction product of the compounds (a) and (b) is used as coating material, the weight ratio between the compounds (b)
og (a) i området fra 0,01 til 50 gi tilfredsstillende resultater. and (a) in the range from 0.01 to 50 give satisfactory results.
Videre kan effekten som oppnås ved fremgangsmåten ifølge nærværende oppfinnelse med hensyn til å hindre polymerskallavsetning forsterkes ved å tilsette til polymerisasjonsblandingen minst en av de ovenfor nevnte oksosyrene, salter derav og reaksjonsproduktene av forbindelsene (a) og (b). Man skal imidlertid merke seg at mengden av disse additiver ikke bør overstige 1000 p.p.m., eller i enkelte tilfeller 100 p.p.m., beregnet på den totale vekten av monomeren eller monomerene, da en større mengde kan ha uheldig innflytelse på kvaliteten av det erholdte polymerproduktet. Furthermore, the effect achieved by the method according to the present invention with regard to preventing polymer shell deposition can be enhanced by adding to the polymerization mixture at least one of the above-mentioned oxo acids, salts thereof and the reaction products of the compounds (a) and (b). However, it should be noted that the amount of these additives should not exceed 1000 p.p.m., or in some cases 100 p.p.m., calculated on the total weight of the monomer or monomers, as a larger amount may have an adverse influence on the quality of the polymer product obtained.
Dessuten kan effekten med hensyn til å hindre polymerskallavsetning ytterligere forsterkes, og da spesielt når polymerisasjonen utføres i et vandig medium, ved å alkallsere det. vandige mediet til en pH-verdl mellom 8 og 11. Hvis forbindelse (b), som tilsettes polymerisas jonsblandingen', ikke er alkalisk,, så kan andre''egnede alkaliske forbindelser tilsettes for oppnåelse av de ovennevnte pH-verdier. Moreover, the effect with regard to preventing polymer shell deposition can be further enhanced, and especially when the polymerization is carried out in an aqueous medium, by alkalizing it. water the medium to a pH value between 8 and 11. If compound (b), which is added to the polymerization mixture, is not alkaline, then other suitable alkaline compounds can be added to achieve the above-mentioned pH values.
Fremgangsmåten ifølge nærværende oppfinnelse er anvendbar i forbindelse med enhver type polymerisasjon av vinylklorid eller kopolymerisasjon av vinylklorid méd en eller flere komon<p>merér, The method according to the present invention is applicable in connection with any type of polymerization of vinyl chloride or copolymerization of vinyl chloride with one or more comonomers,
og da de typer som omfatter suspensjonspolymerisasjon, emulsjons-polymerisas jon, løsningspolymerisasjon og massepolymerisasjon, og under forutsetning av at polymerisasjonen;utføres under tilsetning av minst ett additiv til- polymerisasjonsblandingen før eller under selve polymerisas jonen. and then the types that include suspension polymerization, emulsion polymerization, solution polymerization and mass polymerization, and on the condition that the polymerization is carried out with the addition of at least one additive to the polymerization mixture before or during the actual polymerization.
Anvendte additiver er slike- som vanligvis blandes med polyvinylkloridharpikser i fabrikasjonsprosessen. Denevnte additiver omfatter myknere, smøremidler, fyllstoffer, .forsterkningsmidler, fargestoffer og antistatiske midler såvel som antioksydanter. Additives used are those which are usually mixed with polyvinyl chloride resins in the manufacturing process. Said additives include plasticizers, lubricants, fillers, reinforcing agents, dyes and antistatic agents as well as antioxidants.
og absorbsjonsmidler for ultraviolett lys, og da i mengder som'and absorbents for ultraviolet light, and then in quantities that
ikke har inhiberende effekt på polymerisasjonen. I det følgende gis eksempler på additiver.. does not have an inhibitory effect on the polymerization. In the following, examples of additives are given.
Myknere: ftalsyreester såsom dioktylftalat, dibutylftalat og dimetylftalatj blandingsestere av ftalsyre, såsom butylbenzyl-ftalat; estere av alifatiske dibasiske syrer såsom dioktyladipat, dioktylazelat og dioktylsebadat»estere av.polyvalente alkoholer såsom dietylenglykoldibenzoat og estere av pentaeritritol; estere av alifatiske syrer såsom butyloleat og metylacetylricinolat; fosforsyreestere såsom trikresylfosfat,. trioktylfosfat og trifenyl-fosfat; og epoksy-myknere såsom soyabønneolJe-epoksyd, linfrøolje-epoksyd og 2-etylhéksylepoksyheksahydroftalat. Plasticizers: phthalic acid esters such as dioctyl phthalate, dibutyl phthalate and dimethyl phthalate; mixed esters of phthalic acid such as butyl benzyl phthalate; esters of aliphatic dibasic acids such as dioctyl adipate, dioctyl azelate and dioctyl sebate; esters of polyvalent alcohols such as diethylene glycol dibenzoate and esters of pentaerythritol; esters of aliphatic acids such as butyl oleate and methyl acetyl ricinolate; phosphoric acid esters such as tricresyl phosphate,. trioctyl phosphate and triphenyl phosphate; and epoxy plasticizers such as soybean oil epoxide, linseed oil epoxide and 2-ethylhexylepoxyhexahydrophthalate.
Varmestabilisatorer: uorganiske blysalter såsom tribasisk blysulfat, dibasisk blyfosfitt og basisk blysilikosulfat; metallsåpe såsom blystearat, bariumricinolat, kalsiumlaurat, kalsiumstearat og Heat stabilizers: inorganic lead salts such as tribasic lead sulfate, dibasic lead phosphite and basic lead silicosulfate; metal soap such as lead stearate, barium ricinolate, calcium laurate, calcium stearate and
sinkstearat; organo'tinn-f orbindelser såsom dibutyltinndimetylmaleat,-dioktyltinndilaurat, dibutyltinnlaurat,. dibutyltinn-S,S.' •■ bis(isooktylmerkaptoacetat) og dioktyltinndilaurylmerkaptid; epoksyforbindelser og estere av orgahofosfitter zinc stearate; organotin compounds such as dibutyltin dimethyl maleate, dioctyltin dilaurate, dibutyltin laurate. dibutyltin-S,S.' •■ bis(isooctyl mercaptoacetate) and dioctyltin dilauryl mercaptide; epoxy compounds and esters of organophosphites
Antioksydanter: Bisfenoler såsom 2,2-bis'(4-hydroksyfenyl.)-propan (bisfenol A) og bis(2-hydroksy-5-klorfenyl)sulfLd; 2,4-dihydroksybenzofenon; 2-hydroksy-4-metoksybenzofenon<p>g fenylsålisylat. Antioxidants: Bisphenols such as 2,2-bis'(4-hydroxyphenyl)-propane (bisphenol A) and bis(2-hydroxy-5-chlorophenyl)sulfLd; 2,4-dihydroxybenzophenone; 2-hydroxy-4-methoxybenzophenone<p>g phenylsol salicylate.
Absorberingsmidler for ultraviolett lys: benzofenonderivater såsom 2,4-dihydroksybenzofenon og 2-hydroksy-4-metoksybenzfenon; benzotriazolderivater såsom 2-(2'-hydroksy-5'-metylfenyl)-benzotriazol og 2-(2'-hydroksy-3' »<5>'-di-tert.-butylfenyl)-benzotriazol; og sallsylsyreestere såsom fenylsålisylat og 4-oktylfenylsålisylat. Ultraviolet light absorbers: benzophenone derivatives such as 2,4-dihydroxybenzophenone and 2-hydroxy-4-methoxybenzphenone; benzotriazole derivatives such as 2-(2'-hydroxy-5'-methylphenyl)-benzotriazole and 2-(2'-hydroxy-3'-<5>'-di-tert-butylphenyl)-benzotriazole; and salicylic acid esters such as phenyl salicylate and 4-octylphenyl salicylate.
Antistatiske midler: anioniske overflateaktive midler såsom fettsyresalter, salter av sulfatestere med høyere alkoholer samt salter av sulfatestere med flytende fettoljer; katloniske overflateaktive midler såsom salter av alifatiske aminer og kvaternære amrnoniumsalter; og ikke-ioniske overf lateaktive midler såsom polyoksyetylenalkyletere og sorbitanalkylestere. Antistatic agents: anionic surfactants such as fatty acid salts, salts of sulfate esters with higher alcohols as well as salts of sulfate esters with liquid fatty oils; cationic surfactants such as salts of aliphatic amines and quaternary ammonium salts; and nonionic surfactants such as polyoxyethylene alkyl ethers and sorbitan alkyl esters.
Fyllstoffer: pulverformig kisel, kalsiumkarbonat, leire og . kalsiumsilikat. Fillers: powdered silica, calcium carbonate, clay and . calcium silicate.
Fargestoff: titandioksyd, kjønrøk, blymonooksyd og gult Jernoksyd. Colourant: titanium dioxide, carbon black, lead monoxide and yellow iron oxide.
Smøremidler: flytende parafin,, fast parafin, vokser, voksige hydrokarboner såsom polyetylenvoks, høyere fettsyrer såsom stearinsyre og laurinsyre, amider av fettsyrer såsom stearinsyre-amid, estere såsom butylstearat, fettoljer såsom herdet ricinus-olje, høyere alkoholer såsom cetylalkohol og stearylalkohol og metallsåpe såsom blystearat. Lubricants: liquid paraffin, solid paraffin, waxes, waxy hydrocarbons such as polyethylene wax, higher fatty acids such as stearic acid and lauric acid, amides of fatty acids such as stearic acid amide, esters such as butyl stearate, fatty oils such as hydrogenated castor oil, higher alcohols such as cetyl alcohol and stearyl alcohol and metallic soap such as lead stearate.
Forsterkningsmidler: polymetylmetakrylat, etylenvinylacetat-kopolymerer og ternære kopolymerer av etylenpropylencyklopentadien og podete kopolymererderivater derav. Reinforcing agents: polymethyl methacrylate, ethylene vinyl acetate copolymers and ternary copolymers of ethylene propylene cyclopentadiene and graft copolymer derivatives thereof.
I henhold til fermgangsmåten ifølge nærværende oppfinnelse er tiden, mengden og fremgangsmåten faktorer ved tilsetningen av dei- ovennevnte additiver ikke begrensende for oppfinnelsen, According to the process according to the present invention, the time, amount and method are factors in the addition of the above-mentioned additives not limiting the invention,
og de nevnte faktorer bør velges slik at den forblandede polyvinylkloridharpiksen har de ønskede egenskaper. Vanligvis tilsettes de enten før eller under selve polymerisasjonen. and the aforementioned factors should be chosen so that the premixed polyvinyl chloride resin has the desired properties. Usually they are added either before or during the polymerization itself.
Fremgangsmåten ifølge nærværende oppfinnelse er anvendbar ved enhver type polymerisasjon av vinylklorid omfattende suspensjonspolymerisasjon, emulsjonspolymerisasjon, løsningspolymerisasjon og massepolymerisasjon. Fremgangsmåten er ikke begrenset av polymerisasJonsbetingelsene med hensyn til additiver, f.eks. polymerisasjonsinitiatorer, suspensjonsmidler, emulgeringsmidler, kjedeoverførings-midler og lignende, polymerisasjonstemperatur, agiteringsstyrke etc. Videre er fremgangsmåten ifølge nærværende oppfinnelse anvendbar ikke bare ved homopolymerisasjon av vinylklorid men også ved kopolymerisasjon av. vinylklorid med en eller flere kopolymeriserbare monomerer såsom vinylestere, vinyletere, akrylsyre, metakrylsyre og estere derav, måleinsyre, fumarsyre og estere derav, maleinsyreanhydrid, aromatiske vinylmonomerer, vinylhalogenider unntatt vinylklorid, vinylidenhalogenider, umettede nitriler og olefiner. The method according to the present invention is applicable to any type of polymerization of vinyl chloride, including suspension polymerization, emulsion polymerization, solution polymerization and bulk polymerization. The method is not limited by the polymerization conditions with regard to additives, e.g. polymerization initiators, suspension agents, emulsifiers, chain transfer agents and the like, polymerization temperature, agitation strength, etc. Furthermore, the method according to the present invention is applicable not only for homopolymerization of vinyl chloride but also for copolymerization of. vinyl chloride with one or more copolymerisable monomers such as vinyl esters, vinyl ethers, acrylic acid, methacrylic acid and their esters, maleic acid, fumaric acid and their esters, maleic anhydride, aromatic vinyl monomers, vinyl halides except vinyl chloride, vinylidene halides, unsaturated nitriles and olefins.
De etterfølgende eksempler skal ytterligere anskueliggjøre oppfinnelsen uten å begrense denne. I tabellene graderes polymerskallavsetningen med (a), (b) pg (c) i henhold til mengden, (a) angir skallavsetning på de fleste overflater I reaktoren; (b) angir skallavsetning på deler av'overflatene, nemlig opptil 50#i og (c) angir liten skallavsetning. The following examples shall further illustrate the invention without limiting it. In the tables, the polymer shell deposition is graded with (a), (b) and (c) according to the amount, (a) indicates shell deposition on most surfaces in the reactor; (b) indicates shell deposition on parts of the surfaces, namely up to 50#i and (c) indicates small shell deposition.
Eksempel 1.Example 1.
Til en 2-liters rustfri stålautoklav, som var utstyrt med en turbinblad-agitator, ble det chargert 900 g avionisert vann, 5 g kalsiumstearat, 3 g dioktylftalat, 0,9 g polyvinylalkohol, 15 g kalsiumkarbonat og 20 g oksydert LD-polyetylen. Etter 60 minutters agitering ved 60°C og fjerning av oksygen fra autoklavén ved gjentatte evakueringer bg tilføring av nitrogengass ble 600 g vinylkloridmonomer og 0,25 g , ' -azobisdimetylvaleronitril tilsatt til blandingen, hvoretter det ble foretatt suspensjonspolymerisasjon ved 57°C i ca. 5 timer ved en agitatorhastighet på 1000 o.p.m.. To a 2 liter stainless steel autoclave, which was equipped with a turbine blade agitator, was charged 900 g of deionized water, 5 g of calcium stearate, 3 g of dioctyl phthalate, 0.9 g of polyvinyl alcohol, 15 g of calcium carbonate and 20 g of oxidized LD polyethylene. After 60 minutes of agitation at 60°C and removal of oxygen from the autoclave by repeated evacuations by adding nitrogen gas, 600 g of vinyl chloride monomer and 0.25 g of ,'-azobisdimethylvaleronitrile were added to the mixture, after which suspension polymerization was carried out at 57°C for approx. 5 hours at an agitator speed of 1000 rpm.
Før tilsetningen av de ovennevnte materialer til autoklavén ble overflatene til veggene og autoklavens agitator overtrukket med et fargestoff (forbindelse A),slik som vist i tabell 1, 1 et mengdeforhold som tilsvarer ca. 0,05 g/m tørrstoff ved appliserIng av én 0,l$~ig etanolisk løsning eller dispersjon av fargestoffet, etterfulgt av tørking ved 70°C i 30 minutter. Deretter ble overflatene ytterligere overtrukket med en l$-ig vandig løsning eller dispersjon av en oksosyre eller et salt av oksosyre (forbindelse B), slik som vist i tabellen, i et mengdeforhold som tilsvarer 0,05 g/m'" tørrstoff, hvoretter tørking ved 70°C i 60 minutter foretas. Before the addition of the above-mentioned materials to the autoclave, the surfaces of the walls and the agitator of the autoclave were coated with a dye (compound A), as shown in Table 1, 1 a quantity ratio corresponding to approx. 0.05 g/m dry substance by application of one 0.l$~ig ethanolic solution or dispersion of the dye, followed by drying at 70°C for 30 minutes. Then, the surfaces were further coated with a 15-µg aqueous solution or dispersion of an oxo acid or a salt of an oxo acid (compound B), as shown in the table, in a quantity ratio corresponding to 0.05 g/m'" dry matter, after which drying at 70°C for 60 minutes is carried out.
Etter fullføring av hver polymerisasjonskjøring ble overflatene undersøkt med hensyn til skallavsetning. Resulatatene vises i After completion of each polymerization run, the surfaces were examined for scale deposition. The results are shown in
tabellen.the table.
For sammenligning ble overflatene overtrukket enten med forbindelse A eller forbindelse B i et mengdeforhold som tilsvarer 0,1 g/m<2>tørrstoff, og den samme polymerisasjon ble utført. Resultatene vises i tabellene II og III. For comparison, the surfaces were coated with either compound A or compound B in a quantity ratio corresponding to 0.1 g/m<2>dry matter, and the same polymerization was carried out. The results are shown in Tables II and III.
Eksempel 2 Example 2
Til samme polymerisasjonsreaktor som ble anvendt i eksempel 1To the same polymerization reactor as used in example 1
ble det chargert 100 g soyabønneolje-epoksyd, 12 g titandioksyd, 5-g parafinvoks, 2 g dioktylftalat og 100 g avionisert'vann, 100 g of soybean oil epoxy, 12 g of titanium dioxide, 5 g of paraffin wax, 2 g of dioctyl phthalate and 100 g of deionized water were charged,
og deretter foretok man blanding ved 60°C i 90 minutter. Deretter ble 0,8 g polyvinylalkohol, 0,4 h metylceilulose og 800 g avionisert vann tilsatt og blandet ved 50°C i J>0 minutter. Etter and then mixing was carried out at 60°C for 90 minutes. Then 0.8 g of polyvinyl alcohol, 0.4 h of methyl cellulose and 800 g of deionized water were added and mixed at 50°C for 10 minutes. After
fjerning av oksygen fra reaktorens indre ved hjelp av fortrengning'med nitrogen ble 600 g vinylkloridmonomer og 0,2 g cx, Øi'-azobisdimetylvaleronitril tilsatt til blandingen, hvoretter man foretok suspensjonspolymerisasjon under oppvarming ved 60°C og agitering removal of oxygen from the interior of the reactor by means of displacement' with nitrogen, 600 g of vinyl chloride monomer and 0.2 g of cx, Øi'-azobisdimethylvaleronitrile were added to the mixture, after which suspension polymerization was carried out under heating at 60°C and agitation
ved 1000 o.p.m. 15 timer, og ved slutten av polymerisasjonen tilsattes 8 g dibutyltinn-S,S'-bis(isooktylmerkaptoacetat) under kontinuerlig agitering i ytterligere 30 minutter. at 1000 rpm 15 hours, and at the end of the polymerization, 8 g of dibutyltin-S,S'-bis(isooctyl mercaptoacetate) were added with continuous agitation for a further 30 minutes.
Før tilføringen av ovennevnte materialer til reaktoren,ble reaktorens vegger overtrukket med forbindelsene A og B, slik Before the addition of the above materials to the reactor, the walls of the reactor were coated with compounds A and B, as
som vist i tabell IV, Og på samme måte som beskrevet i eksempel 1. as shown in Table IV, And in the same manner as described in Example 1.
Polymerskallavsetningen etter hver fullført polymerisasjonskjøring ble undersøkt. Resultatene vises i tabellen. The polymer shell deposition after each completed polymerization run was investigated. The results are shown in the table.
For å sammenligne ble samme arbeidsoperasjon gjentatt, men da med den forandring at forbindelsene A og B ble anvendt hver for seg og ikke i kombinasjon som beleggmateriale. Resultatene av disse forsøk vises også i tabellen. In order to compare, the same work operation was repeated, but then with the change that compounds A and B were used separately and not in combination as coating material. The results of these tests are also shown in the table.
Eksempel 3. Example 3.
Til samme polymerisasjonsreaktor som anvendt i eksempel 1 bleTo the same polymerization reactor as used in example 1 was
det chargert 8 g dioktylftalat, 12 g titandioksyd, 6 g kalsiumkarbonat, 8 g parafinvoks og 100 g avionisert vann, hvoretter man foretok blanding ved 70°C I 2 timer. Deretter ble 0,8 g polyvinylalkohol, 0,3 g metylcellulose og 800 ,g avionisert vann tilsatt og blandet ved 50°C i 30 minutter. Etter fjerning av oksygen fra reaktorens innside ved fortrengning med nitrogen ble 550 g vinylkloridmonomer og 0,22 g ^x, c*'-azobisdimetylvaleronitril tilsatt. Deretter fulgte,suspensjonspolymerisasjon under oppvarming ved 57°C og agitering ved 1000 o.p.m. i 6 timer. Ved slutten av polymerisas jonen tilsattes lg blsfenol A og 8".g kalsiurnutearat til .polymerisasjonsblandingen, og deretter foretok man agitering ved 60°C i ytterligere 1 time. 8 g of dioctyl phthalate, 12 g of titanium dioxide, 6 g of calcium carbonate, 8 g of paraffin wax and 100 g of deionized water were charged, after which mixing was carried out at 70°C for 2 hours. Then 0.8 g of polyvinyl alcohol, 0.3 g of methyl cellulose and 800 g of deionized water were added and mixed at 50°C for 30 minutes. After removing oxygen from the inside of the reactor by displacement with nitrogen, 550 g of vinyl chloride monomer and 0.22 g of x,c*'-azobisdimethylvaleronitrile were added. This was followed by suspension polymerization under heating at 57°C and agitation at 1000 rpm. for 6 hours. At the end of the polymerization, 1 g of chlorophenol A and 8 g of calcium neutearate were added to the polymerization mixture, and then agitation was carried out at 60°C for a further 1 hour.
Før tilføringen av ovennevnte materialer til reaktoren, ble reaktorens vegger overtrukket med forbindelser A og B, slik som vist i tabell V, og på samme måte som beskrevet i eksempel 1. Polymerskallavsetningen ble bestemt, etter fullføring av hver polymerisasjonskjøring, og resultatene vises i tabellen. Prior to the addition of the above materials to the reactor, the walls of the reactor were coated with compounds A and B, as shown in Table V, and in the same manner as described in Example 1. The polymer shell deposition was determined, after completion of each polymerization run, and the results are shown in the table .
Det ble utført sammenligningsforsøk hvor enten forbindelse A eller forbindelse B hver for seg ble anvendt som beleggmateriale. Resulatatene vises i nedenstående tabell V. Comparison experiments were carried out where either compound A or compound B were used separately as coating material. The results are shown in Table V below.
Eksempel 4. Example 4.
Forsøk ble utført under samme betingelser som beskrevet i eksempel 3 med unntagelse for at polymerisasjonen var en kopolymerisasjon av en monomer blanding bestående av 50 g vinyl acetat og 550 g vinylklorid istedenfor homopolymerisasjon av vinylklorid. Experiments were carried out under the same conditions as described in example 3, with the exception that the polymerization was a copolymerization of a monomer mixture consisting of 50 g of vinyl acetate and 550 g of vinyl chloride instead of homopolymerization of vinyl chloride.
Sammenlignings!'orsøk ble også utført under samme betingelser som angitt i eksempel j5. Resultatene vises i tabell VI. Comparative research was also carried out under the same conditions as stated in example j5. The results are shown in Table VI.
Eksempel 5. Example 5.
Samme arbeidsoperasjoner med overtrekking og polymerisasjon som angitt i eksempel 1 ble gjentatt med unntagelse for at belegg-materialet bestod av en 0,05$-ig etanolisk dispersjon av et fargestoff (forbindelse A) og en oksosyre eller et salt av en oksosyre (forbindelse B) i like mengder ved hvert forsøk, slik som vist i tabell VII. Resultatene fra bestemmelsen av polymerskallavsetningen vises også i denne tabell. The same work operations with coating and polymerization as indicated in example 1 were repeated with the exception that the coating material consisted of a 0.05% ethanolic dispersion of a dye (compound A) and an oxo acid or a salt of an oxo acid (compound B ) in equal amounts at each trial, as shown in Table VII. The results from the determination of the polymer shell deposition are also shown in this table.
Eksempel 6. Example 6.
Ved dette forsøk ble kopolymerisasjon av vinylklorid og vinylacetat utført under samme betingelser som angitt i eksempel 4, og arbeids-operasjonen med overtrekking var den samme som beskrevet 1 eksempel 5, nemlig med forbindelsene A og B som vist i tabell VIII. Resultatene vises også i denne tabell In this experiment, copolymerization of vinyl chloride and vinyl acetate was carried out under the same conditions as stated in example 4, and the working operation with coating was the same as described in example 5, namely with the compounds A and B as shown in Table VIII. The results are also shown in this table
Eksempel 7».,.-«,■..... Example 7».,.-«,■.....
Samme arbeidsoperasjoner med overtrekking og polymerisasjon som beskrevet' i eksempel 1 ble utført med unntagelse for at det som beleggforbindelse A ble anvendt "Nigrosine Black" i form av en 0, 1%- tg etanolisk eller toluenholdig.løsning, og da i de forskjellige mengder som angitt i tabell IX. mens forbindelse B var natrlumsilikat i form av en .1 vekts-^-ig vandig løsning i en mengde som tilsvarte 0,05 g/m'" tørrstoff. Resultatene vises i tabell IX. The same work operations with coating and polymerization as described' in example 1 were carried out with the exception that "Nigrosine Black" was used as coating compound A in the form of a 0.1% by weight ethanolic or toluene-containing solution, and then in the various quantities as indicated in Table IX. while compound B was sodium silicate in the form of a .1 by weight aqueous solution in an amount corresponding to 0.05 g/m" dry matter. The results are shown in Table IX.
Merknader: Notes:
(1) I forsøkene nr. 92 til 98 ble det anvendt etanoliske løsninger av "Nigrosine Black". (2) I forsøkene nr. 99 til 101 ble det anvendt toluenløsninger av "Nigrosine Black". (3) I forsøk nr. 100 ble "Nigrosine Black"-overtrekkene tørket, og de tørkede overflatene ble forsiktig tørket med en fin klut som var fuktet med etanol, hvoretter man på nytt tørket i 60 minutter med varm luft ved 70°C, og hvoretter man foretok overtrekking rned en vandig løsning av natriumsilikat. (1) In experiments Nos. 92 to 98, ethanolic solutions of "Nigrosine Black" were used. (2) In experiments Nos. 99 to 101, toluene solutions of "Nigrosine Black" were used. (3) In Experiment No. 100, the "Nigrosine Black" coatings were dried, and the dried surfaces were gently dried with a fine cloth moistened with ethanol, and then dried again for 60 minutes with hot air at 70°C, and after which coating was carried out with an aqueous solution of sodium silicate.
E ksempel 8.Example 8.
Suspensjonspolymerisasjon av vinylklorid ble utført under de samme betingelser som ved forsøk nr. 95 i eksempel 7, og da med tilsetning av natriumsilikat til det vandige mediet i mengder på henholdsvis 5 vekts-#, 0,1 vekts-$, 0,0003 vekts-$ eller 0,0001 vekts-% Suspension polymerization of vinyl chloride was carried out under the same conditions as in experiment no. 95 in example 7, and then with the addition of sodium silicate to the aqueous medium in amounts of respectively 5 wt-#, 0.1 wt-$, 0.0003 wt- $ or 0.0001% by weight
beregnet på vinylkloridmonomer, i den hensikt ytterligere åcalculated on vinyl chloride monomer, for the purpose of further to
forbedre forhindringen av polymerskallavsetning. Den nevnte polymerisasjon ble gjentatt inntil man erholdt polymerskallavsetning på reaktorveggenes overflater. Antallet polymerisasjonskjørlnger uten oppkomst av' polymerskallavsetning var henholdsvis 9»7, 5 improve the prevention of polymer shell deposition. The aforementioned polymerization was repeated until polymer shell deposition was obtained on the surfaces of the reactor walls. The number of polymerization runs without occurrence of polymer shell deposition was 9, 7, 5 respectively
eller 1, avhengig av mengden tilsatt natriumsilikat, mens antallet polymerisasjonskjørlnger uten tilsetning av natriumsilikat bare varl. or 1, depending on the amount of added sodium silicate, while the number of polymerization runs without the addition of sodium silicate only varied.
Eksempel 9.Example 9.
Overflatene til innerveggene til en 1000 liter stor rustfri stål-/polymerisasjonsreaktor og overflatene til agitatoren av skovltype ble overtrukket med en 0,5 vekts-$ metanollsk løsning av "Sudan B" og "Nigrosine" i de mengdeforhold sorn angis i tabell X. Den overtrukkede flate var herved 4 rn", og beleggmengden tilsvarte 0,05 g/m P ": tørrstoff. Deretter ble reaktor•en ohargert med -500 kg av en vandig løsning inneholdende 10 g metallsalt, d.v.s. natriumsilikat eller natriumhydrogenkarbonat, som angitt i tabellen. Løsningen ble oppvarmet ved 90°C i 30 minutter under agitering ved 110 o.p.m. Etter avkjøling av løsningen ble 200 g partielt forsåpet polyvinylalkohol, 100 g dimetylvaleronitril, 3,0 kg kalsiumstearat, 1,0 kg risvoks, 200 g polyetylenvoks, 4,0 kg kalsiumkarbonat, The surfaces of the inner walls of a 1000 liter stainless steel/polymerization reactor and the surfaces of the paddle type agitator were coated with a 0.5 wt% methanolic solution of "Sudan B" and "Nigrosine" in the ratios shown in Table X. The coated surface was 4 rn", and the amount of coating corresponded to 0.05 g/m P ": dry matter. Subsequently, the reactor was oharged with -500 kg of an aqueous solution containing 10 g of metal salt, i.e. sodium silicate or sodium bicarbonate, as indicated in the table. The solution was heated at 90°C for 30 minutes with agitation at 110 rpm. After cooling the solution, 200 g of partially saponified polyvinyl alcohol, 100 g of dimethyl valeronitrile, 3.0 kg of calcium stearate, 1.0 kg of rice wax, 200 g of polyethylene wax, 4.0 kg of calcium carbonate,
3,0 kg titandioksyd, 400 g dioktylftalat, 600 g dioktyltinndilaurylmerkaptid og 200 kg vinylkloridmonomer tilsatt. Deretter fulgte suspensjonspolymerisasjon på vanlig måte ved oppvarming ved 55°C 3.0 kg titanium dioxide, 400 g dioctyl phthalate, 600 g dioctyl tin dilauryl mercaptide and 200 kg vinyl chloride monomer added. Suspension polymerization then followed in the usual way by heating at 55°C
i 7 timer. Etter fullføring av polymerisasjonen ble den tømte reaktoren vasket med vann, og mengden polymerskallavsetning på overflatene ble bestemt. Resultatene vises i tabell X for 7 hours. After completion of the polymerization, the emptied reactor was washed with water, and the amount of polymer shell deposition on the surfaces was determined. The results are shown in Table X
Eksempel 10. Example 10.
Innerveggene til en 1000 liter stor polymerisasjonsreaktor ble overtrukket med en beleggløsning eller -dispersjon, som ble fremstil ved å blande en 1 vekts-^-ig løsning eller dispersjon i løsningsmidlet til den polare organiske forbindelsen eller de polare organiske forbindelsene og en vandig løsning eller dispersjon av metallsaltet, slik som vist i tabell XI, hvorved mengdeforholdet mellom de to polare organiske forbindelsene og det. anvendte metallsaltet var 1:1:1 (vektsforhold). Deretter fulgte oppvarming ved 90°C 1 30 minutter. Etter at den overtrukkede veggoverflaten var.vasket med vann, ble reaktoren chargert med 200 kg vinylkloridmonomer, 500 kg avionisert vann, 100 g.diiso-propylperoksydikarbonat, 200 g hydroksypropylmetylcellulose, The inner walls of a 1,000-liter polymerization reactor were coated with a coating solution or dispersion, which was prepared by mixing a 1 wt% solution or dispersion in the solvent of the polar organic compound or compounds and an aqueous solution or dispersion of the metal salt, as shown in Table XI, whereby the quantity ratio between the two polar organic compounds and that. the metal salt used was 1:1:1 (weight ratio). This was followed by heating at 90°C for 1 30 minutes. After the coated wall surface was washed with water, the reactor was charged with 200 kg of vinyl chloride monomer, 500 kg of deionized water, 100 g of diisopropyl peroxydicarbonate, 200 g of hydroxypropyl methylcellulose,
1,0 kg dlbasisk blystearat, 1,0 kg bariumstearat og 600 g stearinsyre, hvoretter det ble foretatt polymerisasjon ved 45°C i 1.0 kg of dibasic lead stearate, 1.0 kg of barium stearate and 600 g of stearic acid, after which polymerization was carried out at 45°C in
8 timer ved en agiteringshastighet på l60 o.p.m. Etter fullført polymerisasjon ble polymerskallavsetningen på veggene bestemt som vist i tabellen.. 8 hours at an agitation speed of 160 rpm. After completion of polymerization, the polymer shell deposition on the walls was determined as shown in the table.
Eksempel 11. Example 11.
Innerveggene og øvrige overflater til polymerisasjonsapparaturen , bestående av en kombinasjon av en første 2-liters rustfri stålpolymerisasjonsreaktor av den vertikale typen og en andre 4^1iters rustfri stålpolymerisasjonsreaktor av den horisontale typen,.ble overtrukket med beleggløsning eller -dispersjon, The inner walls and other surfaces of the polymerization apparatus, consisting of a combination of a first 2 liter stainless steel polymerization reactor of the vertical type and a second 4^1 liter stainless steel polymerization reactor of the horizontal type, were coated with coating solution or dispersion,
som vist i tabell XII, hvoretter det ble foretatt vasking med vann samt tørking. Til den første reaktoren ble det chargert 800 g vinylkloridmonomer, 0,4- g dimetylvaleronitril, 8 g kalsiumstearat, 0,l6 g sinkstearat, 2,4 g soyabønneolje-epoksyd og 4 g pentaeritritol. Deretter fulgte massepolymerisasjon ved as shown in Table XII, after which washing with water and drying were carried out. To the first reactor was charged 800 g of vinyl chloride monomer, 0.4 g of dimethyl valeronitrile, 8 g of calcium stearate, 0.16 g of zinc stearate, 2.4 g of soybean oil epoxide and 4 g of pentaerythritol. Mass polymerization followed
60°C i to timer ved en aglteringshastighet på 900 o.p.m. Deretter ble polymerisasjonsblandingen overført til den andre 60°C for two hours at an agitation speed of 900 rpm. Then the polymerization mixture was transferred to the other
reaktoren, i/hvilken det var chargert 800 g vinylkloridmonomer og 0,4 g dimetylvaleronitril. Deretter foretok man polymerisasjon ved 57°Ci\10 timer ved en aglteringshastighet på 100 o.p.m. the reactor, into which 800 g of vinyl chloride monomer and 0.4 g of dimethylvaleronitrile were charged. Polymerization was then carried out at 57°Ci/10 hours at an agitation speed of 100 rpm.
Mengdene av polymerskallavsetninger fremgår av tabellen. The amounts of polymer shell deposits appear in the table.
Claims (18)
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JP50090633A JPS5214688A (en) | 1975-07-24 | 1975-07-24 | A process for polymerizing vinyl chloride |
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BE (1) | BE844496A (en) |
BR (1) | BR7604840A (en) |
CU (1) | CU34555A (en) |
DE (1) | DE2632469A1 (en) |
DK (1) | DK332276A (en) |
ES (1) | ES449990A1 (en) |
FR (1) | FR2318898A1 (en) |
IT (1) | IT1065055B (en) |
NL (1) | NL7608182A (en) |
NO (1) | NO762540L (en) |
PT (1) | PT65403B (en) |
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JPS548690A (en) * | 1977-06-20 | 1979-01-23 | Goodrich Co B F | Method of preventing polymer from adhering on inner surface of polymerization reactor |
EP0003875B1 (en) * | 1978-02-24 | 1981-06-24 | Imperial Chemical Industries Plc | Coating product for use in a reactor for vinyl halide polymerisation process, the reactor and the process |
JPS606361B2 (en) * | 1979-10-22 | 1985-02-18 | 信越化学工業株式会社 | Polymerization method of vinyl chloride monomer |
DE2946461A1 (en) * | 1979-11-17 | 1981-05-27 | Hoechst Ag, 6000 Frankfurt | METHOD FOR PRODUCING VINYL CHLORIDE POLYMERISATS |
JPS59170102A (en) * | 1983-03-17 | 1984-09-26 | Shin Etsu Chem Co Ltd | Polymerization of vinyl monomer |
CS245419B1 (en) * | 1983-07-11 | 1986-10-16 | Rudolf Lukas | Method of untreated particles' and incrustations' formation reduction during polymerization and copolymerizationof vinyl monomers |
IL91230A (en) * | 1988-08-10 | 1994-01-25 | Shinetsu Chemical Co | Method of preventing polymer scale formation |
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- 1976-07-19 YU YU01776/76A patent/YU177676A/en unknown
- 1976-07-21 ES ES449990A patent/ES449990A1/en not_active Expired
- 1976-07-21 NO NO762540A patent/NO762540L/no unknown
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- 1976-07-23 BE BE169220A patent/BE844496A/en unknown
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FR2318898A1 (en) | 1977-02-18 |
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CU34555A (en) | 1979-09-08 |
JPS5328348B2 (en) | 1978-08-14 |
BE844496A (en) | 1976-11-16 |
PT65403B (en) | 1978-01-27 |
YU177676A (en) | 1982-05-31 |
DE2632469A1 (en) | 1977-02-10 |
DK332276A (en) | 1977-01-25 |
IT1065055B (en) | 1985-02-25 |
JPS5214688A (en) | 1977-02-03 |
BR7604840A (en) | 1977-08-09 |
ES449990A1 (en) | 1977-08-16 |
NL7608182A (en) | 1977-01-26 |
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