JP5956038B1 - 処理フィラーおよびそれらの使用 - Google Patents
処理フィラーおよびそれらの使用 Download PDFInfo
- Publication number
- JP5956038B1 JP5956038B1 JP2015162669A JP2015162669A JP5956038B1 JP 5956038 B1 JP5956038 B1 JP 5956038B1 JP 2015162669 A JP2015162669 A JP 2015162669A JP 2015162669 A JP2015162669 A JP 2015162669A JP 5956038 B1 JP5956038 B1 JP 5956038B1
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- JP
- Japan
- Prior art keywords
- nitrogen
- phosphor
- condensation
- treated
- strong base
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000945 filler Substances 0.000 title claims description 56
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 375
- 238000009833 condensation Methods 0.000 claims abstract description 312
- 230000005494 condensation Effects 0.000 claims abstract description 312
- 239000000203 mixture Substances 0.000 claims abstract description 299
- 239000002245 particle Substances 0.000 claims abstract description 264
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 195
- 239000007787 solid Substances 0.000 claims abstract description 129
- 230000002378 acidificating effect Effects 0.000 claims abstract description 56
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 312
- GQHTUMJGOHRCHB-UHFFFAOYSA-N 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine Chemical group C1CCCCN2CCCN=C21 GQHTUMJGOHRCHB-UHFFFAOYSA-N 0.000 claims description 290
- 239000003054 catalyst Substances 0.000 claims description 102
- OEBXWWBYZJNKRK-UHFFFAOYSA-N 1-methyl-2,3,4,6,7,8-hexahydropyrimido[1,2-a]pyrimidine Chemical compound C1CCN=C2N(C)CCCN21 OEBXWWBYZJNKRK-UHFFFAOYSA-N 0.000 claims description 89
- 238000000034 method Methods 0.000 claims description 60
- 239000003960 organic solvent Substances 0.000 claims description 53
- 230000000052 comparative effect Effects 0.000 claims description 40
- 125000000217 alkyl group Chemical group 0.000 claims description 30
- 238000013005 condensation curing Methods 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- SGUVLZREKBPKCE-UHFFFAOYSA-N 1,5-diazabicyclo[4.3.0]-non-5-ene Chemical compound C1CCN=C2CCCN21 SGUVLZREKBPKCE-UHFFFAOYSA-N 0.000 claims description 22
- LINDOXZENKYESA-UHFFFAOYSA-N TMG Natural products CNC(N)=NC LINDOXZENKYESA-UHFFFAOYSA-N 0.000 claims description 22
- 150000002466 imines Chemical class 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 19
- 125000005375 organosiloxane group Chemical group 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 19
- FVKFHMNJTHKMRX-UHFFFAOYSA-N 3,4,6,7,8,9-hexahydro-2H-pyrimido[1,2-a]pyrimidine Chemical compound C1CCN2CCCNC2=N1 FVKFHMNJTHKMRX-UHFFFAOYSA-N 0.000 claims description 18
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 18
- 125000003118 aryl group Chemical group 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 16
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 14
- 150000004767 nitrides Chemical class 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 14
- 229920001400 block copolymer Polymers 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 10
- 150000004645 aluminates Chemical class 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 10
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- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
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- 239000000126 substance Substances 0.000 claims description 2
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- -1 polypropylene Polymers 0.000 description 65
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- 239000000047 product Substances 0.000 description 47
- 125000004433 nitrogen atom Chemical group N* 0.000 description 45
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 37
- 238000001723 curing Methods 0.000 description 33
- 150000001412 amines Chemical class 0.000 description 29
- LAWOZCWGWDVVSG-UHFFFAOYSA-N dioctylamine Chemical compound CCCCCCCCNCCCCCCCC LAWOZCWGWDVVSG-UHFFFAOYSA-N 0.000 description 29
- 239000000463 material Substances 0.000 description 27
- 239000011701 zinc Substances 0.000 description 26
- 125000000753 cycloalkyl group Chemical group 0.000 description 23
- 125000002947 alkylene group Chemical group 0.000 description 22
- 125000003710 aryl alkyl group Chemical group 0.000 description 21
- 150000001875 compounds Chemical class 0.000 description 20
- 239000010936 titanium Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 239000002253 acid Substances 0.000 description 19
- 229910052950 sphalerite Inorganic materials 0.000 description 19
- 229910052984 zinc sulfide Inorganic materials 0.000 description 19
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- 229910052725 zinc Inorganic materials 0.000 description 17
- 229910052782 aluminium Inorganic materials 0.000 description 16
- 125000004432 carbon atom Chemical group C* 0.000 description 16
- 239000011521 glass Substances 0.000 description 16
- 229920005989 resin Polymers 0.000 description 15
- 239000011347 resin Substances 0.000 description 15
- 229910052712 strontium Inorganic materials 0.000 description 15
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 14
- 239000011575 calcium Substances 0.000 description 13
- 229930195733 hydrocarbon Natural products 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 229910010413 TiO 2 Inorganic materials 0.000 description 12
- 238000011068 loading method Methods 0.000 description 12
- 229910052684 Cerium Inorganic materials 0.000 description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 11
- 239000011230 binding agent Substances 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 11
- 238000001914 filtration Methods 0.000 description 11
- 230000008901 benefit Effects 0.000 description 10
- 239000011777 magnesium Substances 0.000 description 10
- 229910052748 manganese Inorganic materials 0.000 description 10
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- 229910052788 barium Inorganic materials 0.000 description 9
- 229910052793 cadmium Inorganic materials 0.000 description 9
- 150000002430 hydrocarbons Chemical class 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 9
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 9
- 125000000923 (C1-C30) alkyl group Chemical group 0.000 description 8
- 229910052787 antimony Inorganic materials 0.000 description 8
- 229910052791 calcium Inorganic materials 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 8
- 229920002050 silicone resin Polymers 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 229910052771 Terbium Inorganic materials 0.000 description 7
- 238000009835 boiling Methods 0.000 description 7
- 230000006870 function Effects 0.000 description 7
- 239000011133 lead Substances 0.000 description 7
- 239000011541 reaction mixture Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 229910052726 zirconium Inorganic materials 0.000 description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 150000001409 amidines Chemical class 0.000 description 6
- 150000007514 bases Chemical class 0.000 description 6
- UURSXESKOOOTOV-UHFFFAOYSA-N dec-5-ene Chemical compound CCCCC=CCCCC UURSXESKOOOTOV-UHFFFAOYSA-N 0.000 description 6
- 238000003795 desorption Methods 0.000 description 6
- 239000003085 diluting agent Substances 0.000 description 6
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 6
- 150000002357 guanidines Chemical class 0.000 description 6
- 238000011065 in-situ storage Methods 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 238000003878 thermal aging Methods 0.000 description 6
- 229910052718 tin Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 125000001033 ether group Chemical group 0.000 description 5
- 229910052733 gallium Inorganic materials 0.000 description 5
- 150000002576 ketones Chemical class 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 150000002825 nitriles Chemical class 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Chemical group 0.000 description 5
- 229910052698 phosphorus Chemical group 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000012756 surface treatment agent Substances 0.000 description 5
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 5
- VSTXCZGEEVFJES-UHFFFAOYSA-N 1-cycloundecyl-1,5-diazacycloundec-5-ene Chemical compound C1CCCCCC(CCCC1)N1CCCCCC=NCCC1 VSTXCZGEEVFJES-UHFFFAOYSA-N 0.000 description 4
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Natural products CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 4
- 229910004283 SiO 4 Inorganic materials 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 150000004703 alkoxides Chemical class 0.000 description 4
- 125000003545 alkoxy group Chemical group 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 4
- 150000001733 carboxylic acid esters Chemical class 0.000 description 4
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- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 4
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
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- 235000000177 Indigofera tinctoria Nutrition 0.000 description 3
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 3
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- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 description 3
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- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 3
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- 229910020068 MgAl Inorganic materials 0.000 description 2
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- GSCOPSVHEGTJRH-UHFFFAOYSA-J [Ti+4].CCCC(=O)CC([O-])=O.CCCC(=O)CC([O-])=O.CCCC(=O)CC([O-])=O.CCCC(=O)CC([O-])=O Chemical compound [Ti+4].CCCC(=O)CC([O-])=O.CCCC(=O)CC([O-])=O.CCCC(=O)CC([O-])=O.CCCC(=O)CC([O-])=O GSCOPSVHEGTJRH-UHFFFAOYSA-J 0.000 description 2
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- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 2
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- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
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- HSVPRYWNEODRGU-UHFFFAOYSA-J butanoate;zirconium(4+) Chemical compound [Zr+4].CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O HSVPRYWNEODRGU-UHFFFAOYSA-J 0.000 description 2
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- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- CWYZDPHNAGSFQB-UHFFFAOYSA-N n-propylbutan-1-amine Chemical compound CCCCNCCC CWYZDPHNAGSFQB-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 125000004894 pentylamino group Chemical group C(CCCC)N* 0.000 description 1
- 125000001792 phenanthrenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C=CC12)* 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 125000003386 piperidinyl group Chemical group 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920003255 poly(phenylsilsesquioxane) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006375 polyphtalamide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical compound CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 description 1
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 1
- XDAGXZXKTKRFMT-UHFFFAOYSA-N propan-2-imine Chemical group CC(C)=N XDAGXZXKTKRFMT-UHFFFAOYSA-N 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 125000001725 pyrenyl group Chemical group 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 125000000719 pyrrolidinyl group Chemical group 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- KCIKCCHXZMLVDE-UHFFFAOYSA-N silanediol Chemical group O[SiH2]O KCIKCCHXZMLVDE-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940063675 spermine Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000003107 substituted aryl group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000007525 superbases Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 125000001935 tetracenyl group Chemical group C1(=CC=CC2=CC3=CC4=CC=CC=C4C=C3C=C12)* 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- 125000003960 triphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C3=CC=CC=C3C12)* 0.000 description 1
- MBYLVOKEDDQJDY-UHFFFAOYSA-N tris(2-aminoethyl)amine Chemical compound NCCN(CCN)CCN MBYLVOKEDDQJDY-UHFFFAOYSA-N 0.000 description 1
- DAOVYDBYKGXFOB-UHFFFAOYSA-N tris(2-methylpropoxy)alumane Chemical compound [Al+3].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] DAOVYDBYKGXFOB-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
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Abstract
Description
縮合硬化型ポリオルガノシロキサンと、
ある量の窒素含有超強塩基が表面に配置された粒状固体を含む処理粒子と
を含む、縮合硬化型シリコーン組成物であって、
前記した粒状固体上に配置された窒素含有超強塩基の量が、前記した粒状固体上の複数の酸性部位の実質的な数を中和するのに十分な量であり、および前記した粒状固体上の酸性部位の実質的な数が、配置された窒素含有塩基で中和される、縮合硬化型シリコーン組成物により、達成することができる。
(実施例1)(PhMeSiO2/2)0.52(PhSiO3/2)0.42(45重量%フェニル−T)の調製
(実施例2)
(実施例3)
(実施例4)
(実施例5)
比較例(CE)A(1):塩基ではなくトルエンでの処理
(実施例6)レオロジー測定
比較例(CE)B(1):
実施例7〜9ならびに比較例B(2)からB(4)およびC(2)からC(4):
実施例10〜12ならびに比較例B(5)およびC(5)からC(7):
(実施例16)(予測例、prophetic)
(実施例17)(prophetic)
(実施例18)(prophetic)
(実施例19)(prophetic)
(実施例20)(prophetic)
(実施例21)(prophetic)
(実施例22)(prophetic)
(実施例23)(prophetic)
実施例24aおよび24bならびに比較例B(8)およびC(9):DBUのイソプロパノール溶液で蛍光体を処理、蛍光体なし、または未処理蛍光体
Claims (28)
- 縮合硬化型ポリオルガノシロキサンと、
ある量の窒素含有超強塩基が表面に配置された粒状固体を含む処理粒子と
を含む、縮合硬化型シリコーン組成物であって、
前記粒状固体上に配置された窒素含有超強塩基の量が、前記粒状固体上の少なくとも90%の酸性部位を中和するのに十分な量であり、および前記粒状固体上の酸性部位の少なくとも90%が、配置された窒素含有超強塩基で中和される、縮合硬化型シリコーン組成物。 - 前記粒状固体上に配置された窒素含有超強塩基の量が、前記縮合硬化型シリコーン組成物が硬化して1であるタンデルタ値に達するために必要な時間が150℃で30秒から1時間であるために十分な量である、請求項1に記載の縮合硬化型シリコーン組成物。
- 前記粒状固体が、粒状蛍光体である、請求項1または2に記載の縮合硬化型シリコーン組成物。
- 前記粒状蛍光体が、セリウムドープ蛍光体、アルミン酸塩蛍光体、ケイ酸塩蛍光体、ガーネット蛍光体、および窒化物蛍光体のうちの少なくとも1つを含む、請求項3に記載の縮合硬化型シリコーン組成物。
- 前記窒素含有超強塩基が、一般式:
- 前記窒素含有超強塩基が、
1,8−ジアザビシクロ[5.4.0]ウンデカ−7−エン(DBU);
1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(TBD);
1,5−ジアザビシクロ[4.3.0]−5−ノネン(DBN);および
7−メチル−1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(MTBD)のうちの少なくとも1つである、請求項1から5のいずれか一項に記載の縮合硬化型シリコーン組成物。 - 縮合触媒をさらに含む、請求項1から6のいずれか一項に記載の縮合硬化型シリコーン組成物。
- 前記縮合触媒が、独立して窒素含有超強塩基である、請求項7に記載の縮合硬化型シリコーン組成物。
- 前記縮合硬化型ポリオルガノシロキサンが、
0から10モルパーセントの式[R3SiO1/2]のM構成単位と、
40から90モルパーセントの式[R2SiO2/2]のD構成単位と、
10から60モルパーセントの式[RSiO3/2]のT構成単位と、
0.5から35モルパーセントのケイ素結合ヒドロキシ(SiOH)と
を含み;
M、DおよびT構成要素のモルパーセントの合計が、100モルパーセントであり;
各Rが、独立して、C1からC30ヒドロカルビルであり;
前記D構成単位[R2SiO2/2]が、1線状ブロックにつき平均50から300のD構成単位[R2SiO2/2]を有する線状ブロックに配列されており;
前記T構成単位[RSiO3/2]が、少なくとも500g/モルのブロック重量を有する非線状ブロックに配列されており;
前記M構成単位[R3SiO1/2]が、T単位に連結されており;
前記非線状ブロックの少なくとも30%が、互いに架橋しており;
各線状ブロックが、−Si−O−Si−結合によって少なくとも1つの非線状ブロックに結合されている、オルガノシロキサンブロックコポリマーを含み、
前記オルガノシロキサンブロックコポリマーが、少なくとも20,000g/モルの重量平均分子量を有する、
請求項1から8のいずれか一項に記載の縮合硬化型シリコーン組成物。 - 請求項1から9のいずれか一項に記載の縮合硬化型シリコーン組成物の縮合硬化の硬化生成物。
- 硬化ポリオルガノシロキサンを調製するための方法であって、
請求項1から10のいずれか一項に記載の縮合硬化型シリコーン組成物を、縮合触媒の存在下で縮合硬化させて、硬化ポリオルガノシロキサンを得る工程を含み、
前記処理粒子上に配置された窒素含有超強塩基の量が、未処理粒子上の少なくとも90%の酸性部位を中和させるのに十分な量である、方法。 - 複数の酸性部位を有する粒状固体を処理するための方法であって、
前記粒状固体を窒素含有超強塩基と接触させて、ある量の窒素含有超強塩基が表面に配置された処理粒子を得る工程を含み、前記粒状固体上に配置された前記窒素含有超強塩基の量が、前記粒状固体上の少なくとも90%の酸性部位を中和するのに十分な量であり、前記粒状固体が窒化物または蛍光体である、方法。 - 複数の酸性部位を有する粒状固体を処理するための方法であって、
前記粒状固体を窒素含有超強塩基と接触させて、ある量の窒素含有超強塩基が表面に配置された処理粒子を得る工程を含み、前記粒状固体上に配置された前記窒素含有超強塩基の量が、前記粒状固体上の少なくとも90%の酸性部位を中和するのに十分な量であり、
ある量の窒素含有超強塩基が表面に配置された前記処理粒子を単離して、単離された処理粒子を得る工程;
ある量の窒素含有超強塩基が表面に配置された前記単離された処理粒子を、配置された窒素含有超強塩基の、すべてでないが、一部分をそれらから除去するように加工して、加工された処理粒子を得る工程
をさらに含み;
前記加工が、ある量の窒素含有超強塩基が表面に配置された前記単離された処理粒子を、配置された窒素含有超強塩基の、すべてでないが、一部分をそれらから除去するために十分な温度で十分な時間加熱して、加工された処理粒子を得ることを含み、その結果、ある量の窒素含有超強塩基が表面に配置された前記加工された処理粒子を含む縮合硬化型シリコーン組成物が硬化して1であるタンデルタ値に達するために必要な時間が、150℃で30秒から1時間になる、方法。 - ある量の窒素含有超強塩基が表面に配置された粒状フィラーを含み、前記粒状フィラー上に配置された窒素含有超強塩基の量が、前記粒状フィラー上の少なくとも90%の酸性部位を中和するのに十分な量であり、および前記粒状フィラー上の酸性部位の少なくとも90%が、配置された窒素含有超強塩基で中和され、前記粒状フィラーが窒化物である、処理フィラー粒子。
- 前記窒素含有超強塩基が、一般式:
- ある量の窒素含有超強塩基が表面に配置された粒状蛍光体を含む処理蛍光体粒子であって、前記粒状蛍光体上に配置された窒素含有超強塩基の量が、前記粒状蛍光体上の少なくとも90%の酸性部位を中和するのに十分な量であり、および前記粒状蛍光体上の酸性部位の少なくとも90%が、配置された窒素含有超強塩基で中和され;前記粒状蛍光体上に配置された窒素含有超強塩基の量が、前記処理蛍光体粒子を、縮合硬化型ポリオルガノシロキサンと前記処理蛍光体粒子とを含む縮合硬化型シリコーン組成物で使用したときに、前記縮合硬化型シリコーン組成物が硬化して150℃で1であるタンデルタ値に達するために必要な時間が、前記縮合硬化型ポリオルガノシロキサンと未処理蛍光体粒子(すなわち、前記窒素含有超強塩基を含有しない蛍光体粒子)とを含む比較対照縮合硬化型シリコーン組成物に必要な時間より少なくとも20秒短くなるために十分な量であることを特徴とする、処理蛍光体粒子。
- 前記窒素含有超強塩基が、一般式:
- 前記窒素含有超強塩基が、
1,8−ジアザビシクロ[5.4.0]ウンデカ−7−エン(DBU);
1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(TBD);
1,5−ジアザビシクロ[4.3.0]−5−ノネン(DBN);および
7−メチル−1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(MTBD)
のうちの少なくとも1つである、請求項16または17に記載の処理蛍光体粒子。 - ある量の窒素含有超強塩基が表面に配置された粒状蛍光体を含む処理蛍光体粒子であって、前記粒状蛍光体上に配置された窒素含有超強塩基の量が、前記粒状蛍光体上の少なくとも90%の酸性部位を中和するのに十分な量であり、および前記粒状蛍光体上の酸性部位の少なくとも90%が、配置された窒素含有超強塩基で中和され;ならびに前記窒素含有超強塩基が、1,8−ジアザビシクロ[5.4.0]ウンデカ−7−エン(DBU);1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(TBD);1,1,3,3−テトラメチルグアニジン(TMG);1,5−ジアザビシクロ[4.3.0]−5−ノネン(DBN);および7−メチル−1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(MTBD)のうちの少なくとも1つである、処理蛍光体粒子。
- 単離された粉末の形態である、請求項19に記載の処理蛍光体粒子。
- 蛍光体粒子の表面に超強塩基のモノリシックコーティングまたはフィルムを含有しない、請求項19または20に記載の処理蛍光体粒子。
- 窒素含有超強塩基を未処理蛍光体粒子に送達するための送達組成物であって、窒素含有超強塩基と有機溶媒とを含み、前記窒素含有超強塩基が、一般式:
- 縮合硬化型ポリオルガノシロキサンと処理蛍光体粒子とを含む縮合硬化型シリコーン組成物を製造するための方法において処理蛍光体粒子を縮合硬化型ポリオルガノシロキサンに送達するための送達組成物であって、前記縮合硬化型シリコーン組成物が硬化して150℃で1であるタンデルタ値に達するために必要な時間が、前記縮合硬化型ポリオルガノシロキサンと未処理蛍光体粒子(すなわち、窒素含有超強塩基を含有しない蛍光体粒子)とを含む比較対照縮合硬化型シリコーン組成物に必要な時間より少なくとも20秒短く;請求項16から19および21のいずれか一項に記載の処理蛍光体粒子と有機溶媒とを含むものである送達組成物。
- ポリオルガノシロキサンと処理蛍光体粒子とを含む縮合硬化型シリコーン組成物の硬化の硬化生成物を含む縮合硬化シリコーン組成物を製造するための方法において処理蛍光体粒子を縮合硬化ポリオルガノシロキサンに送達するための送達組成物であって、前記縮合硬化型シリコーン組成物が硬化して150℃で1であるタンデルタ値に達するために必要な時間が、前記縮合硬化型ポリオルガノシロキサンと未処理蛍光体粒子(すなわち、窒素含有超強塩基を含有しない蛍光体粒子)とを含む比較対照縮合硬化型シリコーン組成物に必要な時間より少なくとも20秒短く;請求項16から19および21のいずれか一項に記載の処理蛍光体粒子と有機溶媒とを含むものである送達組成物。
- 請求項16から19および21のいずれか一項に記載の処理蛍光体粒子を製造するための方法において窒素含有超強塩基を未処理蛍光体粒子に送達するための送達組成物の使用であって、前記送達組成物が、窒素含有超強塩基および有機溶媒を含み、前記窒素含有超強塩基が、1,8−ジアザビシクロ[5.4.0]ウンデカ−7−エン(DBU);1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(TBD);1,5−ジアザビシクロ[4.3.0]−5−ノネン(DBN);および7−メチル−1,5,7−トリアザビシクロ[4.4.0]デカ−5−エン(MTBD)のうちの少なくとも1つである使用。
- 縮合硬化型ポリオルガノシロキサンと処理蛍光体粒子とを含む縮合硬化型シリコーン組成物を製造するための方法において処理蛍光体粒子を縮合硬化型ポリオルガノシロキサンに送達するための送達組成物の使用であって、前記縮合硬化型シリコーン組成物が硬化して150℃で1であるタンデルタ値に達するために必要な時間が、前記縮合硬化型ポリオルガノシロキサンと未処理蛍光体粒子(すなわち、窒素含有超強塩基を含有しない蛍光体粒子)とを含む比較対照縮合硬化型シリコーン組成物に必要な時間より少なくとも20秒短く;前記送達組成物が、請求項16から19および21のいずれか一項に記載の処理蛍光体粒子と有機溶媒とを含むものである使用。
- ポリオルガノシロキサンと処理蛍光体粒子とを含む縮合硬化型シリコーン組成物の硬化の硬化生成物を含む縮合硬化シリコーン組成物を製造するための方法において処理蛍光体粒子を縮合硬化ポリオルガノシロキサンに送達するための送達組成物の使用であって、前記縮合硬化型シリコーン組成物が硬化して150℃で1であるタンデルタ値に達するために必要な時間が、前記縮合硬化型ポリオルガノシロキサンと未処理蛍光体粒子(すなわち、窒素含有超強塩基を含有しない蛍光体粒子)とを含む比較対照縮合硬化型シリコーン組成物に必要な時間より少なくとも20秒短く;前記送達組成物が、請求項16から19および21のいずれか一項に記載の処理蛍光体粒子と有機溶媒とを含むものである使用。
- 硬化型ポリオルガノシロキサンと未処理粒子とを含む組成物を処理するための方法であって、
縮合硬化型ポリオルガノシロキサンと未処理粒子とを含む組成物を、溶媒と、前記未処理粒子上の少なくとも90%の酸性部位を中和するのに十分な量の窒素含有超強塩基とを含む溶液で処理する工程を含み;
前記窒素含有超強塩基を含む溶液が、前記縮合硬化型ポリオルガノシロキサンを実質的に溶解しないものである方法。
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