JP2013022757A - Method for manufacturing woody product - Google Patents
Method for manufacturing woody product Download PDFInfo
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- JP2013022757A JP2013022757A JP2011156802A JP2011156802A JP2013022757A JP 2013022757 A JP2013022757 A JP 2013022757A JP 2011156802 A JP2011156802 A JP 2011156802A JP 2011156802 A JP2011156802 A JP 2011156802A JP 2013022757 A JP2013022757 A JP 2013022757A
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- Prior art keywords
- adhesive
- fine carbon
- carbon fiber
- manufacturing
- wood
- Prior art date
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- Granted
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title abstract description 29
- 239000000853 adhesive Substances 0.000 claims abstract description 147
- 230000001070 adhesive effect Effects 0.000 claims abstract description 136
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 98
- 239000004917 carbon fiber Substances 0.000 claims abstract description 98
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000463 material Substances 0.000 claims abstract description 50
- 239000002131 composite material Substances 0.000 claims abstract description 11
- 239000002023 wood Substances 0.000 claims description 53
- 239000011120 plywood Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000003825 pressing Methods 0.000 claims description 11
- 239000011094 fiberboard Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005304 joining Methods 0.000 claims description 2
- 238000007731 hot pressing Methods 0.000 abstract description 21
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 26
- 229920005989 resin Polymers 0.000 description 25
- 239000011347 resin Substances 0.000 description 25
- 239000007787 solid Substances 0.000 description 22
- 239000006185 dispersion Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 17
- 239000003054 catalyst Substances 0.000 description 15
- 239000000543 intermediate Substances 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 12
- 239000000835 fiber Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 239000000178 monomer Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002270 dispersing agent Substances 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 238000004904 shortening Methods 0.000 description 8
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000009833 condensation Methods 0.000 description 7
- 230000005494 condensation Effects 0.000 description 7
- 238000005979 thermal decomposition reaction Methods 0.000 description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 6
- 229930195733 hydrocarbon Natural products 0.000 description 6
- 150000002430 hydrocarbons Chemical class 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 6
- 229920002554 vinyl polymer Polymers 0.000 description 6
- 239000004215 Carbon black (E152) Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 239000002648 laminated material Substances 0.000 description 5
- 150000002894 organic compounds Chemical class 0.000 description 5
- 239000002356 single layer Substances 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229920000877 Melamine resin Polymers 0.000 description 4
- 238000001241 arc-discharge method Methods 0.000 description 4
- 150000001722 carbon compounds Chemical class 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 235000013312 flour Nutrition 0.000 description 4
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000004848 polyfunctional curative Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000004816 latex Substances 0.000 description 3
- 229920000126 latex Polymers 0.000 description 3
- 239000000123 paper Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000001947 vapour-phase growth Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000009408 flooring Methods 0.000 description 2
- 238000000981 high-pressure carbon monoxide method Methods 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000012948 isocyanate Substances 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 239000011269 tar Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010549 co-Evaporation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000020335 dealkylation Effects 0.000 description 1
- 238000006900 dealkylation reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 description 1
- 238000010130 dispersion processing Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- HANVTCGOAROXMV-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine;urea Chemical compound O=C.NC(N)=O.NC1=NC(N)=NC(N)=N1 HANVTCGOAROXMV-UHFFFAOYSA-N 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- -1 veneer laminate Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002025 wood fiber Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Dry Formation Of Fiberboard And The Like (AREA)
- Laminated Bodies (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Veneer Processing And Manufacture Of Plywood (AREA)
Abstract
Description
本発明は、木質製品の製造方法に関する。 The present invention relates to a method for manufacturing a wooden product.
合板、パーティクルボード（ＰＢ）、ＭＤＦ等の木質材の製造や、これらを基材とし、該基材に単板を接合して化粧板等を製造する場合には、蒸気プレス等のホットプレスを利用した熱圧締が広く行われている。
熱圧締による木質材等の製造においては、その熱圧締時間が、生産性を大きく左右する因子である。そのため、熱圧締時間の短縮化を図る種々の技術が提案されている。
例えば、特許文献１には、パーティクルボードの製造に用いる接着剤に硬化促進剤としてＭＤＩ（ジ・フェニルメタン、ジ・イソシアネート）を添加する方法が提案され、特許文献２には、熱圧締の前に、被着材を高周波により予め加熱しておく方法が提案されている。
また、特許文献３には、接着剤の塗布後、加圧下に５〜２０００Ｈｚの振動を付与する方法が提案されている。
When manufacturing wood materials such as plywood, particle board (PB), MDF, etc., and using these as a base material and joining a single plate to the base material to manufacture a decorative board, etc., a hot press such as a steam press is used. Hot pressing is widely used.
In the production of wooden materials by hot pressing, the hot pressing time is a factor that greatly affects productivity. Therefore, various techniques for shortening the hot pressing time have been proposed.
For example, Patent Document 1 proposes a method of adding MDI (di-phenylmethane, di-isocyanate) as a curing accelerator to an adhesive used in the manufacture of particle board, and Patent Document 2 discloses a method of hot pressing. Previously, a method has been proposed in which the adherend is preheated by high frequency.
Patent Document 3 proposes a method of applying a vibration of 5 to 2000 Hz under pressure after application of an adhesive.
しかし、特許文献１のように、硬化促進剤として副材料を配合する場合には、粘度上昇や硬化が促進され、接着剤として使用可能な時間が短縮されるため、頻繁に、接着剤の調製が必要となったり、大掛かりな装置が必要になる等の不都合がある。
また、特許文献２や３のように、外部装置を用いる場合には、製造ラインに大掛かりな設備投資が必要となるといった問題があった。
However, as in Patent Document 1, when a secondary material is blended as a curing accelerator, viscosity increase and curing are promoted, and the time available for use as an adhesive is shortened. There are inconveniences such as requiring a large-scale device.
Moreover, when using an external device like patent document 2 and 3, there existed a problem that a large-scale capital investment was needed for a manufacturing line.
ところで、接着剤にカーボンナノチューブを配合する技術が知られている。例えば、特許文献４には、金属粒子の代わりにカーボンナノチューブを接着剤に配合し、導電性接着剤の剛性を向上させる技術が記載されており、特許文献５には、ラバーを貼付して卓球のラケットとされる卓球ラケット用ブレードの構成部材どうしを接着する接着剤にカーボンナノチューブを用いることが記載されている。
しかし、これらはカーボンナノチューブの電気伝導性や反発弾性向上能に着目して配合したものである。
By the way, the technique of mix | blending a carbon nanotube with an adhesive agent is known. For example, Patent Document 4 describes a technique for improving the rigidity of a conductive adhesive by blending carbon nanotubes into an adhesive instead of metal particles, and Patent Document 5 describes a table tennis by attaching rubber. It is described that carbon nanotubes are used as an adhesive for bonding constituent members of table tennis racket blades, which are used as rackets.
However, these compounds are compounded by paying attention to the electric conductivity and the resilience improving ability of carbon nanotubes.
従って、本発明の目的は、熱圧締時間を短縮して木質製品を効率よく製造することのできる木質製品の製造方法及びこれを可能とする接着剤を提供することにある。 Accordingly, an object of the present invention is to provide a method for producing a wooden product capable of efficiently producing a wooden product by shortening the hot pressing time, and an adhesive that enables this.
本発明は、接着剤を含む製造中間体を熱圧締して木質製品を得る木質製品の製造方法において、前記接着剤として、微細炭素繊維を配合した接着剤を用いることを特徴とする木質製品の製造方法を提供することにより、上記目的を達成したものである。 The present invention relates to a method for producing a wood product in which a wood product is obtained by heat-pressing a production intermediate containing an adhesive, wherein the wood product is characterized in that an adhesive containing fine carbon fibers is used as the adhesive. The above object is achieved by providing the manufacturing method.
また、本発明は、水性接着剤に微細炭素繊維を配合してなる木質製品製造用の水性接着剤を提供するものである。 Moreover, this invention provides the water-based adhesive for manufacture of the wooden product formed by mix | blending fine carbon fiber with a water-based adhesive.
本発明の木質製品の製造方法及び接着剤によれば、熱圧締時間を短縮して木質製品を効率よく製造することができる。 According to the wood product manufacturing method and the adhesive of the present invention, the wood product can be efficiently manufactured by shortening the hot pressing time.
以下、本発明をその好ましい実施形態に基づいて詳細に説明する。
本発明で製造する木質製品としては、（１）単板間が接着剤を介して接着された合板若しくは単板積層材である木質材、又は木材の小片や繊維等のエレメントどうしが接着剤を介して一体化した木質ボード等の木質材、（２）木質材からなる基材の片面又は両面に、接着剤を介して表面化粧材を接合した木質複合材等が挙げられる。
Hereinafter, the present invention will be described in detail based on preferred embodiments thereof.
The wood products manufactured by the present invention include: (1) a wood material that is a plywood or a single plate laminated material in which the single plates are bonded via an adhesive, or elements such as small pieces of wood or fibers that have adhesives. Wood materials such as a wood board integrated through a wood board, and (2) a wood composite material in which a surface decorative material is joined to one or both sides of a base material made of wood material via an adhesive.
（１）木質材
（１）の木質材としては、合板、単板積層材（ＬＶＬ）、パーティクルボード（ＰＢ）、ファイバーボード（ＭＤＦ等）、ＯＳＢ（Ｏｒｉｅｎｔｅｄ Ｓｔｒａｎｄ Ｂｏａｒｄ）、集成材、ブロックボード等が挙げられる。
(1) Wood material (1) Wood materials such as plywood, single plate laminate (LVL), particle board (PB), fiber board (MDF, etc.), OSB (Oriented Strand Board), laminated wood, block board, etc. Is mentioned.
合板は、木材を薄くスライスして得た単板を、繊維方向が互い違いとなるように複数枚重ねて熱圧接着した木質ボードであり、層間が接着剤を介して接合されている。合板は、厚み方向の一部に、繊維の配向方向を揃えた２層又は３層の単板が存在するようなものであってもよい。
単板積層材（ＬＶＬ）は、木材を薄くスライスして得た単板を、繊維方向を同方向に向けて複数枚重ね熱圧接着した木質ボードであり、層間が接着剤を介して接合されている。
木質材として、合板及び単板積層材を製造する場合、総ての層間又は一部の層間の接着に用いる接着剤として、微細炭素繊維配合の接着剤を用いる。
The plywood is a wood board in which a plurality of single plates obtained by thinly slicing wood are laminated by heat and pressure so that the fiber directions are staggered, and the layers are bonded via an adhesive. The plywood may be such that there is a two-layer or three-layer veneer in which the fiber orientation direction is aligned in part of the thickness direction.
Veneer laminate (LVL) is a wood board in which a single board obtained by thinly slicing wood is laminated by hot-pressure bonding with multiple fibers facing in the same direction, and the layers are joined via an adhesive. ing.
When manufacturing a plywood and a single board laminated material as a wood material, the adhesive agent of a fine carbon fiber is used as an adhesive agent used for adhesion | attachment of all the interlayers or one part interlayer.
パーティクルボードは、木材の切削や破砕等により得た小片（エレメント）を接着剤と共に混合してマット状としたのもの（製造中間体）を熱圧締して得られる木質ボードであり、エレメントどうしを結合するバインダーとして接着剤が用いられる。
ファイバーボードは、木材の蒸射・解繊等により得た木材繊維（エレメント）を接着剤と混合してマット状としたもの（製造中間体）を熱圧締して得られる木質ボードであり、エレメントどうしを結合するバインダーとして接着剤が用いられる。ファイバーボードとしては、ＭＤＦ（中比重繊維板）、やハードボード（ＨＢ）、インシュレーションボードが挙げられるが、本発明は、乾式でフォーミングするパーティクルボードやＭＤＦの製造に適している。製造中間体は乾式フォーミングにより得られたものであることが好ましい。
ＯＳＢ（Ｏｒｉｅｎｔｅｄ Ｓｔｒａｎｄ Ｂｏａｒｄ）は、薄い削片状にした原料のエレメントを配向させて積層、接着したものである。エレメントは、パーティクルボードに用いられるものより面積が大きく薄い形状をしており木材の異方性をより多く残している。
木質製品として、パーティクルボード、ファイバーボード及びＯＳＢを製造する場合、エレメントどうしを結合させる接着剤として、微細炭素繊維配合の接着剤を用いる。
Particle boards are wood boards that are obtained by heat-pressing small pieces (elements) obtained by cutting or crushing wood together with adhesives into mats (production intermediates). An adhesive is used as a binder for binding the.
The fiber board is a wood board that is obtained by heat-pressing a mat-like product (manufacturing intermediate) obtained by mixing wood fibers (elements) obtained by evaporating and defibrating wood with an adhesive. An adhesive is used as a binder for bonding the elements together. Examples of the fiber board include MDF (medium specific gravity fiber board), hard board (HB), and insulation board, but the present invention is suitable for manufacturing dry-formed particle boards and MDFs. The production intermediate is preferably obtained by dry forming.
OSB (Oriented Strand Board) is an element obtained by orienting, laminating, and adhering thin pieces of raw material elements. The element has a larger area and thinner shape than that used for particleboard, leaving more wood anisotropy.
When producing particle boards, fiber boards and OSBs as wood products, an adhesive containing fine carbon fibers is used as an adhesive for bonding elements together.
集成材は、ひき板又は小角材などを、繊維方向を互いに平行にして長さ、幅、厚さ方向に集成接着したものである。ひき板又は小角材を相互間に接着剤を介在させて所定形状に並べたものが製造中間体である。
ブロックボードは、ブロック状の小片を、板状に集成接着したものである。
木質材として、集成材及びブロックボードを製造する場合、ひき板、小角材又は
ブロック状の小片どうしを結合させる接着剤として、微細炭素繊維配合の接着剤を用いる。
The laminated material is obtained by gluing and bonding saw plates or small-angled materials in the length, width, and thickness directions with the fiber directions parallel to each other. A production intermediate is obtained by arranging a sheet or a small square material in a predetermined shape with an adhesive interposed therebetween.
The block board is obtained by collecting and bonding block-shaped pieces in a plate shape.
When manufacturing a laminated material and a block board as a wood material, the adhesive agent of a fine carbon fiber is used as an adhesive agent which joins a board, a small square material, or block-shaped small pieces.
（２）木質複合材
（２）の木質複合材としては、合板、単板積層材、パーティクルボード、ファイバーボード、ＯＳＢ、集成材、ブロックボード等の木質材を基材とし、その基材の片面又は両面に、接着剤を介して、突板等の表面化粧材を接合してなるものが挙げられる。基材の片面又は両面上に、接着剤を介在して表面化粧材を重ねたものが、接着剤を含む製造中間体である。
基材として用いる木質材は、微細炭素繊維を配合していない接着剤を用いて製造された従来品を用いてもよいし、微細炭素繊維配合の接着剤を用いて製造した木質材であってもよい。基材に積層接着させる表面化粧材としては、突板、紙、オレフィン樹脂製シートや塩ビ製シート等の合成樹脂製シート、メラミン含浸紙等が挙げられる。突板は、天然木から得た単板の他、植林木から得た単板であってもよい。
基材の形状としては、フィルム、シート、板、立体成形物など様々な形状が挙げられる。
(2) Wood composite material (2) Wood composite material is made of wood material such as plywood, veneer laminate, particle board, fiber board, OSB, laminated wood, block board, etc. Or what formed by bonding surface decorative materials, such as a veneer, to both surfaces via the adhesive agent is mentioned. A production intermediate including an adhesive is obtained by superposing a surface decorative material on one or both sides of a base material with an adhesive interposed therebetween.
The wood material used as the base material may be a conventional material manufactured using an adhesive not containing fine carbon fibers, or a wood material manufactured using an adhesive containing fine carbon fibers. Also good. Examples of the surface decorative material to be laminated and bonded to the substrate include a veneer, paper, a synthetic resin sheet such as an olefin resin sheet and a vinyl chloride sheet, and melamine impregnated paper. The veneer may be a veneer obtained from a plantation tree in addition to a veneer obtained from a natural wood.
Examples of the shape of the substrate include various shapes such as a film, a sheet, a plate, and a three-dimensional molded product.
また基材には、用途に応じて、例えば、紫外線吸収剤、酸化防止剤、離型剤、帯電防止剤、着色剤、難燃剤、ガラス繊維等の繊維補強剤、無機充填剤等を１種または２種以上含有させたものを用いることができる。 In addition, for the base material, for example, an ultraviolet absorber, an antioxidant, a release agent, an antistatic agent, a colorant, a flame retardant, a fiber reinforcing agent such as glass fiber, an inorganic filler, etc. Or what was made to contain 2 or more types can be used.
次に、本発明で用いる接着剤について説明する。
本発明で用いる接着剤は、微細炭素繊維含有水性接着剤であることが好ましい。
微細炭素繊維は、その外径が、２００ｎｍ以下であることが好ましく、より好ましくは０．５〜１５０ｎｍのものである。
Next, the adhesive used in the present invention will be described.
The adhesive used in the present invention is preferably a fine carbon fiber-containing aqueous adhesive.
The fine carbon fiber preferably has an outer diameter of 200 nm or less, more preferably 0.5 to 150 nm.
本発明で使用する微細炭素繊維は、単層、二層および多層の微細炭素繊維であり、それぞれ目的に応じて用いることができる。多くの用途において、より好ましくは、多層の微細炭素繊維が用いられる。微細炭素繊維の製造方法に関しては、特に限定されないが、触媒を用いる気相成長法、アーク放電法、レーザー蒸発法およびＨｉＰｃｏ法（Ｈｉｇｈ−ｐｒｅｓｓｕｒｅ ｃａｒｂｏｎ ｍｏｎｏｘｉｄｅ ｐｒｏｃｅｓｓ）等、従来公知のいずれの製造方法も用いることができる。 The fine carbon fibers used in the present invention are single-layer, double-layer, and multilayer fine carbon fibers, and can be used according to the purpose. In many applications, more preferably, multi-layered fine carbon fibers are used. The method for producing the fine carbon fiber is not particularly limited, but any of the conventionally known production methods such as a vapor phase growth method using a catalyst, an arc discharge method, a laser evaporation method and a HiPco method (High-pressure carbon monoxide process) can be used. Can be used.
例えば、レーザー蒸着法により単層の微細炭素繊維を作製する方法を以下に示す。原料としてグラファイトパウダーと、ニッケルおよびコバルト微粉末混合ロットを用意する。この混合ロットを６６５ｈＰａ（５００Ｔｏｒｒ）のアルゴン雰囲気下、電気炉により１２５０℃で熱し、そこに３５０ｍＪ／ＰｕｌｓｅのＮｄ：ＹＡＧレーザーの第二高調波パルスを照射し、炭素と金属微粒子を蒸発させることにより、単層の微細炭素繊維を作製することができる。 For example, a method for producing a single-layer fine carbon fiber by laser vapor deposition is shown below. Prepare graphite powder and nickel and cobalt fine powder mixed lot as raw materials. This mixed lot was heated at 1250 ° C. in an electric furnace under an argon atmosphere of 665 hPa (500 Torr), and irradiated with a second harmonic pulse of 350 mJ / Pulse Nd: YAG laser to evaporate carbon and metal fine particles. A single-layer fine carbon fiber can be produced.
以上の作製方法は、あくまで典型例であり、金属の種類、ガスの種類、電気炉の温度、レーザーの波長等を変更してもよい。また、レーザー蒸着法以外の作製法、例えばＨｉＰｃｏ法、気相成長法、アーク放電法、一酸化炭素の熱分解法、微細な空孔中に有機分子を挿入して熱分解するテンプレート法、フラーレン・金属共蒸着法等、他の手法によって単層の微細炭素繊維を調製してもよい。 The above manufacturing method is merely a typical example, and the metal type, gas type, electric furnace temperature, laser wavelength, and the like may be changed. In addition, other than laser deposition methods, for example, HiPco method, vapor phase growth method, arc discharge method, carbon monoxide thermal decomposition method, template method in which organic molecules are inserted into fine pores, thermal decomposition, fullerene -You may prepare a single layer fine carbon fiber by other methods, such as a metal co-evaporation method.
例えば、定温アーク放電法により二層の微細炭素繊維を作製する方法を以下に示す。
基板は表面処理されたＳｉ基板を用い、処理方法としては触媒金属および触媒助剤金属を溶解した溶液中に、アルミナ粉末を３０分間浸し、さらに３時間超音波処理により分散させて得られた溶液をＳｉ基板に塗布し、空気中において１２０℃で２時間乾操させる。微細炭素繊維製造装置の反応室に基板を設置し、反応ガスとして水素とメタンの混合ガスを用い、ガスの供給量は水素を５００ｓｃｃｍ、メタンを１０ｓｃｃｍとし、反応室の圧力を７０Ｔｏｒｒとする。陰極部はＴａよりなる棒状の放電部を用いる。次に陽極部と陰極部および陽極部と基板との間に直流電圧を印加し、放電電流が２．５Ａで一定になるように放電電圧を制御する。放電により陰極部の温度が２３００℃になると正規グロー放電状態から異常グロー放電状態になり、放電電流が２．５Ａ、放電電圧が７００Ｖ、反応ガス温度が３０００℃での状態を１０分間行うことで、基板全体に単層および二層の微細炭素繊維を作製することができる。
For example, a method for producing a two-layer fine carbon fiber by a constant temperature arc discharge method is shown below.
The substrate was a surface-treated Si substrate, and the treatment method was a solution obtained by immersing alumina powder in a solution in which the catalyst metal and the catalyst auxiliary metal were dissolved for 30 minutes and then dispersing by ultrasonic treatment for 3 hours. Is applied to a Si substrate and dried in air at 120 ° C. for 2 hours. A substrate is installed in the reaction chamber of the fine carbon fiber production apparatus, a mixed gas of hydrogen and methane is used as a reaction gas, the supply amount of gas is 500 sccm for hydrogen, 10 sccm for methane, and the pressure in the reaction chamber is 70 Torr. The cathode part uses a rod-like discharge part made of Ta. Next, a DC voltage is applied between the anode part and the cathode part, and between the anode part and the substrate, and the discharge voltage is controlled so that the discharge current becomes constant at 2.5A. When the temperature of the cathode portion is 2300 ° C. due to discharge, the normal glow discharge state is changed to an abnormal glow discharge state, and the discharge current is 2.5 A, the discharge voltage is 700 V, and the reaction gas temperature is 3000 ° C. for 10 minutes. Single-layer and double-layer fine carbon fibers can be produced over the entire substrate.
以上の作製方法は、あくまで一例であり、金属の種類、ガスの種類等、諸条件を変更してもよい。また、アーク放電法以外の作製法によって二層の微細炭素繊維を調製してもよい。 The above manufacturing method is merely an example, and various conditions such as the type of metal and the type of gas may be changed. Further, a two-layer fine carbon fiber may be prepared by a production method other than the arc discharge method.
例えば、気相成長法により三次元構造を有する多層の微細炭素繊維を作製する方法を以下に示す。
基本的には、遷移金属超微粒子を触媒として炭化水素等の有機化合物をＣＶＤ法で化学熱分解して繊維構造体（以下、中間体）を得、これをさらに高温熱処理することで多層の微細炭素繊維を作製することができる。
For example, a method for producing a multi-layered fine carbon fiber having a three-dimensional structure by vapor deposition is shown below.
Basically, an organic compound such as a hydrocarbon is chemically pyrolyzed by CVD using transition metal ultrafine particles as a catalyst to obtain a fiber structure (hereinafter referred to as an intermediate), which is further subjected to high-temperature heat treatment to produce multilayer fine particles. Carbon fibers can be made.
原料有機化合物としては、べンゼン、トルエン、キシレンなどの炭化水素、一酸化炭素、エタノール等のアルコール類が使用できるが、炭素源として分解温度の異なる少なくとも２つ以上の炭素化合物を用いることが好ましい。なお、少なくとも２つ以上の炭素化合物とは、必ずしも原料有機化合物として２種以上のものを使用するというものではなく、原料有機化合物としては１種のものを使用した場合であっても、繊維構造体の合成過程においては、例えば、トルエンやキシレンの水素脱アルキル化などのような反応を生じて、その後の熱分解反応系においては分解温度の異なる２つ以上の炭素化合物となっているような態様を含むものである。雰囲気ガスには、アルゴン、へリウム、キセノン等の不活性ガスや水素を用い、触媒としては鉄、コバルト、モリブデンなどの遷移金属あるいはフェロセン、酢酸金属塩などの遷移金属化合物と硫黄あるいはチオフェン、硫化鉄などの硫黄化合物の混合物を使用する。 As the raw material organic compound, hydrocarbons such as benzene, toluene and xylene, alcohols such as carbon monoxide and ethanol can be used, but it is preferable to use at least two carbon compounds having different decomposition temperatures as a carbon source. . Note that at least two or more carbon compounds do not necessarily use two or more types of raw material organic compounds, and even when one type of raw material organic compound is used, the fiber structure In the body synthesis process, for example, a reaction such as hydrogen dealkylation of toluene or xylene occurs, and in the subsequent thermal decomposition reaction system, it becomes two or more carbon compounds having different decomposition temperatures. Including embodiments. The atmosphere gas is an inert gas such as argon, helium, or xenon, or hydrogen, and the catalyst is a transition metal such as iron, cobalt, or molybdenum, or a transition metal compound such as ferrocene or metal acetate, and sulfur or thiophene or sulfide. Use a mixture of sulfur compounds such as iron.
中間体の合成は、通常行われている炭化水素などのＣＶＤ法を用い、原料となる炭化水素および触媒の混合液を蒸発させ、水素ガス等をキャリアガスとして反応炉内に導入し、８００〜１３００℃での温度で熱分解する。これにより、１５〜１００ｎｍの外径を有する炭素繊維が、相互に前記触媒の粒子を核として成長した粒状体部で結合した疎な三次元構造を有する微細炭素繊維構造体（中間体）が複数集まった数ｃｍから数十ｃｍの大きさの集合体が合成される。 The synthesis of the intermediate is carried out by using a CVD method such as hydrocarbon which is usually performed, evaporating a mixture of hydrocarbon and catalyst as raw materials, introducing hydrogen gas or the like into the reaction furnace as a carrier gas, Pyrolysis at a temperature of 1300 ° C. As a result, a plurality of fine carbon fiber structures (intermediates) having a sparse three-dimensional structure in which carbon fibers having an outer diameter of 15 to 100 nm are bonded to each other by granular parts grown using the catalyst particles as nuclei. Aggregates having a size of several centimeters to several tens of centimeters are synthesized.
原料となる炭化水素の熱分解反応は、主として触媒粒子ないしこれを核として成長した粒状体表面において生じ、分解によって生じた炭素の再結晶化が当該触媒粒子ないし粒状体より一定方向に進むことで、繊維状に成長する。
しかしこの熱分解速度と成長速度とのバランスの意図的な変化、例えば上記したように炭素源として分解温度の異なる少なくとも２つ以上の炭素化合物を用いることで、一次元的方向にのみ炭素物質を成長させることなく、粒状体を中心として三次元的に炭素物質を成長させる。このような三次元的な微細炭素繊維の成長は、熱分解速度と成長速度とのバランスにのみ依存するものではなく、触媒粒子の結晶面選択性、反応炉内における滞留時間、炉内温度分布等によっても影響を受ける。概して、上記したような原料有機化合物の熱分解速度よりも炭素原子の再結晶化による成長速度の方が速いと、炭素物質は繊維状に成長し、一方、成長速度よりも熱分解速度の方が速いと、炭素物質は触媒粒子の周面方向に成長する。従って、熱分解速度と成長速度とのバランスを意図的に変化させることで、上記したような炭素物質の成長を一定方向とすることなく、制御下に多方向化して、三次元構造を形成することができるものである。なお、生成する中間体において、繊維が粒状体により相互に結合された前記のような三次元構造を容易に形成させるためには、触媒等の組成、反応炉内における滞留時間、反応温度およびガス温度等も最適化することが好ましい。
The thermal cracking reaction of the hydrocarbon as a raw material mainly occurs on the surface of the granular particles grown using the catalyst particles or the core, and the recrystallization of carbon generated by the decomposition proceeds in a certain direction from the catalytic particles or granular materials. Grows in a fibrous form.
However, by intentionally changing the balance between the thermal decomposition rate and the growth rate, for example, using at least two or more carbon compounds having different decomposition temperatures as a carbon source as described above, the carbon material can be changed only in a one-dimensional direction. Without growing, the carbon material is grown three-dimensionally around the granular material. The growth of such three-dimensional fine carbon fibers does not depend only on the balance between the thermal decomposition rate and the growth rate, but the crystal surface selectivity of the catalyst particles, the residence time in the reactor, and the temperature distribution in the furnace It is also affected by such factors. In general, when the growth rate by recrystallization of carbon atoms is faster than the thermal decomposition rate of the raw organic compound as described above, the carbon material grows in a fibrous form, while the thermal decomposition rate is higher than the growth rate. Is faster, the carbon material grows in the direction of the circumferential surface of the catalyst particles. Therefore, by deliberately changing the balance between the pyrolysis rate and the growth rate, the growth of the carbon material as described above is made multi-directional under control to form a three-dimensional structure. It is something that can be done. In order to easily form the three-dimensional structure in which the fibers are bonded to each other by the granular material in the intermediate product to be produced, the composition of the catalyst, the residence time in the reaction furnace, the reaction temperature, and the gas It is preferable to optimize the temperature and the like.
触媒および炭化水素の混合ガスを８００〜１３００℃での範囲の一定温度で加熱生成して得られた中間体は、炭素原子からなるパッチ状のシート片を貼り合わせたような構造を有し、ラマン分光分析では、欠陥が多いことを示すＤバンドが非常に大きく出る。また、生成した中間体は、未反応原料、非繊維状炭素物、タール分および触媒金属を含んでいる。 The intermediate obtained by heating and generating a mixed gas of catalyst and hydrocarbon at a constant temperature in the range of 800 to 1300 ° C. has a structure such that patch-like sheet pieces made of carbon atoms are bonded together, In the Raman spectroscopic analysis, a D band indicating that there are many defects appears very large. Moreover, the produced | generated intermediate body contains the unreacted raw material, non-fibrous carbon material, a tar content, and a catalyst metal.
従って、このような中間体から触媒金属等の残留物を除去し、欠陥が少ない所期の微細炭素繊維構造体を得るために、適切な方法で２４００〜３０００℃の高温熱処理を行う。 Accordingly, high temperature heat treatment at 2400 to 3000 ° C. is performed by an appropriate method in order to remove the catalyst metal and other residues from such an intermediate and to obtain an intended fine carbon fiber structure with few defects.
すなわち、例えば、この中間体を８００〜１２００℃で加熱して未反応原料やタール分などの揮発分を除去した後、２４００〜３０００℃の高温でアニール処理することによって所期の構造体を調製し、同時に繊維に含まれる触媒金属を蒸発させて除去する。なお、この際、物質構造を保護するために不活性ガス雰囲気中に還元ガスまたは微量の一酸化炭素ガスを添加してもよい。 That is, for example, the intermediate is heated at 800 to 1200 ° C. to remove volatile components such as unreacted raw materials and tars, and then annealed at a high temperature of 2400 to 3000 ° C. to prepare the desired structure. At the same time, the catalyst metal contained in the fiber is removed by evaporation. At this time, a reducing gas or a small amount of carbon monoxide gas may be added to the inert gas atmosphere in order to protect the material structure.
前記中間体を２４００〜３０００℃の範囲の温度でアニール処理すると、炭素原子からなるパッチ状のシート片は、それぞれ結合して複数のグラフェンシート状の層を形成する。 When the intermediate is annealed at a temperature in the range of 2400 to 3000 ° C., the patch-like sheet pieces made of carbon atoms are bonded to each other to form a plurality of graphene sheet-like layers.
また、このような高温熱処理前もしくは処理後において、微細炭素繊維構造体の円相当平均径を数ｃｍに解砕処理する工程と、解砕処理された微細炭素繊維構造体の円相当平均径を５０〜１００μｍに粉砕処理する工程とを経ることで、所望の円相当平均径を有する微細炭素繊維を作製する。 Further, before or after such high-temperature heat treatment, the step of crushing the equivalent circle average diameter of the fine carbon fiber structure to several centimeters, and the equivalent circle average diameter of the fine carbon fiber structure subjected to the crush treatment The fine carbon fiber which has a desired circle equivalent average diameter is produced through the process of grind | pulverizing to 50-100 micrometers.
以上の作製方法は、あくまで一例であり、金属の種類、ガスの種類等、諸条件を変更してもよい。また、気相成長法以外の作製法によって作製された多層の微細炭素繊維を使用してもよい。 The above manufacturing method is merely an example, and various conditions such as the type of metal and the type of gas may be changed. Moreover, you may use the multilayer fine carbon fiber produced by production methods other than a vapor phase growth method.
微細炭素繊維含有水性接着剤は、公知の水性接着剤に対して微細炭素繊維を添加することにより得られる。水性接着剤に微細炭素繊維を添加して微細炭素繊維含有水性接着剤を製造する場合、微細炭素繊維の添加量は、熱伝導性の向上及び微細炭素繊維の安定な分散状態を得る観点から、水性接着剤１００質量部に対して０．０１〜３０質量部であることが好ましく、より好ましくは０．２〜２０質量部であり、更に好ましくは０．５〜１５質量部である。 The fine carbon fiber-containing aqueous adhesive is obtained by adding fine carbon fibers to a known aqueous adhesive. When a fine carbon fiber-containing water-based adhesive is produced by adding fine carbon fibers to the aqueous adhesive, the amount of fine carbon fibers added is from the viewpoint of obtaining an improved thermal conductivity and a stable dispersion state of the fine carbon fibers. It is preferable that it is 0.01-30 mass parts with respect to 100 mass parts of aqueous adhesives, More preferably, it is 0.2-20 mass parts, More preferably, it is 0.5-15 mass parts.
また、同様の観点から、微細炭素繊維の添加量は、水性接着剤中の主剤固形分（特に接着剤中の樹脂分）１００質量部に対して０．０１〜３０質量部であることが好ましく、より好ましくは０．１〜１０質量部であり、更に好ましくは０．３〜５質量部である。 From the same viewpoint, the amount of fine carbon fibers added is preferably 0.01 to 30 parts by mass with respect to 100 parts by mass of the main component solids in the aqueous adhesive (particularly the resin in the adhesive). More preferably, it is 0.1-10 mass parts, More preferably, it is 0.3-5 mass parts.
また、微細炭素繊維を添加する水性接着剤としては、各種公知のものを特に制限なく用いることができるが、酢酸ビニル系樹脂エマルジョン、アクリル系樹脂エマルジョン、アクリル−スチレン系樹脂エマルジョン、スチレン・ブタジエン系樹脂ラテックス（以下、ＳＢＲと称する）等の、合成樹脂ポリマーが水中に分散したエマルジョン型接着剤や、メラミン−ホルムアルデヒド縮合系樹脂、ユリア・メラミン−ホルムアルデヒド共縮合系樹脂、フェノール縮合系樹脂、レゾルシノール縮合系樹脂等の熱硬化性縮合型接着剤や、水性高分子イソシアネート系接着剤であることが好ましい。
通常、木質製品用としては水性接着剤が使用されるが、ポリエステル樹脂等から得られる化粧シートを木質基材に接着する場合には、アクリル系、ポリウレタン系等の溶剤系接着剤が使用されることもあり、この場合、当該接着剤に微細炭素繊維を添加してもよい。
As the water-based adhesive to which fine carbon fibers are added, various known ones can be used without particular limitation, but vinyl acetate resin emulsion, acrylic resin emulsion, acrylic-styrene resin emulsion, styrene / butadiene system Resin latex (hereinafter referred to as SBR) and other emulsion type adhesives in which a synthetic resin polymer is dispersed in water, melamine-formaldehyde condensation resin, urea-melamine-formaldehyde cocondensation resin, phenol condensation resin, resorcinol condensation It is preferably a thermosetting condensation adhesive such as a resin, or an aqueous polymer isocyanate adhesive.
Usually, water-based adhesives are used for wood products, but when a decorative sheet obtained from a polyester resin or the like is adhered to a wood base material, solvent-based adhesives such as acrylic and polyurethane are used. In this case, fine carbon fibers may be added to the adhesive.
酢酸ビニル系樹脂エマルジョンに含まれる樹脂成分としては、酢酸ビニル、プロピオン酸ビニル等の酢酸ビニル系モノマーの単独重合体又は共重合体、酢酸ビニルモノマーと他のビニル系モノマーとの共重合体等が挙げられる。ここでいう「他のビニル系モノマー」としては、例えば、特開２００５−３４４０８４号公報の段落〔００１０〕に記載のものが挙げられる。
ＳＢＲに含まれる樹脂成分としては、スチレン系モノマーとブタジエン系モノマーとの共重合体、又はこれらのモノマーと他のビニル系モノマーとの共重合体が挙げられる。ここでいう「他のビニル系モノマー」としては、例えば、特開２００５−３４４０８４号公報の段落〔００１７〕に記載のものが挙げられる。
アクリル系樹脂エマルジョンに含まれる樹脂成分としては、アクリル酸エステルモノマーの単独重合又は共重合体、或いはアクリル酸エステルモノマーと他のビニル系モノマーとの共重合体が挙げられる。ここでいう「他のビニル系モノマー」としては、例えば特開２００５−３４４０８４号公報の段落〔００１５〕に記載のものが挙げられる。
これらの接着剤は、一種を単独で用いることもできるし、二種以上を組み合わせて用いることもできる。
Examples of the resin component contained in the vinyl acetate resin emulsion include homopolymers or copolymers of vinyl acetate monomers such as vinyl acetate and vinyl propionate, and copolymers of vinyl acetate monomers with other vinyl monomers. Can be mentioned. Examples of the “other vinyl monomer” herein include those described in paragraph [0010] of JP-A-2005-344084.
Examples of the resin component contained in the SBR include a copolymer of a styrene monomer and a butadiene monomer, or a copolymer of these monomers and another vinyl monomer. Examples of the “other vinyl monomers” mentioned here include those described in paragraph [0017] of JP-A-2005-344084.
Examples of the resin component contained in the acrylic resin emulsion include a homopolymer or copolymer of an acrylate monomer, or a copolymer of an acrylate monomer and another vinyl monomer. Examples of the “other vinyl monomers” mentioned here include those described in paragraph [0015] of JP-A-2005-344084.
These adhesives can also be used individually by 1 type, and can also be used in combination of 2 or more type.
微細炭素繊維含有水性接着剤は、水性接着剤に対して、微細炭素繊維を添加して調製することが好ましい。また、微細炭素繊維の安定な分散状態を得る観点から、微細炭素繊維と共に微細炭素繊維分散剤を添加することも好ましい。微細炭素繊維及び微細炭素繊維分散剤を添加する場合、両者を同時に添加してもよく、順次添加してもよい。また、交互に添加してもよい。順次添加する場合、微細炭素繊維分散剤を水性接着剤に添加した後に微細炭素繊維を添加する方が好ましい。また、微細炭素繊維分散剤を水性接着剤に添加した後に微細炭素繊維を添加して分散処理をし、微細炭素繊維分散液を調製した後で添加剤を添加したほうがよい。また、微細炭素繊維の凝集体を十分に解繊・分散させ、該凝集体が５μｍ以下となる微細炭素繊維分散液を得ることが好ましいが、そのためには、水性接着剤に対して、少なくとも前記の微細炭素繊維分散剤と微細炭素繊維を添加し、あらかじめ微細炭素繊維の凝集体を十分に解繊・分散せしめた後、所望の各種添加剤を加えるほうが好ましい。特に、水性接着剤中で粘性を示す樹脂成分等の添加剤については、該添加剤の添加を、微細炭素繊維の分散操作時に、あるいは分散操作に先だって行うと、その粘性のために微細炭素繊維の凝集体の十分な解繊・分散が得られず、５μｍを超える凝集体が残り、所望の分散状態の微細炭素繊維分散液が得られない恐れがある。 The fine carbon fiber-containing aqueous adhesive is preferably prepared by adding fine carbon fibers to the aqueous adhesive. From the viewpoint of obtaining a stable dispersion state of fine carbon fibers, it is also preferable to add a fine carbon fiber dispersant together with the fine carbon fibers. When adding a fine carbon fiber and a fine carbon fiber dispersant, both may be added simultaneously or sequentially. Moreover, you may add alternately. When adding sequentially, it is more preferable to add a fine carbon fiber after adding a fine carbon fiber dispersing agent to an aqueous adhesive. Moreover, after adding a fine carbon fiber dispersing agent to a water-based adhesive, it is better to add a fine carbon fiber, and after carrying out a dispersion process and preparing a fine carbon fiber dispersion, an additive is added. In addition, it is preferable to sufficiently defibrate and disperse the aggregate of fine carbon fibers to obtain a fine carbon fiber dispersion liquid in which the aggregate is 5 μm or less. It is more preferable to add the fine carbon fiber dispersant and the fine carbon fiber, sufficiently disaggregate and disperse the fine carbon fiber aggregates in advance, and then add various desired additives. In particular, for additives such as resin components that exhibit viscosity in aqueous adhesives, if the additive is added during or prior to the dispersion of fine carbon fibers, the fine carbon fibers are used due to their viscosity. Sufficient defibration / dispersion of the agglomerates cannot be obtained, and agglomerates exceeding 5 μm remain, and there is a possibility that a fine carbon fiber dispersion in a desired dispersion state cannot be obtained.
さらに、水性接着剤１００質量部に対して、５質量部を超える微細炭素繊維を分散させようとする場合は、あらかじめ水性接着剤に微細炭素繊維分散剤を添加し溶解させた後、微細炭素繊維を添加するほうが、微細炭素繊維の良好な分散のために好ましい。 Furthermore, when it is going to disperse | distribute the fine carbon fiber exceeding 5 mass parts with respect to 100 mass parts of aqueous adhesives, after adding a fine carbon fiber dispersing agent to an aqueous adhesive beforehand and making it melt | dissolve, fine carbon fiber Is preferable for good dispersion of the fine carbon fibers.
水性接着剤に微細炭素繊維を分散させる分散処理には、一般的な分散機を用いることができる。例えば、ビーズミル分散機、ＴＫラボディスパー、ＴＫフィルミックス、ＴＫパイプラインミクサー、ＴＫホモミックラインミル、ＴＫホモジェッター、ＴＫユニミキサー、ＴＫホモミックラインフロー、ＴＫアジホモディスパー（以上、特殊機化工業（株）製）、ホモジナイザー・ポリトロン（（株）セントラル科学貿易製）、ホモジナイザー・ヒストロン（（株）日音医理科機器製作所製）、バイオミキサー（（株）日本精機製作所製）、ターボ型撹拌機（（株）小平製作所製）、ウルトラディスパー（浅田鉄鋼（株）製）、エバラマイルザー（荏原製作所（株）製）、超音波装置または超音波洗浄機（アズワン（株）製）等が挙げられる。これらの機器を用いて分散処理を行なう際の、該機器等の条件設定は、所望する微細炭素繊維の分散状態に応じて、適宜設定すればよい。 A general disperser can be used for the dispersion treatment in which fine carbon fibers are dispersed in the aqueous adhesive. For example, bead mill disperser, TK lab disper, TK fill mix, TK pipeline mixer, TK homomic line mill, TK homo jetter, TK unimixer, TK homomic line flow, TK azimu homo disper ), Homogenizer polytron (manufactured by Central Science Trading Co., Ltd.), homogenizer histron (manufactured by Nissin Medical Science Equipment Co., Ltd.), biomixer (manufactured by Nippon Seiki Seisakusho Co., Ltd.), turbo-type stirring Machines (manufactured by Kodaira Manufacturing Co., Ltd.), Ultra Dispers (manufactured by Asada Steel Co., Ltd.), Ebara Mileser (manufactured by Ebara Manufacturing Co., Ltd.), ultrasonic equipment or ultrasonic cleaners (manufactured by ASONE Corporation), etc. Can be mentioned. What is necessary is just to set suitably the conditions of this apparatus etc. when performing dispersion processing using these apparatuses according to the dispersion state of the desired fine carbon fiber.
微細炭素繊維分散剤としては、アニオン性、カチオン性又はノニオン性の界面活性剤を用いることができるが、溶剤系接着剤の場合は、使用される溶剤に溶解する界面活性剤が好ましく、水性接着剤の場合は、水溶性の界面活性剤を用いることが好ましい。微細炭素繊維分散剤は、一種を単独で用いることもできるし、二種以上を組み合わせて用いることもできる。 As the fine carbon fiber dispersant, an anionic, cationic or nonionic surfactant can be used. In the case of a solvent-based adhesive, a surfactant that dissolves in the solvent used is preferable, and an aqueous adhesive is used. In the case of an agent, it is preferable to use a water-soluble surfactant. A fine carbon fiber dispersing agent can also be used individually by 1 type, and can also be used in combination of 2 or more type.
水性接着剤に対する微細炭素繊維分散剤の添加量は、該微細炭素繊維の添加量に対して０．１〜２００質量％が好ましく、より好ましくは１〜１００質量％である。 The addition amount of the fine carbon fiber dispersant with respect to the aqueous adhesive is preferably 0.1 to 200% by mass, more preferably 1 to 100% by mass with respect to the addition amount of the fine carbon fiber.
また、微細炭素繊維含有水性接着剤は、更に、熱圧接着時に発生し得る膨れや反り等の様々な不具合の防止ないし軽減、製品の仕上がりや接着剤の充填効果の向上等を目的として、架橋剤や小麦粉等の充填剤等の添加剤を含むことができ、その種類や添加量は特に制限されない。 In addition, the fine carbon fiber-containing water-based adhesive is further cross-linked for the purpose of preventing or reducing various problems such as blistering and warping that can occur during hot-pressure bonding, improving the finish of the product, and the filling effect of the adhesive. An additive such as a filler or a filler such as flour can be included, and the type and amount thereof are not particularly limited.
また、微細炭素繊維含有水性接着剤には、必要に応じ、その種類の水性接着剤に従来配合されている各種公知の成分を配合することもできる。 Moreover, various well-known components conventionally mix | blended with the kind of water-based adhesive can also be mix | blended with the fine carbon fiber containing water-based adhesive as needed.
本発明の木質製品の製造方法により、上述した木質複合材を製造するには、例えば、上述した基材の両面又は片面に上述した微細炭素繊維含有水性接着剤を塗布し、その塗布面に突板等の表面化粧材を重ね蒸気プレス等のホットプレスに導入して熱圧締する。熱圧締の温度は、熱圧締時間の短縮と製品の含水率や反り等への影響とのバランスをとる観点等から９０〜１４０℃が好ましく、より好ましくは１００〜１２０℃である。また、熱圧締の時間は、適宜に決定することができるが、熱圧締時間の短縮と使用する接着剤の硬化性とのバランスをとる観点等から、例えば、約０．３ｍｍ厚の湿式化粧単板を接着して天然木化粧合板を製造する場合には、２５〜４５秒が好ましく、より好ましくは３５〜４０秒である。 In order to produce the above-described wood composite material by the wood product production method of the present invention, for example, the above-mentioned fine carbon fiber-containing water-based adhesive is applied to both surfaces or one surface of the above-mentioned base material, and the veneer is applied to the coated surface. Etc. are introduced into a hot press such as a steam press and hot pressed. The temperature of the hot pressing is preferably 90 to 140 ° C., more preferably 100 to 120 ° C. from the viewpoint of balancing the shortening of the hot pressing time and the influence on the moisture content and warpage of the product. In addition, the hot pressing time can be determined as appropriate, but from the viewpoint of balancing the shortening of the hot pressing time with the curability of the adhesive used, for example, a wet press with a thickness of about 0.3 mm is used. In the case of producing a natural wood decorative plywood by bonding a decorative veneer, the time is preferably 25 to 45 seconds, more preferably 35 to 40 seconds.
本発明の木質製品の製造方法によれば、接着剤に熱伝導性に優れた微細炭素繊維を含ませることによって、ホットプレスからの熱が接着剤に良好に伝達されるため、接着剤の硬化速度が向上し、個々の木質製品の熱圧締に要する時間の短縮化を図ることができる。これにより、木質製品の生産性が向上する。
また、微細炭素繊維の被着材へのアンカー効果によって初期接着力が高まると推察され、熱圧締時間の短縮化に寄与する。これに対して、炭素粒子やカーボンファイバーを添加した接着剤を配合した場合には、これらは外径が数十μｍで、微細炭素繊維に比して嵩高く絡みにくいため、むしろ接着力が低下する。
According to the method for producing a woody product of the present invention, the heat from the hot press is well transferred to the adhesive by including the fine carbon fiber excellent in thermal conductivity in the adhesive, so that the adhesive is cured. The speed can be improved and the time required for hot-pressing individual wood products can be shortened. This improves the productivity of the wooden product.
Moreover, it is speculated that the initial adhesive force is increased by the anchor effect of the fine carbon fiber to the adherend, which contributes to shortening of the hot pressing time. On the other hand, when blended with carbon particles or carbon fiber-added adhesives, these have an outer diameter of several tens of μm and are bulky and difficult to get entangled compared to fine carbon fibers. To do.
また、本発明で使用する微細炭素繊維は、ＭＤＩのような硬化促進剤ではないため、接着剤の可使時間への影響も小さい。
また、微細炭素繊維を分散した接着剤に関して、長時間での保存安定性が極めて良好であり、微細炭素繊維を分散していないものと比較しても、遜色のない保存安定性が確保できる。
Moreover, since the fine carbon fiber used in the present invention is not a curing accelerator such as MDI, the influence on the usable life of the adhesive is small.
Moreover, regarding the adhesive in which fine carbon fibers are dispersed, the storage stability in a long time is very good, and the storage stability comparable to that in which fine carbon fibers are not dispersed can be secured.
微細炭素繊維含有水性接着剤を基材に塗布する方法としては、各種公知の塗布方法を特に制限なく用いることができるが、例えば、ハケ、ブラシ、ハンドローラーによる塗布、ロールコーター、ロールスプレッダーによる塗布、エアースプレー、エアレススプレー、低圧霧化スプレーによる塗布、バーコーダー法による塗布、スピンコーター、ディップコーターを用いた塗布等が挙げられる。 As a method for applying the fine carbon fiber-containing water-based adhesive to the substrate, various known application methods can be used without particular limitation. For example, application by brush, brush, hand roller, application by roll coater, roll spreader Application by air spray, airless spray, low-pressure atomization spray, application by bar coder method, application using spin coater, dip coater, and the like.
本発明の木質製品の製造方法は、前述のように、木質製品として、天然木化粧合板等の特殊加工合板等の、基材の片面又は両面に表面化粧材を熱圧接着した木質複合材を製造するのに代えて、木質製品として、合板、単板積層材（ＬＶＬ）、パーティクルボード（ＰＢ）、ファイバーボード、ＯＳＢ、集成材、ブロックボード等の木質材を製造するものであってもよい。これらの場合、従来の方法と同様にして、これらの木質材を製造するに当たり、単板間に微細炭素繊維を含む接着剤を介在させたり、エレメントどうしを結合させるバインダーとして、微細炭素繊維を含む接着剤を用いる。 As described above, the method for producing a woody product of the present invention is a woody composite material in which a surface decorative material is bonded to one surface or both surfaces of a base material such as a specially processed plywood such as a natural wood decorative plywood. Instead of manufacturing, wood products such as plywood, veneer laminate (LVL), particle board (PB), fiber board, OSB, laminated wood, block board, etc. may be produced as wood products. . In these cases, when producing these wood materials in the same manner as in the conventional method, an adhesive containing fine carbon fibers is interposed between the single plates, or fine carbon fibers are included as a binder for bonding the elements together. Use an adhesive.
例えば、合板又は単板積層材を製造する場合には、複数枚の単板を、単板どうし間に微細炭素繊維を含む接着剤を介在させて積層した後、これらを、ホットプレスにより一体的に熱圧締して、合板又は単板積層材を得る。
また、パーティクルボード（ＰＢ）、ファイバーボード、ＯＳＢを製造する場合には、エレメント（切削片、小片，繊維等）と微細炭素繊維を含む接着剤とを混合してフォーミングした後、これらを、ホットプレスにより一体的に熱圧締して、パーティクルボード（ＰＢ）、ファイバーボード又はＯＳＢを得る。
また、集成材、ブロックボード等を製造する場合には、ひき板、小角材、ブロック状の小片を、目的とする形状になるように並べ、それらの相互間を、微細炭素繊維を含む接着剤で接合した後、それらを、ホットプレスにより一体的に熱圧締して、集成材、ブロックボードを得る。
このような木質製品を製造する場合にも、上述した微細炭素繊維を含有する接着剤が好ましく用いられる。
For example, when manufacturing a plywood or a veneer laminate, after laminating a plurality of veneers with an adhesive containing fine carbon fibers interposed between the veneers, these are integrated by hot pressing. To obtain a plywood or veneer laminate.
When manufacturing particle boards (PB), fiber boards, and OSBs, elements (cut pieces, small pieces, fibers, etc.) and an adhesive containing fine carbon fibers are mixed and formed, and then these are heated. A particle board (PB), fiber board, or OSB is obtained by hot-pressing integrally by pressing.
Moreover, when manufacturing laminated timber, block board, etc., it arranges so that a board, a small square material, and a block-like piece may become the target shape, and the adhesive agent which contains fine carbon fiber between them. Then, they are integrally heat-pressed by hot pressing to obtain a laminated material and a block board.
Also when manufacturing such a wooden product, the adhesive agent containing the fine carbon fiber mentioned above is used preferably.
本発明の木質製品の製造方法で製造した木質材や複合木質材は、多様な用途に好ましく用いることができ、用途は特に制限はないが、例えば、天井、床、建具等の造作材、机（天板等）、箱棚、タンス、ベッド等の家具、床材、化粧フローリング材、階段の踏み板、間仕切り壁の構成材等として用いることができる。また、木質材や複合木質材は、人の目に触れる側の表面等に、樹脂フィルムや化粧紙等の化粧シートを貼着したり、強度を向上させたり色を変化させたりする塗装を更に施してもよい。 The wood material and composite wood material produced by the method for producing a wood product of the present invention can be preferably used for various uses, and the use is not particularly limited. For example, a construction material such as a ceiling, a floor, and a joinery, a desk (Top plate, etc.), furniture such as box shelf, chest, bed, etc., flooring, decorative flooring, stair tread, partition wall, etc. In addition, for wooden materials and composite wooden materials, a decorative sheet such as a resin film or decorative paper is applied to the surface that is in contact with the human eye, or a coating that improves strength or changes color is further applied. You may give it.
次に、実施例及び比較例に基づいて本発明を具体的に説明するが、本発明は、以下の実施例によって何ら限定されるものではない。以下の説明において、特に断らない限り、「部」は「質量部」、「％」は「質量％」を意味する。 Next, the present invention will be specifically described based on examples and comparative examples, but the present invention is not limited to the following examples. In the following description, “part” means “part by mass” and “%” means “% by mass” unless otherwise specified.
１．接着剤の調製
〔接着剤ａ１〕
酢酸ビニル系の水性接着剤（住友林業クレスト株式会社製、商品名「インスターボンドＫＨ−１０９３」、固形分（樹脂分）５１％）１００部に、硬化剤Ａ（住友林業クレスト株式会社製、商品名「ハードナーＨ−４０００」）１０部他を混合して接着剤ａ１を得た。
〔接着剤ａ２〕
接着剤ａ１と同一の水性接着剤（固形分（樹脂分）５１％）に、該固形分の３％に相当する量の微細炭素繊維を配合して分散させた。そして、この分散液１００部に対して、硬化剤Ａ１０部他を混合して接着剤ａ２を得た。
1. Preparation of adhesive [Adhesive a1]
100 parts vinyl acetate-based water-based adhesive (manufactured by Sumitomo Forestry Crest Co., Ltd., trade name “Instar Bond KH-1093”, solid content (resin content) 51%), hardener A (manufactured by Sumitomo Forestry Crest Co., Ltd., A product name "Hardener H-4000") 10 parts and others were mixed to obtain an adhesive a1.
[Adhesive a2]
An amount of fine carbon fiber corresponding to 3% of the solid content was blended and dispersed in the same aqueous adhesive (solid content (resin content) 51%) as that of the adhesive a1. And 100 parts of this dispersion was mixed with 10 parts of curing agent A to obtain an adhesive a2.
〔接着剤ａ３〕
接着剤ａ１と同一の水性接着剤（固形分（樹脂分）５１％）に、該固形分の２．２５％に相当する量の微細炭素繊維を配合して分散させた。そして、この分散液１００部に対して、硬化剤Ａ１０部他を混合して接着剤ａ３を得た。
〔接着剤ａ４〕
接着剤ａ１と同一の水性接着剤（固形分（樹脂分）５１％）に、該固形分の１．５％に相当する量の微細炭素繊維を配合して分散させた。そして、この分散液１００部に対して、硬化剤Ａ１０部他を混合して接着剤ａ４を得た。
[Adhesive a3]
An amount of fine carbon fiber corresponding to 2.25% of the solid content was blended and dispersed in the same aqueous adhesive (solid content (resin content) 51%) as that of the adhesive a1. And 100 parts of this dispersion was mixed with 10 parts of curing agent A to obtain an adhesive a3.
[Adhesive a4]
An amount of fine carbon fiber corresponding to 1.5% of the solid content was mixed and dispersed in the same aqueous adhesive (solid content (resin content) 51%) as that of the adhesive a1. And 100 parts of this dispersion was mixed with 10 parts of curing agent A to obtain an adhesive a4.
〔接着剤ｂ１〕
ＳＢＲ系の水性接着剤（住友林業クレスト株式会社製、商品名「インスターボンドＬＢ３７０」、固形分（樹脂分）３８％）１００部に対して硬化剤Ｂ（住友林業クレスト株式会社製、商品名「ハードナーＨ−３７０」）５部他を混合して、接着剤ｂ１を得た。
〔接着剤ｂ２〕
接着剤ｂ１と同一の水性接着剤（固形分（樹脂分）３８％）に、該固形分の３％に相当する量の微細炭素繊維を配合して分散させた。そして、この分散液１００部に対して硬化剤Ｂ５部他を混合して、接着剤ｂ２を得た。
[Adhesive b1]
SBR-based water-based adhesive (manufactured by Sumitomo Forestry Crest Co., Ltd., trade name “Instar Bond LB370”, solid content (resin content) 38%) 100 parts hardener B (Sumitomo Forestry Crest Co., Ltd., trade name) "Hardener H-370") 5 parts and others were mixed to obtain an adhesive b1.
[Adhesive b2]
An amount of fine carbon fiber corresponding to 3% of the solid content was blended and dispersed in the same aqueous adhesive (solid content (resin content) 38%) as the adhesive b1. And 100 parts of this dispersion was mixed with 5 parts of curing agent B and others to obtain an adhesive b2.
〔接着剤ｃ１〕
ＳＢＲ系の水性接着剤（固形分（樹脂分）３８％）１００部に、５０部のユリア・メラミン−ホルムアルデヒド縮合系接着剤（固形分（樹脂分）５２％）、小麦粉３０部及び塩化アンモニウム０．１部を均一に混合して、接着剤ｃ１を得た。
〔接着剤ｃ２〕
接着剤ｃ１と同一の水性接着剤（固形分（樹脂分）３８％）に、該固形分の３％に相当する量の微細炭素繊維を配合して分散させた。そして、この分散液１００部に対して、５０部のユリア・メラミン−ホルムアルデヒド縮合系接着剤（固形分（樹脂分）５２％）、小麦粉３０部及び塩化アンモニウム０．１部を均一に混合して、接着剤ｃ２を得た。
[Adhesive c1]
100 parts of SBR-based aqueous adhesive (solid content (resin content) 38%), 50 parts of urea / melamine-formaldehyde condensation adhesive (solid content (resin content) 52%), 30 parts of flour and ammonium chloride 0 .1 part was mixed uniformly to obtain an adhesive c1.
[Adhesive c2]
An amount of fine carbon fiber corresponding to 3% of the solid content was blended and dispersed in the same aqueous adhesive (solid content (resin content) 38%) as the adhesive c1. To 100 parts of this dispersion, 50 parts of urea / melamine / formaldehyde condensation adhesive (solid content (resin content) 52%), 30 parts of flour and 0.1 part of ammonium chloride were mixed uniformly. An adhesive c2 was obtained.
表１に、得られた各接着剤について、水性接着剤の樹脂分１００部に対する微細炭素繊維の配合量（部）を示した。表１中、「硬化剤Ａ」より上の各項目における括弧内の数値は、各項目に記載の接着剤（以下、主剤接着剤という）１００部中の固形分割合（部）を示し、「硬化剤Ａ」から「塩化アンモニウム」までの各項目は、前記の主剤接着剤１００部に対して添加した物質の添加量（水分を含む量、部）及びその固形分量（部）を示し、「計」の項の括弧内の数値は、最終的に得られた接着剤中の固形分割合（実測値）を示す。なお、硬化剤Ａの固形分割合は１５％、硬化剤Ｂの固形分割合は８％、小麦粉の固形分割合は８５％であった。
接着剤ａ２〜ａ４，ｂ２，ｃ２には、微細炭素繊維として、平均直径が６０ｎｍの微細炭素繊維を用いた。
Table 1 shows the blending amount (parts) of fine carbon fibers with respect to 100 parts of the resin content of the aqueous adhesive for each of the obtained adhesives. In Table 1, numerical values in parentheses in each item above “curing agent A” indicate a solid content ratio (parts) in 100 parts of the adhesive (hereinafter referred to as main agent adhesive) described in each item. Each item from “curing agent A” to “ammonium chloride” indicates the amount of the substance added to 100 parts of the main agent adhesive (amount including water, part) and its solid content (part). The numerical value in parentheses in the “Total” section indicates the solid content ratio (actual measurement value) in the finally obtained adhesive. The solid content ratio of the curing agent A was 15%, the solid content ratio of the curing agent B was 8%, and the solid content ratio of the flour was 85%.
For the adhesives a2 to a4, b2 and c2, fine carbon fibers having an average diameter of 60 nm were used as fine carbon fibers.
２．複合木質材の製造及び評価
実施例１〜１２及び比較例１〜８のそれぞれについて、縦横３００ｍｍ、厚さ１２ｍｍの合板に、表２に示す接着剤を、表２に示す量（６７又は１００ｇ／ｍ2）塗布し、０．３ｍｍ厚のナラ湿潤単板を乗せた。そして、ホットプレス（平板プレス）を用いて、１１０℃で４０秒間又は６０秒間熱圧接着した。プレス圧は０．６ＭＰａ（一定）とした。解圧直後にナイフ試験を行った。また、これを２４時間養生した後に、合板の日本農林規格に基づいて７５ｍｍ×７５ｍｍの大きさにカットして試験片とし、一類浸漬剥離試験を行った。それらの結果を表２に示した。
2. Production and Evaluation of Composite Wood Material For each of Examples 1 to 12 and Comparative Examples 1 to 8, the adhesive shown in Table 2 was added to the plywood having a length and width of 300 mm and a thickness of 12 mm (67 or 100 g / m 2 ) was applied, and a 0.3 mm thick oak wet veneer was placed. Then, hot press bonding was performed at 110 ° C. for 40 seconds or 60 seconds using a hot press (flat plate press). The press pressure was 0.6 MPa (constant). A knife test was performed immediately after decompression. Moreover, after curing this for 24 hours, based on the Japanese agricultural and forestry standard of a plywood, it cut | disconnected to the magnitude | size of 75 mm x 75 mm, and was set as the test piece, and the one-type immersion peeling test was done. The results are shown in Table 2.
ナイフ試験
プレス解圧直後にナイフで化粧単板に×印のキズを入れ、キズを入れた箇所から強制的に表面単板を引き剥がし、引き剥がす際の抵抗を評価した。引き剥がす際の抵抗感を人の感覚及び目視で判定し、抵抗感が極めて強く、また、接着層の材破率が極めて高いものを「◎」、引き剥がす際の抵抗感が強く、また、接着層の材破率が高いものを「○」、引き剥がす際の抵抗感が弱く、接着層の材破率が低いものを「△」として、相対比較を行った。
Knife test Immediately after the pressure was released from the press, scratches were applied to the decorative veneer with a knife, the surface veneer was forcibly peeled from the scratched area, and the resistance when peeling was evaluated. The resistance when peeling is judged by human sense and visual observation, the resistance is extremely strong, and the adhesive layer has a very high material breakage rate `` ◎ '', the resistance when peeling is strong, Relative comparisons were made with “○” indicating that the adhesive layer had a high material breakage rate, and “△” indicating that the material had a low resistance to tearing and a low material breakage rate.
一類浸漬剥離試験（煮沸繰返し試験）
合板の日本農林規格（ＪＡＳ特殊合板・１類浸漬はくり試験）に準拠して、試験片を沸騰水中に４時間浸漬した後、６０℃の温度で２０時間乾燥し、これを沸騰水中に４時間浸漬し、更に６０℃で３時問乾燥した。試験後、規格の適合基準に基づいて、同一接着層において剥離が生じなかったものを「◎」、２５ｍｍ以上の剥離が生じなかったものを「○」、２５ｍｍ以上の剥離が生じたものを「△」とした。
Type I immersion peeling test (boiling repeated test)
In accordance with the Japanese Agricultural Standards for Plywood (JAS Special Plywood Class 1 immersion peel test), the test piece is immersed in boiling water for 4 hours and then dried at a temperature of 60 ° C. for 20 hours. It was immersed for a period of time and further dried at 60 ° C. for 3 hours. After the test, based on conformity standards, “◎” indicates that no peeling occurred in the same adhesive layer, “◯” indicates that peeling did not occur 25 mm or more, and “0” indicates that peeling occurred 25 mm or more. Δ.
表２の比較例１と比較例２を比較すると、プレス時間（熱圧締時間）の短縮によりナイフ試験の結果が悪化している。これに対して、表２の比較例１と実施例２とを比較すると、実施例２の方がプレス時間（熱圧締時間）が短いにも拘わらずに、ナイフ試験及び１類浸漬剥離試験の結果は同等である。また、比較例３と比較例４を比較すると、プレス時間（熱圧締時間）の短縮によりナイフ試験及び１類浸漬剥離試験の結果が悪化しているのに対して、比較例３と実施例４とを比較すると、実施例４の方がプレス時間（熱圧締時間）が短いにも拘わらずに、ナイフ試験及び１類浸漬剥離試験の結果は同等である。
即ち、微細炭素繊維を添加することで、接着状態の悪化や接着強度等を犠牲にすることなく、熱圧締時間を短縮化させることができることが判る。
When Comparative Example 1 and Comparative Example 2 in Table 2 are compared, the result of the knife test is deteriorated due to the shortening of the press time (thermal pressing time). On the other hand, when Comparative Example 1 and Example 2 in Table 2 are compared, the knife test and the type 1 immersion peel test are performed although Example 2 has a shorter press time (thermal pressing time). The results are equivalent. Further, when Comparative Example 3 and Comparative Example 4 are compared, the results of the knife test and the Type 1 immersion peel test are deteriorated due to the shortening of the press time (thermal pressing time), whereas Comparative Example 3 and Example Compared with 4, the results of the knife test and the type 1 immersion peel test are the same in Example 4, although the press time (hot pressing time) is shorter.
That is, it can be seen that by adding fine carbon fibers, the hot pressing time can be shortened without sacrificing the deterioration of the bonding state or the bonding strength.
また、表２の比較例１と実施例３とを比較すると、実施例３の方が、接着剤の量を減らしているにも拘わらずにナイフ試験の結果が向上している。即ち、微細炭素繊維を添加することで、熱圧締時間を増加させることなく、接着剤の量を減らすことができることが判る。 Further, when comparing Comparative Example 1 and Example 3 in Table 2, the result of the knife test is improved in Example 3 although the amount of the adhesive is reduced. That is, it can be seen that by adding fine carbon fibers, the amount of adhesive can be reduced without increasing the hot pressing time.
表２に示すように、接着剤に微細炭素繊維を添加すると初期接着が向上し、プレス時間を短縮しても、接着性の良好な単板化粧合板（複合木質材）が得られることが判る。
（酢酸ビニル系接着剤）
微細炭素繊維入り接着剤では、プレス時間を２／３にしても、通常条件とほぼ同等の接着性が得られた。また、プレス時間を２／３かつ接着剤塗布量２／３にしても、通常条件とほぼ同等の接着性が得られた。
（ＳＢＲラテックス系接着剤、ＳＢＲラテックス／ユリア・メラミン−ホルムアルデヒド縮合系接着剤）
これらの接着剤についても、微細炭素繊維入り接着剤では、プレス時間を２／３にしても、通常条件とほぼ同等の接着性が得られた。また、プレス時間を２／３かつ接着剤塗布量２／３にしても、通常条件とほぼ同等の接着性が得られた。
As shown in Table 2, it can be seen that when fine carbon fibers are added to the adhesive, the initial adhesion is improved, and even if the pressing time is shortened, a single veneer decorative plywood (composite wood material) with good adhesion can be obtained. .
(Vinyl acetate adhesive)
With the adhesive containing fine carbon fibers, even when the press time was 2/3, adhesiveness almost equivalent to the normal condition was obtained. Further, even when the pressing time was 2/3 and the adhesive application amount was 2/3, the adhesiveness almost equivalent to the normal condition was obtained.
(SBR latex adhesive, SBR latex / urea / melamine-formaldehyde condensation adhesive)
As for these adhesives, the adhesive containing fine carbon fibers was able to obtain adhesiveness substantially equal to the normal conditions even when the press time was 2/3. Further, even when the pressing time was 2/3 and the adhesive application amount was 2/3, the adhesiveness almost equivalent to the normal condition was obtained.
このように、本発明によれば、例えば、熱圧プレスでのプレス時間を２／３に短縮することができ、熱圧プレス工程の生産効率を現状の１．５倍に向上させることが可能である。 Thus, according to the present invention, for example, the press time in the hot press can be shortened to 2/3, and the production efficiency of the hot press process can be improved to 1.5 times the current level. It is.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104385423A (en) * | 2014-10-20 | 2015-03-04 | 贵州恒力源林业科技有限公司 | Manufacturing method of composite artificial board |
| CN105965616A (en) * | 2016-02-03 | 2016-09-28 | 宁波中加低碳新技术研究院有限公司 | Method for manufacturing single substrate composite sheet material |
| CN110712257A (en) * | 2019-11-01 | 2020-01-21 | 国家林业和草原局竹子研究开发中心 | Biomass charcoal-based anticorrosive, mildew-proof and environment-friendly artificial board |
| JP2021519832A (en) * | 2018-03-28 | 2021-08-12 | ゾルテック コーポレイション | Conductive adhesive |
| CN114074369A (en) * | 2020-08-11 | 2022-02-22 | 辽宁德尔新材料有限公司 | Production process of graphene fiber board |
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| US20020039661A1 (en) * | 2000-07-14 | 2002-04-04 | Board Of Control Of Michigan Technological University | Veneer-based product and method of manufacture |
| JP2003080510A (en) * | 2001-09-11 | 2003-03-19 | Asahi Organic Chem Ind Co Ltd | Anti-static wood composite material, its manufacturing method and its use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20020039661A1 (en) * | 2000-07-14 | 2002-04-04 | Board Of Control Of Michigan Technological University | Veneer-based product and method of manufacture |
| JP2003080510A (en) * | 2001-09-11 | 2003-03-19 | Asahi Organic Chem Ind Co Ltd | Anti-static wood composite material, its manufacturing method and its use |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104385423A (en) * | 2014-10-20 | 2015-03-04 | 贵州恒力源林业科技有限公司 | Manufacturing method of composite artificial board |
| CN105965616A (en) * | 2016-02-03 | 2016-09-28 | 宁波中加低碳新技术研究院有限公司 | Method for manufacturing single substrate composite sheet material |
| JP2021519832A (en) * | 2018-03-28 | 2021-08-12 | ゾルテック コーポレイション | Conductive adhesive |
| JP7385588B2 (en) | 2018-03-28 | 2023-11-22 | ゾルテック コーポレイション | Spar cap and its manufacturing method |
| US11834593B2 (en) | 2018-03-28 | 2023-12-05 | Zoltek Corporation | Electrically conductive adhesive |
| CN110712257A (en) * | 2019-11-01 | 2020-01-21 | 国家林业和草原局竹子研究开发中心 | Biomass charcoal-based anticorrosive, mildew-proof and environment-friendly artificial board |
| CN110712257B (en) * | 2019-11-01 | 2021-09-21 | 国家林业和草原局竹子研究开发中心 | Biomass charcoal-based anticorrosive, mildew-proof and environment-friendly artificial board |
| CN114074369A (en) * | 2020-08-11 | 2022-02-22 | 辽宁德尔新材料有限公司 | Production process of graphene fiber board |
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