CN109267344A - 一种碳纤维用上浆剂 - Google Patents
一种碳纤维用上浆剂 Download PDFInfo
- Publication number
- CN109267344A CN109267344A CN201810996723.XA CN201810996723A CN109267344A CN 109267344 A CN109267344 A CN 109267344A CN 201810996723 A CN201810996723 A CN 201810996723A CN 109267344 A CN109267344 A CN 109267344A
- Authority
- CN
- China
- Prior art keywords
- mixing
- carbon fiber
- mass ratio
- quality
- sizing agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 44
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 44
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 43
- 238000004513 sizing Methods 0.000 title claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000839 emulsion Substances 0.000 claims abstract description 34
- 239000005058 Isophorone diisocyanate Substances 0.000 claims abstract description 21
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims abstract description 15
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 14
- -1 octenyl succinate anhydride Chemical class 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 10
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000661 sodium alginate Substances 0.000 claims abstract description 9
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 9
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 9
- 239000001110 calcium chloride Substances 0.000 claims abstract description 8
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 8
- 229920002472 Starch Polymers 0.000 claims abstract description 5
- 239000008107 starch Substances 0.000 claims abstract description 5
- 235000019698 starch Nutrition 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 84
- 238000002156 mixing Methods 0.000 claims description 79
- 239000006185 dispersion Substances 0.000 claims description 46
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 42
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 239000003153 chemical reaction reagent Substances 0.000 claims description 35
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- 150000001875 compounds Chemical class 0.000 claims description 27
- 239000012530 fluid Substances 0.000 claims description 27
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 229910021389 graphene Inorganic materials 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000012752 auxiliary agent Substances 0.000 claims description 18
- 239000006210 lotion Substances 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 18
- 239000004094 surface-active agent Substances 0.000 claims description 17
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 14
- 235000010234 sodium benzoate Nutrition 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 12
- 239000003208 petroleum Substances 0.000 claims description 12
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- 239000004299 sodium benzoate Substances 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 11
- 235000019198 oils Nutrition 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- MUHFRORXWCGZGE-KTKRTIGZSA-N 2-hydroxyethyl (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCO MUHFRORXWCGZGE-KTKRTIGZSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 241000219000 Populus Species 0.000 claims description 6
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 6
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 6
- 150000004996 alkyl benzenes Chemical group 0.000 claims description 6
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229940095098 glycol oleate Drugs 0.000 claims description 6
- 235000021388 linseed oil Nutrition 0.000 claims description 6
- 239000000944 linseed oil Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 2
- 229910002567 K2S2O8 Inorganic materials 0.000 claims 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 238000003825 pressing Methods 0.000 claims 1
- 229910052938 sodium sulfate Inorganic materials 0.000 claims 1
- 235000011152 sodium sulphate Nutrition 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 16
- 239000002131 composite material Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 6
- 238000009792 diffusion process Methods 0.000 abstract description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 238000004945 emulsification Methods 0.000 abstract description 2
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract description 2
- 239000011800 void material Substances 0.000 abstract description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 238000002525 ultrasonication Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000009955 starching Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- RMGDGOMSOATWAS-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate;5-isocyanato-1-(isocyanatomethyl)-1,3,3-trimethylcyclohexane Chemical compound OCCOC(=O)C=C.CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 RMGDGOMSOATWAS-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000218195 Lauraceae Species 0.000 description 1
- 235000017858 Laurus nobilis Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 235000004443 Ricinus communis Nutrition 0.000 description 1
- 235000005212 Terminalia tomentosa Nutrition 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 239000000783 alginic acid Substances 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 239000000648 calcium alginate Substances 0.000 description 1
- 235000010410 calcium alginate Nutrition 0.000 description 1
- 229960002681 calcium alginate Drugs 0.000 description 1
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- 238000010556 emulsion polymerization method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/72—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with metaphosphoric acids or their salts; with polyphosphoric acids or their salts; with perphosphoric acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/1845—Aromatic mono- or polycarboxylic acids
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
- D06M13/2246—Esters of unsaturated carboxylic acids
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/11—Starch or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/13—Alginic acid or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
- D06M15/3562—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing nitrogen
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明涉及了一种碳纤维用上浆剂，属于碳纤维功能型乳液上浆剂领域。本发明通过丙烯酸羟乙酯与异佛尔酮二异氰酸酯反应，得到丙烯酸羟乙酯半封闭的异佛尔酮二异氰酸酯，配合聚乙烯吡咯烷酮结合，在粘接界面形成强的化学键合，大大改善了粘接强度，另一方面，可以和碳纤维材料相结合，大大结合碳纤维材料界面的粘结性及相容性；以海藻酸钠、氯化钙微微球凝胶载体，配合辛烯基琥珀酸淀粉酯、氢化蓖麻油用膜乳化法制备含自乳化微球的复合乳剂，复合乳化成分接触水后能够迅速形成微小乳滴，通过膜表面扩散和骨架空隙扩散，提高各组分的相互作用，提高本体系的界面相容性。本发明解决了目前常用的上浆剂对碳纤维材料界面的粘结性及相容性不佳的问题。
Description
技术领域
本发明属于碳纤维功能型乳液上浆剂领域，特别涉及一种碳纤维用上浆剂。
背景技术
碳纤维凭借自身优异的高比强度、高比模量，抗腐蚀耐高温等优异特性，被广泛应用于热固性与热塑性基体复合材料的增强材料。在碳纤维的生产过程中，由于工艺条件的不同，纤维表面的微观形貌存在着一定的差别，而这势必会影响纤维及其复合材料的性能。一方面，纤维表面凹槽的存在将有助于改善纤维与树脂的界面粘结状况，即有助于复合材料界面性能的提高；但另一方面，碳纤维表面凹槽的存在又可能会使碳纤维本身的性能下降，从而使复合材料的综合性能的下降。研究发现，在树脂基复合材料中存在第三相，即界面相，这一有限区域在物理性能上存在梯度，对纤维和基体树脂之间力的有效传递起主导作用，从而使纤维真正起到承载作用，影响复合材料的最终性能。但由于纤维与基体在性质上存在着很大的差异，而改变此差异的一种方法是在碳纤维与基体之间引入聚合物过渡中间层即进行上浆处理，即一方面使碳纤维粘合在一起，减少纤维之间的摩擦，减少损伤；另一方面可以对界面相起到修饰作用，使界面变得粗糙，强化力学锚定作用的影响。基体树脂容易渗透到与其组成相似的上浆层中，改善纤维对树脂基体的浸润性能，增强化学键合。在纤维的生产过程中，上浆是其中一个极为重要的环节。但由于上浆剂的存在并不能够很好的改善复合材料界面粘结性，从而使复合材料的力学性能的没有得到很大的提高。
发明内容
本发明所要解决的技术问题：针对目前常用的上浆剂对碳纤维材料界面的粘结性及相容性不佳的问题，提供一种碳纤维用上浆剂。
为解决上述技术问题，本发明采用如下所述的技术方案是：
一种碳纤维用上浆剂，按质量份数计，包括如下组分：20~40份二氯甲烷、3~7份多聚磷酸、1~4份苯甲酸钠、4~10份聚乙烯吡咯烷酮、6~10份丙酮，还包括：25~50份复合基液、12~25份复合乳剂。
所述复合基液的制备方法，包括如下步骤：
（1）于40~50℃，按质量比1：6~10取异佛尔酮二异氰酸酯、无水醋酸丁酯混合，通入氮气保护，加入异佛尔酮二异氰酸酯质量10~25%的二月桂醇二丁基锡混合，升温至60~70℃，加入异佛尔酮二异氰酸酯质量15~30%的丙烯酸羟乙酯混合，保温，得改性中间体；
（2）取氧化石墨烯按质量比1：12~20加入无水醋酸丁酯混合，超声波分散，得分散液，取分散液通氮气保护，加入氧化石墨烯质量3~7%的二月桂醇二丁基锡、氧化石墨烯质量12~20%的改性中间体混合，于75~85℃保温搅拌，冷却，过滤，取滤渣用滤渣质量3~6倍的洗液清洗，真空干燥，得改性氧化石墨烯；
（3）于40~55℃，按质量比1：1~3：0.3：20~30取OP-10、十二烷基苯磺酸钠、碳酸氢钠、水混合搅拌，得混液，升温至65~80℃，加入混液质量30~50%的改性氧化石墨烯、混液质量12~30%丙烯酸丁酯、混液质量8~15%的丙烯酸羟乙酯混合搅拌，保温，降温至55~65℃，加入混液质量10~15%的试剂A、混液质量2~5%的引发剂，保温，降温至30~45℃，调节pH，冷却，真空蒸发，即得复合基液。
所述步骤（2）中的洗液：按质量比1：12~18取石油醚、氯化钙溶液混合，即得洗液。
所述步骤（3）中的试剂A：按质量比3：1~2：12~18取K2S2O8、NaHSO3、水混合，即得试剂A。
所述步骤（3）中的引发剂：过硫酸钠、过硫酸钾、过硫酸铵中的任意一种。
所述复合乳剂的制备：于30~45℃，按质量比3：0.1：1：12~20取表面活性剂、助剂、辛烯基琥珀酸淀粉酯、油相混合搅拌，得预混液，取预混液按质量比1：15~20加入海藻酸钠溶液混合，剪切分散，得分散液，取分散液通氮气保护，加入分散液质量10~15%的试剂B混合振荡，加入分散液质量12~20%的油相混合搅拌，室温静置，即得复合乳剂。
所述表面活性剂：按质量比4：1~3取油酸聚乙二醇酯、仲烷基苯磺酸钠混合，即得表面活性剂。
所述助剂：按质量比1：2~4：8取水杨酸钠、乙酰胺、甲醇混合，即得助剂。
所述油相：按质量比1：3~6：20~30取氯化钙、亚麻油、氢化蓖麻油混合，超声处理，即得油相。
所述试剂B：按质量比8：2~5取液体石蜡、石油醚混合，即得试剂B。
本发明与其他方法相比，有益技术效果是：
（1）本发明通过丙烯酸羟乙酯与异佛尔酮二异氰酸酯反应，得到丙烯酸羟乙酯半封闭的异佛尔酮二异氰酸酯，其中未封闭的-NCO再与氧化石墨烯中的活泼氢反应，制改性中间体，接着通过核壳乳液聚合法，将改性中间体接枝于丙烯酸树脂乳液分子结构，配合聚乙烯吡咯烷酮结合，在粘接界面形成强的化学键合，大大改善了粘接强度，另一方面，可以和碳纤维材料相结合，大大结合碳纤维材料界面的粘结性及相容性；
（2）本发明以海藻酸钠、氯化钙微微球凝胶载体，配合辛烯基琥珀酸淀粉酯、氢化蓖麻油用膜乳化法制备含自乳化微球的复合乳剂，微球基质海藻酸钠中的羧酸根对pH敏感性，可在多聚磷酸的作用下溶胀，由于磷酸盐结合Ca2+的能力强，当海藻酸钙微球与磷酸盐介质接触后，表面溶胀形成凝胶层，同时凝胶开始溶蚀，微球中的多种成分则通过凝胶层的扩散和溶蚀双重机制实现释放，加强本上浆料体系对碳纤维的粘结性，另外，复合乳化成分接触水后能够迅速形成微小乳滴，微乳化微球在H+作用下在膜表面生成亲水性的海藻酸，通过膜表面扩散和骨架空隙扩散，提高各组分的相互作用，提高本体系的界面相容性。
具体实施方式
试剂A：按质量比3：1~2：12~18取K2S2O8、NaHSO3、水混合，即得试剂A；
试剂B：按质量比8：2~5取液体石蜡、石油醚混合，即得试剂B；
洗液：按质量比1：12~18取石油醚、浓度0.1mol/L的氯化钙溶液混合，即得洗液；
引发剂：过硫酸钠、过硫酸钾、过硫酸铵中的任意一种；
表面活性剂：按质量比4：1~3取油酸聚乙二醇酯、仲烷基苯磺酸钠混合，即得表面活性剂；
助剂：按质量比1：2~4：8取水杨酸钠、乙酰胺、甲醇混合，即得助剂；
油相：按质量比1：3~6：20~30取氯化钙、亚麻油、氢化蓖麻油混合，于细胞破碎仪超声处理10~15min，即得油相；
复合基液的制备方法，包括如下步骤：
（1）于水浴40~50℃，按质量比1：6~10取异佛尔酮二异氰酸酯、无水醋酸丁酯混合，通入氮气保护，以300~500r/min搅拌20~45min，加入异佛尔酮二异氰酸酯质量10~25%的二月桂醇二丁基锡混合，升温至60~70℃，加入异佛尔酮二异氰酸酯质量15~30%的丙烯酸羟乙酯混合，保温3~5h，得改性中间体；
（2）取氧化石墨烯按质量比1：12~20加入无水醋酸丁酯混合，以45~55kHz频率超声波分散40~60min，得分散液，取分散液通氮气保护，加入氧化石墨烯质量3~7%的二月桂醇二丁基锡、氧化石墨烯质量12~20%的改性中间体混合，于75~85℃保温搅拌6~8h，自然冷却至室温，过滤，取滤渣用滤渣质量3~6倍的洗液清洗后，于70~90℃真空干燥20~24h，得改性氧化石墨烯；
（3）于40~55℃，按质量比1：1~3：0.3：20~30取OP-10、十二烷基苯磺酸钠、碳酸氢钠、去离子水于反应釜混合，以400~600r/min搅拌1~3h，得混液，升温至65~80℃，加入混液质量30~50%的改性氧化石墨烯、混液质量12~30%丙烯酸丁酯、混液质量8~15%的丙烯酸羟乙酯混合搅拌，保温1~3h，降温至55~65℃，加入混液质量10~15%的试剂A、混液质量2~5%的引发剂，保温20~40min，降温至30~45℃，用浓度1mol/L的氨水调节pH至7~8，自然冷却，于60~75℃真空蒸发至原体积的25~40%，即得复合基液；
复合乳剂的制备：于30~45℃，按质量比3：0.1：1：12~20取表面活性剂、助剂、辛烯基琥珀酸淀粉酯、油相混合，以400~600r/min搅拌30~50min，得预混液，取预混液按质量比1：15~20加入浓度0.1mol/L的海藻酸钠溶液混合，以2000~3000r/min剪切分散15~30min，得分散液，取分散液通氮气保护，加入分散液质量10~15%的试剂B混合，以200~300r/min振荡20~45min后，加入分散液质量12~20%的油相混合搅拌，室温静置5~8h，即得复合乳剂；
一种碳纤维用上浆剂，按质量份数计，包括如下组分：20~40份二氯甲烷、3~7份多聚磷酸、1~4份苯甲酸钠、6~10份丙酮、25~50份复合基液、12~25份复合乳剂；
一种碳纤维用上浆剂的制备方法，包括如下步骤：
（1）按质量份数计，20~40份二氯甲烷、3~7份多聚磷酸、1~4份苯甲酸钠、4~10份聚乙烯吡咯烷酮、6~10份丙酮、25~50份复合基液、12~25份复合乳剂；
（2）于水浴20~35℃，取二氯甲烷、多聚磷酸、复合基液于反应釜混合，以400~600r/min搅拌30~50min后，加入复合乳剂、苯甲酸钠、聚乙烯吡咯烷酮、丙酮混合，升温至45~60℃，以45~55kHz频率超声波处理10~20min，即得碳纤维用上浆剂。
实施例1
试剂A：按质量比3：1：12取K2S2O8、NaHSO3、水混合，即得试剂A；
试剂B：按质量比8：2取液体石蜡、石油醚混合，即得试剂B；
洗液：按质量比1：12取石油醚、浓度0.1mol/L的氯化钙溶液混合，即得洗液；
引发剂：过硫酸钠；
表面活性剂：按质量比4：1取油酸聚乙二醇酯、仲烷基苯磺酸钠混合，即得表面活性剂；
助剂：按质量比1：2：8取水杨酸钠、乙酰胺、甲醇混合，即得助剂；
油相：按质量比1：3：20取氯化钙、亚麻油、氢化蓖麻油混合，于细胞破碎仪超声处理10min，即得油相；
复合基液的制备方法，包括如下步骤：
（1）于水浴40℃，按质量比1：6取异佛尔酮二异氰酸酯、无水醋酸丁酯混合，通入氮气保护，以300r/min搅拌20min，加入异佛尔酮二异氰酸酯质量10%的二月桂醇二丁基锡混合，升温至60℃，加入异佛尔酮二异氰酸酯质量15%的丙烯酸羟乙酯混合，保温3h，得改性中间体；
（2）取氧化石墨烯按质量比1：12加入无水醋酸丁酯混合，以45kHz频率超声波分散40min，得分散液，取分散液通氮气保护，加入氧化石墨烯质量3%的二月桂醇二丁基锡、氧化石墨烯质量12%的改性中间体混合，于75℃保温搅拌6h，自然冷却至室温，过滤，取滤渣用滤渣质量3倍的洗液清洗后，于70℃真空干燥20h，得改性氧化石墨烯；
（3）于40℃，按质量比1：1：0.3：20取OP-10、十二烷基苯磺酸钠、碳酸氢钠、去离子水于反应釜混合，以400r/min搅拌1h，得混液，升温至65℃，加入混液质量30%的改性氧化石墨烯、混液质量12%丙烯酸丁酯、混液质量8%的丙烯酸羟乙酯混合搅拌，保温1h，降温至55℃，加入混液质量10%的试剂A、混液质量2%的引发剂，保温20min，降温至30℃，用浓度1mol/L的氨水调节pH至7，自然冷却，于60℃真空蒸发至原体积的25%，即得复合基液；
复合乳剂的制备：于30℃，按质量比3：0.1：1：12取表面活性剂、助剂、辛烯基琥珀酸淀粉酯、油相混合，以400r/min搅拌30min，得预混液，取预混液按质量比1：15加入浓度0.1mol/L的海藻酸钠溶液混合，以2000r/min剪切分散15min，得分散液，取分散液通氮气保护，加入分散液质量10%的试剂B混合，以200r/min振荡20min后，加入分散液质量12%的油相混合搅拌，室温静置5h，即得复合乳剂；
一种碳纤维用上浆剂，按质量份数计，包括如下组分：20份二氯甲烷、3份多聚磷酸、1份苯甲酸钠、6份丙酮、25份复合基液、12份复合乳剂；
一种碳纤维用上浆剂的制备方法，包括如下步骤：
（1）按质量份数计，20份二氯甲烷、3份多聚磷酸、1份苯甲酸钠、4份聚乙烯吡咯烷酮、6份丙酮、25份复合基液、12份复合乳剂；
（2）于水浴20℃，取二氯甲烷、多聚磷酸、复合基液于反应釜混合，以400r/min搅拌30min后，加入复合乳剂、苯甲酸钠、聚乙烯吡咯烷酮、丙酮混合，升温至45℃，以45kHz频率超声波处理10min，即得碳纤维用上浆剂。
实施例2
试剂A：按质量比3：2：18取K2S2O8、NaHSO3、水混合，即得试剂A；
试剂B：按质量比8：5取液体石蜡、石油醚混合，即得试剂B；
洗液：按质量比1：18取石油醚、浓度0.1mol/L的氯化钙溶液混合，即得洗液；
引发剂：过硫酸钾；
表面活性剂：按质量比4：3取油酸聚乙二醇酯、仲烷基苯磺酸钠混合，即得表面活性剂；
助剂：按质量比1：4：8取水杨酸钠、乙酰胺、甲醇混合，即得助剂；
油相：按质量比1：6：30取氯化钙、亚麻油、氢化蓖麻油混合，于细胞破碎仪超声处理15min，即得油相；
复合基液的制备方法，包括如下步骤：
（1）于水浴50℃，按质量比1：10取异佛尔酮二异氰酸酯、无水醋酸丁酯混合，通入氮气保护，以500r/min搅拌45min，加入异佛尔酮二异氰酸酯质量25%的二月桂醇二丁基锡混合，升温至70℃，加入异佛尔酮二异氰酸酯质量30%的丙烯酸羟乙酯混合，保温5h，得改性中间体；
（2）取氧化石墨烯按质量比1：20加入无水醋酸丁酯混合，以55kHz频率超声波分散60min，得分散液，取分散液通氮气保护，加入氧化石墨烯质量7%的二月桂醇二丁基锡、氧化石墨烯质量20%的改性中间体混合，于85℃保温搅拌8h，自然冷却至室温，过滤，取滤渣用滤渣质量6倍的洗液清洗后，于90℃真空干燥24h，得改性氧化石墨烯；
（3）于55℃，按质量比1：3：0.3：30取OP-10、十二烷基苯磺酸钠、碳酸氢钠、去离子水于反应釜混合，以600r/min搅拌3h，得混液，升温至80℃，加入混液质量50%的改性氧化石墨烯、混液质量30%丙烯酸丁酯、混液质量15%的丙烯酸羟乙酯混合搅拌，保温3h，降温至65℃，加入混液质量15%的试剂A、混液质量5%的引发剂，保温40min，降温至45℃，用浓度1mol/L的氨水调节pH至8，自然冷却，于75℃真空蒸发至原体积的40%，即得复合基液；
复合乳剂的制备：于45℃，按质量比3：0.1：1：20取表面活性剂、助剂、辛烯基琥珀酸淀粉酯、油相混合，以600r/min搅拌50min，得预混液，取预混液按质量比1：20加入浓度0.1mol/L的海藻酸钠溶液混合，以3000r/min剪切分散30min，得分散液，取分散液通氮气保护，加入分散液质量15%的试剂B混合，以300r/min振荡45min后，加入分散液质量20%的油相混合搅拌，室温静置8h，即得复合乳剂；
一种碳纤维用上浆剂，按质量份数计，包括如下组分：40份二氯甲烷、7份多聚磷酸、4份苯甲酸钠、10份丙酮、50份复合基液、25份复合乳剂；
一种碳纤维用上浆剂的制备方法，包括如下步骤：
（1）按质量份数计，40份二氯甲烷、7份多聚磷酸、4份苯甲酸钠、10份聚乙烯吡咯烷酮、10份丙酮、50份复合基液、25份复合乳剂；
（2）于水浴35℃，取二氯甲烷、多聚磷酸、复合基液于反应釜混合，以600r/min搅拌50min后，加入复合乳剂、苯甲酸钠、聚乙烯吡咯烷酮、丙酮混合，升温至60℃，以55kHz频率超声波处理20min，即得碳纤维用上浆剂。
实施例3
试剂A：按质量比3：1.5：15取K2S2O8、NaHSO3、水混合，即得试剂A；
试剂B：按质量比8：3取液体石蜡、石油醚混合，即得试剂B；
洗液：按质量比1：15取石油醚、浓度0.1mol/L的氯化钙溶液混合，即得洗液；
引发剂：过硫酸铵；
表面活性剂：按质量比4：2取油酸聚乙二醇酯、仲烷基苯磺酸钠混合，即得表面活性剂；
助剂：按质量比1：3：8取水杨酸钠、乙酰胺、甲醇混合，即得助剂；
油相：按质量比1：5：25取氯化钙、亚麻油、氢化蓖麻油混合，于细胞破碎仪超声处理13min，即得油相；
复合基液的制备方法，包括如下步骤：
（1）于水浴45℃，按质量比1：8取异佛尔酮二异氰酸酯、无水醋酸丁酯混合，通入氮气保护，以400r/min搅拌30min，加入异佛尔酮二异氰酸酯质量20%的二月桂醇二丁基锡混合，升温至65℃，加入异佛尔酮二异氰酸酯质量25%的丙烯酸羟乙酯混合，保温4h，得改性中间体；
（2）取氧化石墨烯按质量比1：15加入无水醋酸丁酯混合，以50kHz频率超声波分散50min，得分散液，取分散液通氮气保护，加入氧化石墨烯质量4%的二月桂醇二丁基锡、氧化石墨烯质量15%的改性中间体混合，于80℃保温搅拌7h，自然冷却至室温，过滤，取滤渣用滤渣质量5倍的洗液清洗后，于80℃真空干燥22h，得改性氧化石墨烯；
（3）于45℃，按质量比1：2：0.3：25取OP-10、十二烷基苯磺酸钠、碳酸氢钠、去离子水于反应釜混合，以500r/min搅拌2h，得混液，升温至70℃，加入混液质量40%的改性氧化石墨烯、混液质量25%丙烯酸丁酯、混液质量13%的丙烯酸羟乙酯混合搅拌，保温2h，降温至60℃，加入混液质量13%的试剂A、混液质量3%的引发剂，保温30min，降温至40℃，用浓度1mol/L的氨水调节pH至7.5，自然冷却，于70℃真空蒸发至原体积的35%，即得复合基液；
复合乳剂的制备：于35℃，按质量比3：0.1：1：17取表面活性剂、助剂、辛烯基琥珀酸淀粉酯、油相混合，以500r/min搅拌40min，得预混液，取预混液按质量比1：17加入浓度0.1mol/L的海藻酸钠溶液混合，以2500r/min剪切分散20min，得分散液，取分散液通氮气保护，加入分散液质量13%的试剂B混合，以250r/min振荡35min后，加入分散液质量17%的油相混合搅拌，室温静置7h，即得复合乳剂；
一种碳纤维用上浆剂，按质量份数计，包括如下组分：25份二氯甲烷、5份多聚磷酸、3份苯甲酸钠、8份丙酮、30份复合基液、22份复合乳剂；
一种碳纤维用上浆剂的制备方法，包括如下步骤：
（1）按质量份数计，30份二氯甲烷、4份多聚磷酸、3份苯甲酸钠、6份聚乙烯吡咯烷酮、8份丙酮、35份复合基液、21份复合乳剂；
（2）于水浴29℃，取二氯甲烷、多聚磷酸、复合基液于反应釜混合，以500r/min搅拌40min后，加入复合乳剂、苯甲酸钠、聚乙烯吡咯烷酮、丙酮混合，升温至50℃，以50kHz频率超声波处理15min，即得碳纤维用上浆剂。
对比例1：与实施例1的制备方法基本相同，唯有不同的是缺少复合基液。
对比例2：与实施例1的制备方法基本相同，唯有不同的是缺少复合乳剂。
对比例3：青岛市某公司生产的碳纤维用上浆剂。
将上述实施例与对比例得到的上浆剂进行检测，先测定未涂抹上浆剂的碳纤维层间剪切强度为80.9GPa，利用浸渍法将上浆剂涂布在表面处理过的碳纤维上，然后于210℃下热处理90s，得到上浆剂涂布碳纤维束。调节上浆剂的附着量，使其相对于表面处理过的碳纤维100 质量份为1质量份。接下来，使用得到的上浆剂涂布碳纤维，再次测定层间剪切强度(ILSS)，I型层间断裂韧性(GIc)，得到的结果如表1所示。
表1：
综合上述，从表1可以看出本发明的碳纤维用上浆剂对碳纤维材料界面的粘结性及相容性更好，值得推广使用。
Claims (10)
1.一种碳纤维用上浆剂，按质量份数计，包括如下组分：20~40份二氯甲烷、3~7份多聚磷酸、1~4份苯甲酸钠、4~10份聚乙烯吡咯烷酮、6~10份丙酮，其特征在于，还包括：25~50份复合基液、12~25份复合乳剂。
2.根据权利要求1所述一种碳纤维用上浆剂，其特征在于，所述复合基液的制备方法，包括如下步骤：
（1）于40~50℃，按质量比1：6~10取异佛尔酮二异氰酸酯、无水醋酸丁酯混合，通入氮气保护，加入异佛尔酮二异氰酸酯质量10~25%的二月桂醇二丁基锡混合，升温至60~70℃，加入异佛尔酮二异氰酸酯质量15~30%的丙烯酸羟乙酯混合，保温，得改性中间体；
（2）取氧化石墨烯按质量比1：12~20加入无水醋酸丁酯混合，超声波分散，得分散液，取分散液通氮气保护，加入氧化石墨烯质量3~7%的二月桂醇二丁基锡、氧化石墨烯质量12~20%的改性中间体混合，于75~85℃保温搅拌，冷却，过滤，取滤渣用滤渣质量3~6倍的洗液清洗，真空干燥，得改性氧化石墨烯；
（3）于40~55℃，按质量比1：1~3：0.3：20~30取OP-10、十二烷基苯磺酸钠、碳酸氢钠、水混合搅拌，得混液，升温至65~80℃，加入混液质量30~50%的改性氧化石墨烯、混液质量12~30%丙烯酸丁酯、混液质量8~15%的丙烯酸羟乙酯混合搅拌，保温，降温至55~65℃，加入混液质量10~15%的试剂A、混液质量2~5%的引发剂，保温，降温至30~45℃，调节pH，冷却，真空蒸发，即得复合基液。
3.根据权利要求2所述一种碳纤维用上浆剂，其特征在于，所述步骤（2）中的洗液：按质量比1：12~18取石油醚、氯化钙溶液混合，即得洗液。
4.根据权利要求2所述一种碳纤维用上浆剂，其特征在于，所述步骤（3）中的试剂A：按质量比3：1~2：12~18取K2S2O8、NaHSO3、水混合，即得试剂A。
5.根据权利要求2所述一种碳纤维用上浆剂，其特征在于，所述步骤（3）中的引发剂：过硫酸钠、过硫酸钾、过硫酸铵中的任意一种。
6.根据权利要求1所述一种碳纤维用上浆剂，其特征在于，所述复合乳剂的制备：于30~45℃，按质量比3：0.1：1：12~20取表面活性剂、助剂、辛烯基琥珀酸淀粉酯、油相混合搅拌，得预混液，取预混液按质量比1：15~20加入海藻酸钠溶液混合，剪切分散，得分散液，取分散液通氮气保护，加入分散液质量10~15%的试剂B混合振荡，加入分散液质量12~20%的油相混合搅拌，室温静置，即得复合乳剂。
7.根据权利要求6所述一种碳纤维用上浆剂，其特征在于，所述表面活性剂：按质量比4：1~3取油酸聚乙二醇酯、仲烷基苯磺酸钠混合，即得表面活性剂。
8.根据权利要求6所述一种碳纤维用上浆剂，其特征在于，所述助剂：按质量比1：2~4：8取水杨酸钠、乙酰胺、甲醇混合，即得助剂。
9.根据权利要求6所述一种碳纤维用上浆剂，其特征在于，所述油相：按质量比1：3~6：20~30取氯化钙、亚麻油、氢化蓖麻油混合，超声处理，即得油相。
10.根据权利要求6所述一种碳纤维用上浆剂，其特征在于，所述试剂B：按质量比8：2~5取液体石蜡、石油醚混合，即得试剂B。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810996723.XA CN109267344A (zh) | 2018-08-29 | 2018-08-29 | 一种碳纤维用上浆剂 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810996723.XA CN109267344A (zh) | 2018-08-29 | 2018-08-29 | 一种碳纤维用上浆剂 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109267344A true CN109267344A (zh) | 2019-01-25 |
Family
ID=65154719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810996723.XA Pending CN109267344A (zh) | 2018-08-29 | 2018-08-29 | 一种碳纤维用上浆剂 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109267344A (zh) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213751A (zh) * | 2021-12-09 | 2022-03-22 | 福建师范大学泉港石化研究院 | 一种碳纤维增强聚丙烯复合材料及其制备方法 |
| CN114806127A (zh) * | 2022-05-10 | 2022-07-29 | 中山市卡邦碳纤维材料制品有限公司 | 一种碳纤维管材及其制造工艺 |
| CN117580994A (zh) * | 2021-07-14 | 2024-02-20 | 竹本油脂株式会社 | 无机纤维用上浆剂、无机纤维、其制造方法以及复合材料 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744285A (zh) * | 2010-02-22 | 2010-06-23 | 江南大学 | 一种乳化胶凝型功能性脂肪酸载体的制备方法 |
| CN103467676A (zh) * | 2013-08-05 | 2013-12-25 | 江苏大学 | 一种水性氧化石墨烯改性聚（氨酯-丙烯酸酯）复合材料的制备方法 |
| CN104975508A (zh) * | 2015-07-30 | 2015-10-14 | 北京化工大学常州先进材料研究院 | 一种水溶性碳纤维上浆剂的制备方法和用途 |
-
2018
- 2018-08-29 CN CN201810996723.XA patent/CN109267344A/zh active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744285A (zh) * | 2010-02-22 | 2010-06-23 | 江南大学 | 一种乳化胶凝型功能性脂肪酸载体的制备方法 |
| CN103467676A (zh) * | 2013-08-05 | 2013-12-25 | 江苏大学 | 一种水性氧化石墨烯改性聚（氨酯-丙烯酸酯）复合材料的制备方法 |
| CN104975508A (zh) * | 2015-07-30 | 2015-10-14 | 北京化工大学常州先进材料研究院 | 一种水溶性碳纤维上浆剂的制备方法和用途 |
Non-Patent Citations (3)
| Title |
|---|
| 裘炳毅: "《现代化妆品科学与技术 中册》", 31 March 2016, 中国轻工业出版社 * |
| 金永学: "氧化石墨烯改性壳核丙烯酸乳液的合成及其表征", 《广州化工》 * |
| 马世昌: "《化学物质词典》", 30 April 1999, 陕西科学技术出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117580994A (zh) * | 2021-07-14 | 2024-02-20 | 竹本油脂株式会社 | 无机纤维用上浆剂、无机纤维、其制造方法以及复合材料 |
| CN114213751A (zh) * | 2021-12-09 | 2022-03-22 | 福建师范大学泉港石化研究院 | 一种碳纤维增强聚丙烯复合材料及其制备方法 |
| CN114806127A (zh) * | 2022-05-10 | 2022-07-29 | 中山市卡邦碳纤维材料制品有限公司 | 一种碳纤维管材及其制造工艺 |
| CN114806127B (zh) * | 2022-05-10 | 2024-02-20 | 中山市卡邦碳纤维材料制品有限公司 | 一种碳纤维管材及其制造方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109267344A (zh) | 一种碳纤维用上浆剂 | |
| CN104389176B (zh) | 一种含有氧化石墨烯的乳液型碳纤维上浆剂及其制备方法 | |
| CN103289010B (zh) | 核壳型纳米SiO2/含氟聚丙烯酸酯无皂乳液的制备方法 | |
| CN103709971B (zh) | 一种双组份拼板胶用乳液及其合成方法 | |
| Kawaguchi et al. | The effect of particle–matrix adhesion on the mechanical behavior of glass filled epoxies: Part 1. A study on yield behavior and cohesive strength | |
| CN106478895A (zh) | 一种氧化石墨烯复合型聚羧酸减水剂及其制备方法 | |
| TW201020243A (en) | Episulfide, mixture containing episulfide, method for producing mixture containing episulfide, curable composition and connection structure | |
| CN105131868B (zh) | 复合防火玻璃的防火液及其制备方法及复合防火玻璃 | |
| TW200846398A (en) | Prepreg, multilayer printed wiring board and electronic parts using same | |
| CN101457499B (zh) | 一种表面施胶剂及其制备方法 | |
| CN107558182A (zh) | 一种改性聚丙烯复合纤维及其制备方法 | |
| CN105647502A (zh) | 一种稠油降粘剂及其制备方法 | |
| CN108034258A (zh) | 一种高阻隔硅橡胶石墨烯复合材料及其制备方法 | |
| Zhou et al. | Mechanical and thermal properties of novel rubber‐toughened epoxy blend prepared by in situ pre‐crosslinking | |
| CN103554909B (zh) | 聚合物-二氧化硅包覆的碳纳米管复合材料、其制备方法、半固化片及覆铜基板 | |
| US4482659A (en) | Toughened thermosetting compositions for composites | |
| CN108504041A (zh) | 一种环氧树脂/聚离子液体复合材料及其制备方法 | |
| CN101941956A (zh) | 一种具有碳碳双键的缩水甘油醚酯、合成方法及其用途 | |
| DE60032624T2 (de) | Bei variablen temperaturen härtbare zusammensetzung | |
| CN107867684B (zh) | 一种氟化氧化石墨烯的制备方法 | |
| CN106283641A (zh) | 一种纤维素纤维的改性方法、改性纤维素纤维及其应用 | |
| CN109280522A (zh) | 耐高温环氧密封胶 | |
| Hou et al. | Processing and properties of IM7/LARCTM-RP46 polyimide composites | |
| CN108547149A (zh) | 一种纺丝油剂用抗静电剂的制备方法 | |
| CN105085933B (zh) | 一种木质素磺酸钠烷基化合成表面活性剂的方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190125 |
|
| WD01 | Invention patent application deemed withdrawn after publication |