CN104194607B - The preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive - Google Patents
The preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive Download PDFInfo
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- CN104194607B CN104194607B CN201410402204.8A CN201410402204A CN104194607B CN 104194607 B CN104194607 B CN 104194607B CN 201410402204 A CN201410402204 A CN 201410402204A CN 104194607 B CN104194607 B CN 104194607B
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 53
- 239000000853 adhesive Substances 0.000 title claims abstract description 32
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 32
- 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 title claims abstract description 26
- 239000011527 polyurethane coating Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000004078 waterproofing Methods 0.000 title claims abstract description 26
- 229910003472 fullerene Inorganic materials 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 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 claims abstract description 40
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 230000035484 reaction time Effects 0.000 claims abstract description 24
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 23
- BJZYYSAMLOBSDY-QMMMGPOBSA-N (2s)-2-butoxybutan-1-ol Chemical compound CCCCO[C@@H](CC)CO BJZYYSAMLOBSDY-QMMMGPOBSA-N 0.000 claims abstract description 17
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005058 Isophorone diisocyanate Substances 0.000 claims abstract description 15
- 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 15
- FDYMERLIFOUIRZ-UHFFFAOYSA-N (3-chloro-4-methyl-2-oxochromen-7-yl) diethyl phosphate Chemical compound CC1=C(Cl)C(=O)OC2=CC(OP(=O)(OCC)OCC)=CC=C21 FDYMERLIFOUIRZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- ROQRAMYLVSOQHK-UHFFFAOYSA-N C(CC)N.[Br] Chemical compound C(CC)N.[Br] ROQRAMYLVSOQHK-UHFFFAOYSA-N 0.000 claims abstract description 12
- AUNGANRZJHBGPY-UHFFFAOYSA-N D-Lyxoflavin Natural products OCC(O)C(O)C(O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-UHFFFAOYSA-N 0.000 claims abstract description 12
- AUNGANRZJHBGPY-SCRDCRAPSA-N Riboflavin Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-SCRDCRAPSA-N 0.000 claims abstract description 12
- FCASKLHVRFDIJB-UHFFFAOYSA-N Riboflavine Natural products Cc1cc2N=C3C(NC(=O)NC3=O)N(CC(O)C(O)C(O)CO)c2cc1C FCASKLHVRFDIJB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 108090000765 processed proteins & peptides Proteins 0.000 claims abstract description 12
- 239000002151 riboflavin Substances 0.000 claims abstract description 12
- 229960002477 riboflavin Drugs 0.000 claims abstract description 12
- 235000019192 riboflavin Nutrition 0.000 claims abstract description 12
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 12
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 12
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 12
- GUEIZVNYDFNHJU-UHFFFAOYSA-N quinizarin Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C(O)=CC=C2O GUEIZVNYDFNHJU-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004970 Chain extender Substances 0.000 claims abstract description 8
- 238000004945 emulsification Methods 0.000 claims abstract description 8
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 8
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- 239000012153 distilled water Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 17
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- -1 fullerene triethanolamine derivative Chemical class 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- VZPHSJLSYGMBGE-UHFFFAOYSA-N C(=O)(O)C1=CC=C(C=C1)P(C1=CC=CC=C1)=O Chemical compound C(=O)(O)C1=CC=C(C=C1)P(C1=CC=CC=C1)=O VZPHSJLSYGMBGE-UHFFFAOYSA-N 0.000 claims description 8
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 8
- LGLOITKZTDVGOE-UHFFFAOYSA-N boranylidynemolybdenum Chemical compound [Mo]#B LGLOITKZTDVGOE-UHFFFAOYSA-N 0.000 claims description 8
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- QLBHNVFOQLIYTH-UHFFFAOYSA-L dipotassium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [K+].[K+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O QLBHNVFOQLIYTH-UHFFFAOYSA-L 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- 238000010025 steaming Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- GAXOIPNLNXSFNG-UHFFFAOYSA-N [Sb]=O.[Ti].[Cr] Chemical compound [Sb]=O.[Ti].[Cr] GAXOIPNLNXSFNG-UHFFFAOYSA-N 0.000 claims description 6
- FKOKUHFZNIUSLW-UHFFFAOYSA-N 2-Hydroxypropyl stearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(C)O FKOKUHFZNIUSLW-UHFFFAOYSA-N 0.000 claims description 3
- QZXSMBBFBXPQHI-UHFFFAOYSA-N N-(dodecanoyl)ethanolamine Chemical compound CCCCCCCCCCCC(=O)NCCO QZXSMBBFBXPQHI-UHFFFAOYSA-N 0.000 claims description 3
- UKMSUNONTOPOIO-UHFFFAOYSA-M behenate Chemical compound CCCCCCCCCCCCCCCCCCCCCC([O-])=O UKMSUNONTOPOIO-UHFFFAOYSA-M 0.000 claims description 3
- 229940116224 behenate Drugs 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 claims description 3
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical compound CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims description 2
- AHKDJQYHVWSRLT-UHFFFAOYSA-N anthragallol Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=C(O)C(O)=C2O AHKDJQYHVWSRLT-UHFFFAOYSA-N 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 abstract description 9
- 239000004814 polyurethane Substances 0.000 abstract description 9
- 239000010985 leather Substances 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 238000009941 weaving Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000000576 coating method Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- AHLWZBVXSWOPPL-RGYGYFBISA-N 20-deoxy-20-oxophorbol 12-myristate 13-acetate Chemical compound C([C@]1(O)C(=O)C(C)=C[C@H]1[C@@]1(O)[C@H](C)[C@H]2OC(=O)CCCCCCCCCCCCC)C(C=O)=C[C@H]1[C@H]1[C@]2(OC(C)=O)C1(C)C AHLWZBVXSWOPPL-RGYGYFBISA-N 0.000 description 6
- 241001602688 Pama Species 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 230000000630 rising effect Effects 0.000 description 6
- 239000000779 smoke Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- IRZTUXPRIUZXMP-UHFFFAOYSA-N rubiadin Chemical group C1=CC=C2C(=O)C3=C(O)C(C)=C(O)C=C3C(=O)C2=C1 IRZTUXPRIUZXMP-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N perisophthalic acid Natural products OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- NHZLNPMOSADWGC-UHFFFAOYSA-N 4-amino-N-(2-quinoxalinyl)benzenesulfonamide Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=CN=C(C=CC=C2)C2=N1 NHZLNPMOSADWGC-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- JZUFKLXOESDKRF-UHFFFAOYSA-N Chlorothiazide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC2=C1NCNS2(=O)=O JZUFKLXOESDKRF-UHFFFAOYSA-N 0.000 description 1
- 241000127225 Enceliopsis nudicaulis Species 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229960002155 chlorothiazide Drugs 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229940016409 methylsulfonylmethane Drugs 0.000 description 1
- 229960001156 mitoxantrone Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006264 polyurethane film Polymers 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229960003097 sulfaquinoxaline Drugs 0.000 description 1
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 1
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Paints Or Removers (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polyurethanes Or Polyureas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses preparation method fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive, under the condition existing in made fullerene catalyst, PTMG is mixed with IPDI, at 60 ~ 85 DEG C, react 1 ~ 2h, add coroxon and bromine propylamine peptide woods, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A, to base polyurethane prepolymer for use as, A adds chain extender, butanone and Riboflavine sodium phosphate, under 60 ~ 85 DEG C of conditions, react 2.5 ~ 3.5h, add fire retardant, 75 ~ 85 DEG C of reaction temperatures, reaction time 1 ~ 2h, add again 1, 4-dihydroxy anthraquinone, polyacrylamide and tackifier, 75 DEG C of reaction temperatures, reaction time 1 ~ 2h, add again triethylamine to carry out neutralization reaction 30 ~ 50min, add water emulsification 30min, obtain fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive, prepared having is fire-retardant, fast light, the triple capabilities of waterproof, and polyurethane environmental protection, cheap, be widely used in body of wall, furniture, ironware surface, as plastics, glass, papermaking, weaving, the adhesive of leather.
Description
Technical fieldThe present invention relates to the preparation method of anti-flaming dope and adhesive, particularly the preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive.
Background technology
Polyurethane is mainly used in the aspects such as leather finish, textile printing and dyeing, paper-making industry, building coating, adhesive, be sprayed at coating and the paint on external and internal wall, furniture, ironware surface, all the time all directly or indirectly contacting with the mankind, poisonous, harmful coating is the moment health that threatening people also. Because the field using often contacts sunshine, owing to containing a large amount of ultraviolet lights harmful to coloured object in sunray, approximately 290～460nm of its wavelength, these harmful ultraviolet lights, by redox chemically, make the variation of coating generation color.
Waterproof material main application fields comprises the roofing of building construction, underground, exterior wall and indoor; The municipal works such as urban road bridges and the underground space; The bridge of highway and high-speed railway, tunnel; The traffic engineering such as underground railway; The hydraulic engineerings such as flume, reservoir, dam body, natural flow station and water treatment, be applicable to roofing and lavatory bathe between, the waterproof of basement, cistern, metope, antiseepage, protection against the tide. Divide and can be used for the fields such as papermaking, weaving, leather according to application material.
Polyurethane carries out polymerization and often adopts dibutyl tin laurate to make catalyst, but because Heavy Metal, Sn works the mischief to environment along with the degraded of polyurethane. Utilize fullerene that organotin is carried out and is fixed, reduce the harm of polyurethane coating residue to environment.
The normal employing of polyurethane light resistance adds ultra-violet absorber and antioxidant to improve light resistance, but traditional synthetized oxidation preventive agent has butylhydroxy anisole, t-butyl hydroperoxide, TBHQ etc., there is larger toxic and side effect and carcinogenicity, therefore need to find high-efficiency environment friendly, fast light technology.
Along with improving constantly of living standards of the people, safety has become the focus of growing interest, and fire is the important hidden danger of life threatening, property safety, therefore, the daily material used of the people becomes the focus of research as polyurethane, acrylic resin and other flame retardant of plastic.
Summary of the invention
Technical problem to be solved by this invention is, preparation method fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive is provided, select through 4-amino-2, the fullerene of 6-dibromophenol stannic chloride hydrochloride modification is made catalyst, PTMG reacts with IPDI, utilize coroxon and bromine propylamine peptide woods to be fixed fullerene, with light resistance material as chain extender, by Riboflavine sodium phosphate raising chain extension efficiency, with fire retardant to polyurethane-modified, 1, 4-dihydroxy anthraquinone is made waterproof material, select tackifier to improve the viscosity of polyurethane, make fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive.
The preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive, is characterized in that:
(1), the preparation of fullerene catalyst: take 40mg fullerene in there-necked flask, add 20g triethanolamine and ethanol 12g, 70 DEG C of reaction 8h of oil bath under nitrogen protection, the excessive triethanolamine of pressure reducing and steaming and ethanol, the brown sticky matter of gained dissolves with the vibration of 10ml distilled water, add again 50ml acetone, there are a large amount of brown flocculent deposits to separate out, centrifugal, sediment acetone washed twice, vacuum drying, obtains the fullerene triethanolamine derivative of 140mg brown ceramic powder shape; Again 140mg fullerene triethanolamine derivative is dissolved in to 20ml distilled water, pour 30ml into and be dissolved with 4-amino-2, in the aqueous solution of 6-dibromophenol stannic chloride hydrochloride 200mg, be heated to 90 DEG C, have brown precipitation to produce, after insulation 30min, centrifugal while hot, distilled water washing 4 times for solids, vacuum drying, obtain brown solid, be prepared fullerene catalyst.
(2), fire retardant preparation: the aqueous solution of nitric acid dissolved oxygen antimony chromium titanium 2g and the molybdenum boride 2.5g that are 0.1mol/L by 30ml concentration, rising temperature 50 C, add two (4-carboxyl phenyl) phenyl phosphine oxide 1.25g, adjusting mixed solution pH is 4, reaction 1h, 50 DEG C add EDTAP dipotassium ethylene diamine tetraacetate 2.5g, and fully stirring reaction 2h, obtains fire retardant;
(3), under the condition existing in the made fullerene catalyst of step (1), PTMG is mixed by weight 2:1 ~ 5:1 with IPDI, at 60 ~ 85 DEG C, react 1 ~ 2h, add coroxon and bromine propylamine peptide woods, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A, described fullerene catalyst consumption is 0.3 ~ 0.6% of PTMG and IPDI gross weight, coroxon consumption is PTMG, 0.2 ~ 0.4% of IPDI and fullerene catalyst gross weight, bromine propylamine peptide woods is PTMG, 0.2 ~ 0.8% of IPDI and fullerene catalyst gross weight,
(4), add the chain extender of base polyurethane prepolymer for use as A weight 1.8 ~ 3.6% and butanone and the Riboflavine sodium phosphate of base polyurethane prepolymer for use as A weight 13 ~ 26% to base polyurethane prepolymer for use as A, under 60 ~ 85 DEG C of conditions, react 2.5 ~ 3.5h, add the prepared fire retardant of step (2), 75 ~ 85 DEG C of reaction temperatures, reaction time 1 ~ 2h, add again 1, 4-dihydroxy anthraquinone, polyacrylamide and tackifier, 75 DEG C of reaction temperatures, reaction time 1 ~ 2h, add again the triethylamine that base polyurethane prepolymer for use as A weight is 10 ~ 15% and carry out neutralization reaction 30 ~ 50min, add water emulsification 30min, obtain fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive, Riboflavine sodium phosphate, fire retardant, 1, 4-dihydroxy anthraquinone, polyacrylamide, tackifier are respectively 5 ~ 8% of base polyurethane prepolymer for use as A weight, 3 ~ 7%, 3 ~ 5%, 1 ~ 2%, 2 ~ 4%.
The molecular weight of PTMG is 2000; Chain extender is 1,3-dihydroxy-2-methylanthraquinone, 1,3,6-trihydroxy-2-methyl-9,10-anthraquinone-3-O-(6-O-acetyl group)-β-D-Glucose, 2-methyl isophthalic acid, 3, any one in 6-trihydroxyanthraquinone, Isosorbide-5-Nitrae-dihydroxy-6-tectoquinone; Polyacrylamide is anionic; Tackifier are any one of coconut monoethanol amide, Ji Wusi behenate, propylene glycol stearate, different stearic aminopropyl amine oxide, Sodium Polyacrylate.
The present invention has following characteristics:
(1) coroxon and bromine propylamine peptide woods are fixed catalyst, have reduced polyurethane due to the toxicity difficult problem that Heavy Metal, Sn causes, improve the levelability of polyurethane film simultaneously;
(2) triethanolamine and ethanol carry out modification to fullerene, then organotin are carried out to modification with the fullerene of modification, and prepared catalyst efficiency is high, low to the toxicity of environment;
(3) two (4-carboxyl phenyl) phenyl phosphine oxides of the existing one-tenth charcoal of prepared fire retardant, also have the molybdenum boride that presses down cigarette, also have the antimony oxide chromium titanium of synergistic;
(4) selecting fast light material is chain extender, has improved fast light efficiency, and the fast light material environment friendly of selecting;
(5) improve the efficiency of chain extender with Riboflavine sodium phosphate;
(6) Isosorbide-5-Nitrae-dihydroxy anthraquinone is made waterproof material;
(7) select tackifier, PAMA to improve the viscosity of polyurethane.
Detailed description of the inventionFurther illustrate the present invention below in conjunction with example.
Example one
(1), the preparation of fullerene catalyst: take 40mg fullerene in 250ml there-necked flask, add 20g triethanolamine and ethanol 12g, 70 DEG C of stirring reaction 8h of oil bath under nitrogen protection, the excessive triethanolamine of pressure reducing and steaming and ethanol, the brown sticky matter of gained dissolves with the vibration of 10ml distilled water, add again 50ml acetone, there are a large amount of brown flocculent deposits to separate out, centrifugal, sediment acetone washed twice, vacuum drying, obtains the fullerene triethanolamine derivative of 140mg brown ceramic powder shape; Above-mentioned 140mg fullerene triethanolamine derivative is dissolved in to 20ml distilled water, pour 30ml into and be dissolved with 200mg4-amino-2, in the aqueous solution of 6-dibromophenol stannic chloride hydrochloride, be heated to 90 DEG C, have brown precipitation to produce, after insulation 30min, centrifugal while hot, distilled water washing 4 times for solids, vacuum drying, obtain brown solid, be prepared fullerene catalyst;
(2), fire retardant preparation: the aqueous solution of nitric acid that is 0.1mol/L by 30ml concentration, antimony oxide chromium titanium 2g, molybdenum boride 2.5g join in 50ml there-necked flask, rising temperature 50 C, add two (4-carboxyl phenyl) phenyl phosphine oxide 1.25g, adjusting mixed solution pH is 4, stirring reaction 1h, 50 DEG C add EDTAP dipotassium ethylene diamine tetraacetate 2.5g, and fully stirring reaction 2h, obtains fire retardant;
(3), in the 500ml there-necked flask with thermometer, agitator, add PTMG 40g, IPDI 20g and the prepared fullerene catalyst 0.18g of step (1), at 60 DEG C, react 1h, add coroxon 0.12g and bromine propylamine peptide woods 0.12g, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A60.1g;
(4), to add in performed polymer A 1,3-dihydroxy-2-methylanthraquinone 1.1g, butanone 7.8g and Riboflavine sodium phosphate 3g, under 60 DEG C of conditions, react 2.5h, add the prepared fire retardant 1.8g of step (2), 75 DEG C of reaction temperatures, reaction time 1h, add again 1,4-dihydroxy anthraquinone 1.8g, PAMA 0.6g and coconut monoethanol amide 1.2g, 75 DEG C of reaction temperatures, reaction time 1h, then add triethylamine 6g to carry out neutralization reaction 30min, the 120g emulsification 30min that adds water, obtains fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive.
Example two
(1), the preparation of fullerene catalyst: take 40mg fullerene in 250ml there-necked flask, add 20g triethanolamine and ethanol 12g, 70 DEG C of stirring reaction 8h of oil bath under nitrogen protection, the excessive triethanolamine of pressure reducing and steaming and ethanol, the brown sticky matter of gained dissolves with the vibration of 10ml distilled water, add again 50ml acetone, there are a large amount of brown flocculent deposits to separate out, centrifugal, sediment acetone washed twice, vacuum drying, obtains the fullerene triethanolamine derivative of 140mg brown ceramic powder shape; Above-mentioned 140mg fullerene triethanolamine derivative is dissolved in to 20ml distilled water, pour 30ml into and be dissolved with 4-amino-2, in the aqueous solution of 6-dibromophenol stannic chloride hydrochloride 200mg, be heated to 90 DEG C, have brown precipitation to produce, after insulation 30min, centrifugal while hot, distilled water washing 4 times for solids, vacuum drying, obtain brown solid, be prepared fullerene catalyst;
(2), fire retardant preparation: the aqueous solution of nitric acid that is 0.1mol/L by 30ml concentration, antimony oxide chromium titanium 2g and molybdenum boride 2.5g join in 50ml there-necked flask, rising temperature 50 C, add two (4-carboxyl phenyl) phenyl phosphine oxide 1.25g, adjusting mixed solution pH is 4, stirring reaction 1h, 50 DEG C add EDTAP dipotassium ethylene diamine tetraacetate 2.5g, and fully stirring reaction 2h, obtains fire retardant;
(3), in the 500ml there-necked flask with thermometer, agitator, add PTMG 75g, IPDI 15g and the prepared fullerene catalyst 0.54g of step (1), at 85 DEG C, react 2h, add coroxon 0.36g and bromine propylamine peptide woods 0.72g, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A91g;
(4), to base polyurethane prepolymer for use as, A adds 1, 3, 6-trihydroxy-2-methyl-9, 10-anthraquinone-3-O-(6-O-acetyl group)-β-D-Glucose 3.3g, butanone 23.7g and Riboflavine sodium phosphate 7.3g, under 85 DEG C of conditions, react 3.5h, add the prepared fire retardant 6.4g of step (2), 85 DEG C of reaction temperatures, reaction time 2h, add again 1, 4-dihydroxy anthraquinone 4.6g, PAMA 1.8g and seasons penta 4 behenate 3.6g, 75 DEG C of reaction temperatures, reaction time 2h, add again triethylamine 13.7g to carry out neutralization reaction 50min, 130g emulsification 30min adds water, obtain fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive.
Example three
(1), the preparation of fullerene catalyst: take 40mg fullerene in 250ml there-necked flask, add 20g triethanolamine and ethanol 12g, 70 DEG C of stirring reaction 8h of oil bath under nitrogen protection, the excessive triethanolamine of pressure reducing and steaming and ethanol, the brown sticky matter of gained dissolves with the vibration of 10ml distilled water, add again 50ml acetone, there are a large amount of brown flocculent deposits to separate out, centrifugal, sediment acetone washed twice, vacuum drying, obtains the fullerene triethanolamine derivative of 140mg brown ceramic powder shape; Above-mentioned 140mg fullerene triethanolamine derivative is dissolved in to 20ml distilled water, pour 30ml into and be dissolved with 4-amino-2, in the aqueous solution of 6-dibromophenol stannic chloride hydrochloride 200mg, be heated to 90 DEG C, have brown precipitation to produce, after insulation 30min, centrifugal while hot, distilled water washing 4 times for solids, vacuum drying, obtain brown solid, be prepared fullerene catalyst;
(2), fire retardant preparation: the aqueous solution of nitric acid that is 0.1mol/L by 30ml concentration, antimony oxide chromium titanium 2g and molybdenum boride 2.5g join in 50ml there-necked flask, rising temperature 50 C, add two (4-carboxyl phenyl) phenyl phosphine oxide 1.25g, adjusting mixed solution pH is 4, stirring reaction 1h, 50 DEG C add EDTAP dipotassium ethylene diamine tetraacetate 2.5g, and fully stirring reaction 2h, obtains fire retardant;
(3), in the 500ml there-necked flask with thermometer, agitator, add PTMG 75g, IPDI 30g and the made fullerene catalyst 0.47g of step (1), at 75 DEG C, react 1.5h, add coroxon 0.32g and bromine propylamine peptide woods 0.53g, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A106g;
(4), to base polyurethane prepolymer for use as A2-methyl isophthalic acid, 3, 6-trihydroxyanthraquinone 2.9g, butanone 20.7g and Riboflavine sodium phosphate 6.9g, under 75 DEG C of conditions, react 3h, add the prepared fire retardant 5.3g of step (2), 80 DEG C of reaction temperatures, reaction time 1.5h, add again 1, 4-dihydroxy anthraquinone 4.2g, PAMA 1.6g and propylene glycol stearate 3.2g, 75 DEG C of reaction temperatures, reaction time 1.5h, add again triethylamine 13.3g to carry out neutralization reaction 40min, 130g emulsification 30min adds water, obtain fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive.
Example four
(1), the preparation of fullerene catalyst: take 40mg fullerene in 250ml there-necked flask, add 20g triethanolamine and ethanol 12g, 70 DEG C of stirring reaction 8h of oil bath under nitrogen protection, the excessive triethanolamine of pressure reducing and steaming and ethanol, the brown sticky matter of gained dissolves with the vibration of 10ml distilled water, add again 50ml acetone, there are a large amount of brown flocculent deposits to separate out, centrifugal, sediment acetone washed twice, vacuum drying, obtains the fullerene triethanolamine derivative of 140mg brown ceramic powder shape; Above-mentioned 140mg fullerene triethanolamine derivative is dissolved in to 20ml distilled water, pour 30ml into and be dissolved with 4-amino-2, in the aqueous solution of 6-dibromophenol stannic chloride hydrochloride 200mg, be heated to 90 DEG C, have brown precipitation to produce, after insulation 30min, centrifugal while hot, distilled water washing 4 times for solids, vacuum drying, obtain brown solid, be prepared fullerene catalyst;
(2), fire retardant preparation: the aqueous solution of nitric acid that is 0.1mol/L by 30ml concentration, mercaptan antimony 2g, molybdenum boride 2.5g join in 50ml there-necked flask, rising temperature 50 C, add two (4-carboxyl phenyl) phenyl phosphine oxide 1.25g, adjusting mixed solution pH is 4, stirring reaction 1h, 50 DEG C add EDTAP dipotassium ethylene diamine tetraacetate 2.5g, and fully stirring reaction 2h, obtains fire retardant;
(3), in the 500ml there-necked flask with thermometer, agitator, add PTMG 40g, IPDI 20g and the prepared fullerene catalyst 0.18g of step (1), at 60 DEG C, react 1h, add coroxon 0.12g, bromine propylamine peptide woods 0.12g and Antorane 0.23g, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A60.1g;
(4), to add in base polyurethane prepolymer for use as A 1, 4 dihydroxy-6-tectoquinone 1.1g, butanone 7.8g and Riboflavine sodium phosphate 3g, under 60 DEG C of conditions, react 2.5h, add the prepared fire retardant 1.8g of step (2) and chlorothiazide 0.23g, 75 DEG C of reaction temperatures, reaction time 1h, add again 1, 4-dihydroxy anthraquinone 1.8g, PAMA 0.6g and different stearic aminopropyl amine oxide 1.2g, 75 DEG C of reaction temperatures, reaction time 1h, add again triethylamine 6g to carry out neutralization reaction 30min, 120g emulsification 30min adds water, obtain fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive.
Example five
(1), the preparation of fullerene catalyst: take 40mg fullerene in 250ml there-necked flask, add 20g triethanolamine and ethanol 12g, 70 DEG C of stirring reaction 8h of oil bath under nitrogen protection, the excessive triethanolamine of pressure reducing and steaming and ethanol, the brown sticky matter of gained dissolves with the vibration of 10ml distilled water, add again 50ml acetone, there are a large amount of brown flocculent deposits to separate out, centrifugal, sediment acetone washed twice, vacuum drying, obtains the fullerene triethanolamine derivative of 140mg brown ceramic powder shape; Above-mentioned 140mg fullerene triethanolamine derivative is dissolved in to 20ml distilled water, pour 30ml into and be dissolved with 4-amino-2, in the aqueous solution of 6-dibromophenol stannic chloride hydrochloride 200mg, be heated to 90 DEG C, have brown precipitation to produce, after insulation 30min, centrifugal while hot, distilled water washing 4 times for solids, vacuum drying, obtain brown solid, be prepared fullerene catalyst;
(2), fire retardant preparation: the aqueous solution of nitric acid that is 0.1mol/L by 30ml concentration, mercaptan antimony 2g, molybdenum boride 2.5g join in 50ml there-necked flask, rising temperature 50 C, add two (4-carboxyl phenyl) phenyl phosphine oxide 1.25g, adjusting mixed solution pH is 4, stirring reaction 1h, 50 DEG C add EDTAP dipotassium ethylene diamine tetraacetate 2.5g, and fully stirring reaction 2h, obtains fire retardant;
(3), in the 500ml there-necked flask with thermometer, agitator, add PTMG 75g, IPDI 30g and the made fullerene catalyst 0.47g of step (1), at 75 DEG C, react 1.5h, add coroxon 0.32g and bromine propylamine peptide woods 0.53g, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A106g;
(4), to base polyurethane prepolymer for use as A2-methyl isophthalic acid, 3, 6. trihydroxyanthraquinone 2.9g, butanone 20.7g, methyl sulfonyl methane 3.8g and Riboflavine sodium phosphate 6.9g, under 75 DEG C of conditions, react 3h, add the prepared fire retardant 5.3g of step (2) and sulfaquinoxaline 0.32g, 80 DEG C of reaction temperatures, reaction time 1.5h, add again 1, 4-dihydroxy anthraquinone 4.2g, PAMA 1.6g and Sodium Polyacrylate 3.2g, 75 DEG C of reaction temperatures, reaction time 1.5h, add again triethylamine 13.3g to carry out neutralization reaction 40min, 130g emulsification 30min adds water, obtain fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive.
Further illustrate beneficial effect of the present invention below by related experiment data:
For quantitative description resistance to light of coating energy, adopt spectrophotometer to detect, to obtain inverse difference △ E, the light resistance of coating and finish paint is described. △ E has represented change color degree, and △ E is larger, and color change is more obvious. In general, △ E value is the slight variation of 0～1.5 genus; △ E value is that 1.5～3.0 genus can be felt variation; △ E value be 3.0～6.0 belong to significant changes (referring to Wang Fang, party's climax, Wang Liqin, the light degradation [J] of several organic historical relic's protection polymer coatings. Northwest University's journal, 2005,35 (5): 56 ~ 58).
Table one is fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive institute film forming light resistance
| Time/min | Example one | Example two | Example three | Example four | Example five |
| 90 | 0.3 | 0.3 | 0.4 | 0.1 | 0.1 |
| 150 | 0.7 | 0.4 | 0.4 | 0.2 | 0.3 |
| 270 | 0.8 | 0.5 | 0.6 | 0.2 | 0.3 |
| 330 | 0.9 | 0.7 | 0.6 | 0.4 | 0.3 |
| 390 | 1.2 | 0.9 | 0.8 | 0.5 | 0.3 |
| 450 | 1.2 | 1.0 | 0.8 | 0.6 | 0.3 |
| 510 | 1.2 | 1.2 | 0.9 | 0.7 | 0.7 |
| 540 | 1.3 | 1.2 | 1.0 | 0.9 | 0.8 |
| 600 | 1.3 | 1.2 | 1.2 | 1.1 | 0.9 |
Can find from table one, example one all in slight excursion, shows good light resistance to the prepared coating of example five and adhesive light resistance.
Table two is fast light and water proofing property waterborne flame retardant polyurethane coating and the sunproof mechanical property of adhesive institute film forming
| Experimental group | Example one | Example two | Example three | Example four | Example five |
| Elongation at break/% | 161 | 146 | 156 | 167 | 169 |
| Tensile strength/MPa | 5.8 | 5.7 | 5.7 | 6.0 | 6.0 |
| Abrasion resisting/level | 3.5 | 4 | 4 | 4 | 4 |
The reference of table two middle finger object detection method (Jiang Weiqi. leather finished product physical and chemical inspection [M]. China Light Industry Press, 1999), coating of the present invention and adhesive gained film elongation at break, tensile strength, wear-resistant all performances are better.
Table three is fast light and the anti-flammability of water proofing property waterborne flame retardant polyurethane coating and adhesive gained film
| Example one | Example two | Example three | Example four | Example five | Market PU-1 | |
| Maximum smoke density | 23 | 26 | 28 | 12 | 7 | 43 |
| Reach maximum smoke density time/s | 180 | 180 | 185 | 210 | 210 | 120 |
| Oxygen index (OI) | 25.5 | 25.7 | 25.8 | 26.8 | 27.8 | 22 |
| Flaming combustion time/s | 23.4 | 22.4 | 14.3 | 11.8 | 10.1 | 25.1 |
| Flameless combustion time/s | 0 | 0 | 0 | 0 | 0 | 0 |
The detection of table three indices is respectively according to following standard: smoke density is measured according to GB8323-2008, and oxygen index (OI) adopts GB/T5454-1997 " textile combustion performance test-oxygen index method " to measure; Flaming combustion time and flameless combustion time are to be measured by GB/T5455-1997 " textile combustion energy test-normal beam technique ".
As shown in Table 3, the present invention is fast light while burning with water proofing property flame retardant polyurethane coating and adhesive gained film, and maximum smoke density significantly reduces, and reaches maximum smoke density time significant prolongation, and oxygen index (OI) obviously improves, and obviously shorten burning time.
Table four is fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive institute filming performance
| Experimental group | Example one | Example two | Example three | Example four | Example five |
| Film outward appearance (resistance to water 48h) | Transparent | Transparent | Transparent | Transparent | Transparent |
| Hardness | B | B | B | B | B |
| Adhesive force/level | 2 | 3 | 3 | 3 | 3 |
| Pliability/mm | 2 | 2 | 2 | 2 | 3 |
Water proofing property employing is got appropriate emulsion and is evenly coated on glass plate, after drying and forming-film, glass plate is put into deionized water and soak under uniform temperature, observes film and becomes blue, turns white, bubbles, sends out the situation of wrinkling, coming off.
Can find from table four, from film outward appearance, hardness, adhesive force, flexibility better performances.
Claims (5)
1. the preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive, is characterized in that:
(1), the preparation of fullerene catalyst: take 40mg fullerene in there-necked flask, add 20g triethanolamine and ethanol 12g, 70 DEG C of reaction 8h of oil bath under nitrogen protection, the excessive triethanolamine of pressure reducing and steaming and ethanol, the brown sticky matter of gained dissolves with the vibration of 10ml distilled water, add again 50ml acetone, there are a large amount of brown flocculent deposits to separate out, centrifugal, sediment acetone washed twice, vacuum drying, obtains the fullerene triethanolamine derivative of 140mg brown ceramic powder shape; Again 140mg fullerene triethanolamine derivative is dissolved in to 20ml distilled water, pour 30ml into and be dissolved with 4-amino-2, in the aqueous solution of 6-dibromophenol stannic chloride hydrochloride 200mg, be heated to 90 DEG C, have brown precipitation to produce, after insulation 30min, centrifugal while hot, distilled water washing 4 times for solids, vacuum drying, obtain brown solid, be prepared fullerene catalyst.
(2), fire retardant preparation: the aqueous solution of nitric acid dissolved oxygen antimony chromium titanium 2g and the molybdenum boride 2.5g that are 0.1mol/L by 30ml concentration, increase the temperature to 50 DEG C, add two (4-carboxyl phenyl) phenyl phosphine oxide 1.25g, adjusting mixed solution pH is 4, reaction 1h, 50 DEG C add EDTAP dipotassium ethylene diamine tetraacetate 2.5g, and fully stirring reaction 2h, obtains fire retardant;
(3), under the condition existing in the made fullerene catalyst of step (1), PTMG is mixed by weight 2:1 ~ 5:1 with IPDI, at 60 ~ 85 DEG C, react 1 ~ 2h, add coroxon and bromine propylamine peptide woods, reaction time 3h, 70 DEG C of reaction temperatures, obtain base polyurethane prepolymer for use as A, described fullerene catalyst consumption is 0.3 ~ 0.6% of PTMG and IPDI gross weight, coroxon consumption is PTMG, 0.2 ~ 0.4% of IPDI and fullerene catalyst gross weight, bromine propylamine peptide woods is PTMG, 0.2 ~ 0.8% of IPDI and fullerene catalyst gross weight,
(4), add the chain extender of base polyurethane prepolymer for use as A weight 1.8 ~ 3.6% and butanone and the Riboflavine sodium phosphate of base polyurethane prepolymer for use as A weight 13 ~ 26% to base polyurethane prepolymer for use as A, under 60 ~ 85 DEG C of conditions, react 2.5 ~ 3.5h, add the prepared fire retardant of step (2), 75 ~ 85 DEG C of reaction temperatures, reaction time 1 ~ 2h, add again 1, 4-dihydroxy anthraquinone, polyacrylamide and tackifier, 75 DEG C of reaction temperatures, reaction time 1 ~ 2h, the triethylamine that adds again base polyurethane prepolymer for use as A weight 10 ~ 15% carries out neutralization reaction 30 ~ 50min, add water emulsification 30min, obtain fast light and water proofing property waterborne flame retardant polyurethane coating and adhesive, Riboflavine sodium phosphate, fire retardant, 1, 4-dihydroxy anthraquinone, polyacrylamide, tackifier are respectively 5 ~ 8% of base polyurethane prepolymer for use as A weight, 3 ~ 7%, 3 ~ 5%, 1 ~ 2%, 2 ~ 4%.
2. the preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating as claimed in claim 1 and adhesive, is characterized in that: the molecular weight of PTMG is 2000.
3. the preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating as claimed in claim 1 and adhesive; it is characterized in that: chain extender is 1; 3-dihydroxy-2-methylanthraquinone, 1; 3; 6-trihydroxy-2-methyl-9,10-anthraquinone-3-O-(6-O-acetyl group)-β-D-Glucose, 2-methyl isophthalic acid, 3; 6. any one in trihydroxyanthraquinone, Isosorbide-5-Nitrae-dihydroxy-6-tectoquinone.
4. the preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating as claimed in claim 1 and adhesive, is characterized in that: polyacrylamide is anionic.
5. the preparation method of fast light and water proofing property waterborne flame retardant polyurethane coating as claimed in claim 1 and adhesive, is characterized in that: tackifier are any one of coconut monoethanol amide, Ji Wusi behenate, propylene glycol stearate, different stearic aminopropyl amine oxide, Sodium Polyacrylate.
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Effective date of registration: 20160429 Address after: 100000 Beijing city Huairou District Yanqi Economic Development Zone South Street No. 2 room 3220 2 3 Office Patentee after: HUIRONG HI-TECH NEW MATERIAL TECHNOLOGY Co.,Ltd. Address before: 264000 16-2, Fu Qing Street, Zhifu District, Shandong, Yantai Patentee before: Duan Xiaoning |
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| C53 | Correction of patent of invention or patent application | ||
| CI01 | Publication of corrected invention patent application |
Correction item: Inventor|Patentee|Address|Patent agency|agent Correct: Yan Wen|Zheng Silong|Yan Mulin|Xu Li|HUIRONG HI-TECH NEW MATERIAL TECHNOLOGY CO., LTD.|100000 Beijing city Huairou District Yanqi Economic Development Zone South Street No. 2 room 3220 2 3 Office|Beijing intellectual property agency|Tang Dongfeng False: Duan Xiaoning|Luo Sheng|Wang Yaqian|Song Li|Xia Xueying|Duan Xiaoning|264000 16-2, Fu Qing Street, Zhifu District, Shandong, Yantai|None Number: 19 Volume: 32 |
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| CI03 | Correction of invention patent |
Correction item: Inventor|Patentee|Address|Patent agency|agent Correct: Yan Wen|Zheng Silong|Yan Mulin|Xu Li|HUIRONG HI-TECH NEW MATERIAL TECHNOLOGY CO., LTD.|100000 Beijing city Huairou District Yanqi Economic Development Zone South Street No. 2 room 3220 2 3 Office|Beijing intellectual property agency|Tang Dongfeng False: Duan Xiaoning|Luo Sheng|Wang Yaqian|Song Li|Xia Xueying|Duan Xiaoning|264000 16-2, Fu Qing Street, Zhifu District, Shandong, Yantai|None Number: 19 Page: The title page Volume: 32 |
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| ERR | Gazette correction | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160511 |