CN104449310B - The preparation method of the simple coating of technique - Google Patents
The preparation method of the simple coating of technique Download PDFInfo
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- CN104449310B CN104449310B CN201410602683.8A CN201410602683A CN104449310B CN 104449310 B CN104449310 B CN 104449310B CN 201410602683 A CN201410602683 A CN 201410602683A CN 104449310 B CN104449310 B CN 104449310B
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- 239000011248 coating agent Substances 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims abstract description 7
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 claims abstract description 7
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 6
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- RNFNDJAIBTYOQL-UHFFFAOYSA-N chloral hydrate Chemical compound OC(O)C(Cl)(Cl)Cl RNFNDJAIBTYOQL-UHFFFAOYSA-N 0.000 claims description 4
- 229960002327 chloral hydrate Drugs 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 claims description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 3
- 229920001730 Moisture cure polyurethane Polymers 0.000 abstract description 7
- 150000001298 alcohols Chemical class 0.000 abstract description 6
- 239000004970 Chain extender Substances 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 4
- -1 nitrogen-containing compound Chemical class 0.000 abstract description 3
- 125000000896 monocarboxylic acid group Chemical group 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 229920002635 polyurethane Polymers 0.000 description 11
- 239000004814 polyurethane Substances 0.000 description 11
- 239000003063 flame retardant Substances 0.000 description 7
- 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 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 6
- 239000000779 smoke Substances 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical group O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- FGYHQFZISBDLDR-UHFFFAOYSA-N OCCC[PH2]=O Chemical compound OCCC[PH2]=O FGYHQFZISBDLDR-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 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
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3271—Hydroxyamines
- C08G18/3275—Hydroxyamines containing two hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/341—Dicarboxylic acids, esters of polycarboxylic acids containing two carboxylic acid groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3802—Low-molecular-weight compounds having heteroatoms other than oxygen having halogens
- C08G18/3804—Polyhydroxy compounds
- C08G18/3806—Polyhydroxy compounds having chlorine and/or bromine atoms
- C08G18/3808—Polyhydroxy compounds having chlorine and/or bromine atoms having chlorine atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3819—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen
- C08G18/3842—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring
- C08G18/3851—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring containing three nitrogen atoms in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3878—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus
- C08G18/388—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus having phosphorus bound to carbon and/or to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3893—Low-molecular-weight compounds having heteroatoms other than oxygen containing silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
Abstract
The invention discloses the preparation method of a kind of coating, under conditions of dibutyltin dilaurate catalyst exists, dihydroxylic alcohols is mixed with hexamethylene diisocyanate, at 70 ~ 90 DEG C, react 1.0 ~ 3.0h, obtain base polyurethane prepolymer for use as；Hydrophilic chain extender, silicol and organic solvent is added in base polyurethane prepolymer for use as, 1.5 ~ 3.5h is reacted under the conditions of 65 ~ 95 DEG C, add nitrogen-containing compound and react 1 ~ 3h in 65 ~ 85 DEG C, it is the ratio of 0.6:1 ~ 1.2:1 in the mol ratio of COOH/NH2, add triethylamine and be neutralized reaction 30 ~ 70min, add water and carry out emulsifying, form a kind of anti-flammability coating.Prepared anti-flammability coating environmental protection, cheap, the market demand can be met.
Description
The application is divisional application, the application number of original application: 201310094271.3, the applying date: 2013-03-22, denomination of invention: the preparation method of a kind of anti-flammability coating。
Technical field
The present invention relates to the preparation method of a kind of coating, particularly to the preparation method of a kind of anti-flammability coating.
Background technology
Aqueous polyurethane is as one important research direction of coating, its (also known as water-based polyurethane) is a kind of polyurethane resin in the strand of polyurethane containing hydrophilic radical, with water, there is the strongest affinity, use specific technique can be allowed to disperse and formed stable system in water.Aqueous polyurethane is mainly used in the aspects such as leather finish, textile printing and dyeing, paper-making industry, building coating, adhesive, and involved is nearly all combustible material, and these materials as the most fire retardant treated, necessarily become the potential safety hazard of initiation fire in use.Aqueous polyurethane flame-retarded, is one of the important directions of aqueous polyurethane functionalization.
Summary of the invention
The present invention is actually subjected to solve the technical problem that and is to provide a kind of aqueous flame retardant polyurethane coating.
In order to solve above-mentioned technical problem, present invention employs techniques below scheme.
(1), under conditions of dibutyltin dilaurate catalyst exists, it is 1.5:1 ~ 4.5:1 by the mol ratio of NCO/OH, dihydroxylic alcohols is mixed with hexamethylene diisocyanate, at 70 ~ 90 DEG C, react 1.0 ~ 3.0h, obtain base polyurethane prepolymer for use as A；Described catalyst amount is the 0.5 ~ 0.9% of dihydroxylic alcohols and hexamethylene diisocyanate gross weight；
(2), in product A, addition carboxyl-content is the hydrophilic chain extender of product A weight 1.5 ~ 3.5%, the silicol of product A weight 10.5 ~ 15.5% and the organic solvent of product A weight 10 ~ 20%, reacts 1.5 ~ 3.5h, obtain product B under the conditions of 65 ~ 95 DEG C；
(3) it is the 2 ~ 6% of product A weight toward B adds nitrogen-containing compound, again, reacts 1 ~ 3h in 65 ~ 85 DEG C, be the ratio of 0.6:1 ~ 1.2:1 in the mol ratio of COOH/NH2, add triethylamine and be neutralized reaction 30 ~ 70min, add water and carry out emulsifying, obtain product C, be anti-flammability coating；
Dihydroxylic alcohols is any one in chloral hydrate, double (hydroxypropyl) phosphine oxide of normal-butyl；Hydrophilic chain extender is any one in maleic acid, succinic acid, ethanedioic acid；Silicol number-average molecular weight is 600 ~ 1000g/mol；Organic solvent is any one in pyridine, Ketohexamethylene, N,N-dimethylacetamide；Nitrogen-containing compound is any one in dihydroxy dimethyl tripolycyanamide, diethanolamine.
The invention have the characteristics that:
(1) replace the dihydroxylic alcohols of conventional synthesis base polyurethane prepolymer for use as with anti-flammability dihydroxylic alcohols, and play silicon, nitrogen, chlorine or silicon, nitrogen, phosphorus synergism, improve coating anti-flammability；
(2) replace the organic solvent DMF of traditional polyurethane with pyridine, Ketohexamethylene, N,N-dimethylacetamide, preparation technology is simple；
Detailed description of the invention
The present invention is further illustrated below in conjunction with example.
Example one
(1), in the four-hole boiling flask equipped with the 500ml stirring slurry, thermometer, condensing tube, chloral hydrate 16.5g is mixed with hexamethylene diisocyanate 33.3g, under conditions of dibutyltin dilaurate catalyst 0.249g exists, at 70 DEG C, react 1 h, obtain 49.9g base polyurethane prepolymer for use as A；
(2), in product A, addition hydrophilic chain extender maleic acid 0.96g, number-average molecular weight are 600 g/mol silicol 5.24g and pyridine 4.99g, react 1.5 h, obtain product B under the conditions of 65 DEG C；
(3), again in product B adding dihydroxy dimethyl tripolycyanamide 1.0g, in 65 DEG C of reaction 1h, addition triethylamine 2.79g is neutralized reaction 30 min, the 140g that adds water and carries out emulsifying formation 202.2g flame-retardant polyurethane C.
Example two
(1), in the four-hole boiling flask equipped with the 500ml stirring slurry, thermometer, condensing tube, double for normal-butyl (hydroxypropyl) phosphine oxide 22.2g are mixed with hexamethylene diisocyanate 75.6g, under conditions of dibutyltin dilaurate catalyst 0.88g exists, at 90 DEG C, react 3 h, obtain 97.6g base polyurethane prepolymer for use as A；
(2), in product A, addition succinic acid 4.48g, number-average molecular weight are 1000 g/mol silicol 15.1g and Ketohexamethylene 19.5g, react 3.5 h, obtain product B under the conditions of 95 DEG C；
(3), again in product B adding diethanolamine 5.86g, reaction temperature 85 DEG C, response time 3h, addition triethylamine 6.39g are neutralized reaction 70 min, the 130g that adds water and carry out emulsifying, form 275g flame-retardant polyurethane C.
Example three
(1), in the four-hole boiling flask equipped with the 500ml stirring slurry, thermometer, condensing tube, chloral hydrate 16.5g is mixed with hexamethylene diisocyanate 66.6g, under conditions of dibutyltin dilaurate catalyst 0.58g exists, at 80 DEG C, react 2 h, obtain 83g base polyurethane prepolymer for use as A；
(2), in product A, addition ethanedioic acid 1.66g, number-average molecular weight are 800 g/mol silicol 10.8g and N,N-dimethylacetamide 12.5g, react 2.5 h, obtain product B under the conditions of 75 DEG C；
(3), again in B adding dihydroxy dimethyl tripolycyanamide 3.32g, reaction temperature 75 DEG C, response time 2h, addition triethylamine 4.1g are neutralized reaction 50 min, the 140g that adds water and carry out emulsifying, form 245.9g flame-retardant polyurethane C；
Table one and table two are coating institute film forming gained performance indications prepared by present example two.
Film anti-flammability is to be weighed by smoke density method (maximum smoke density, reach the maximum smoke density time), oxygen index (OI), vertical combustion index (flaming combustion time, glowing time), elongation at break characterizes its mechanical property, and table one is example two gained polyaminoester emulsion and the flame-retardant polyurethane SPUA-352 performance comparison on market.
Table one anti-flammability paint film flame retardant effect index
The detection of table one indices is respectively according to following standard: smoke density measures according to GB8323-2008；Oxygen index (OI) uses GB/T5454-1997 " textile combustion performance test-oxygen index method " to measure；Flaming combustion time and glowing time are to be measured by GB/T 5455-1997 " textile combustion energy test-normal beam technique ".
As shown in Table 1, after anti-flammability paint film of the present invention is lighted, maximum smoke density significantly reduces, and reaches the maximum smoke density time and significantly extends, and oxygen index (OI) significantly improves, and burning time substantially shortens.
Table two anti-flammability paint film gained elongation at break
The reference of table two middle finger object detection method (Jiang Weiqi. leather finish physical and chemical inspection [M]. China Light Industry Press, 1999,82 ~ 96), the elongation at break of the SPUA-352 institute film forming that anti-flammability coating gained film elongation at break of the present invention is more best than market fire resistance is big.
Claims (1)
1. the preparation method of a coating, it is characterised in that including:
(1), chloral hydrate 16.5g is mixed with hexamethylene diisocyanate 66.6g, under conditions of dibutyltin dilaurate catalyst 0.58g exists, at 80 DEG C, react 2h, obtain product A；
(2), in product A, addition ethanedioic acid 1.66g, number-average molecular weight are 800g/mol silicol 10.8g and N,N-dimethylacetamide 12.5g, react 2.5h, obtain product B under the conditions of 75 DEG C；
(3), again in B adding dihydroxy dimethyl tripolycyanamide 3.32g, reaction temperature 75 DEG C, response time 2h, addition triethylamine 4.1g are neutralized reaction 50min, the 140g that adds water and carry out emulsifying, form coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410602683.8A CN104449310B (en) | 2013-03-22 | 2013-03-22 | The preparation method of the simple coating of technique |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310094271.3A CN103113821B (en) | 2013-03-22 | 2013-03-22 | Preparation method of flame-retardant coating |
| CN201410602683.8A CN104449310B (en) | 2013-03-22 | 2013-03-22 | The preparation method of the simple coating of technique |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310094271.3A Division CN103113821B (en) | 2013-03-22 | 2013-03-22 | Preparation method of flame-retardant coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104449310A CN104449310A (en) | 2015-03-25 |
| CN104449310B true CN104449310B (en) | 2016-08-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410602683.8A Expired - Fee Related CN104449310B (en) | 2013-03-22 | 2013-03-22 | The preparation method of the simple coating of technique |
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| CN1749291A (en) * | 2005-09-29 | 2006-03-22 | 上海申真企业发展有限公司 | Flame-retardant polyurethane water dispersion and its preparing method |
| CN102516489A (en) * | 2011-12-14 | 2012-06-27 | 华南理工大学 | Preparation method and application of wear resistant hydroxyl terminated polyurethane resin used for protection coating of silica key |
| CN102827571A (en) * | 2012-09-28 | 2012-12-19 | 广东多正化工科技有限公司 | Preparation method of water-based polyurethane adhesive |
| CN102898936A (en) * | 2012-10-13 | 2013-01-30 | 段宝荣 | Method for preparing fire-retarding aqueous polyurethane |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1749291A (en) * | 2005-09-29 | 2006-03-22 | 上海申真企业发展有限公司 | Flame-retardant polyurethane water dispersion and its preparing method |
| CN102516489A (en) * | 2011-12-14 | 2012-06-27 | 华南理工大学 | Preparation method and application of wear resistant hydroxyl terminated polyurethane resin used for protection coating of silica key |
| CN102827571A (en) * | 2012-09-28 | 2012-12-19 | 广东多正化工科技有限公司 | Preparation method of water-based polyurethane adhesive |
| CN102898936A (en) * | 2012-10-13 | 2013-01-30 | 段宝荣 | Method for preparing fire-retarding aqueous polyurethane |
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