CN104292924B - A kind of anti-flaming dope and its preparation method - Google Patents
A kind of anti-flaming dope and its preparation method Download PDFInfo
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- CN104292924B CN104292924B CN201410495182.4A CN201410495182A CN104292924B CN 104292924 B CN104292924 B CN 104292924B CN 201410495182 A CN201410495182 A CN 201410495182A CN 104292924 B CN104292924 B CN 104292924B
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- flaming dope
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- wetting agent
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 235000019832 sodium triphosphate Nutrition 0.000 claims abstract description 40
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 30
- 239000002904 solvent Substances 0.000 claims abstract description 29
- 239000000080 wetting agent Substances 0.000 claims abstract description 29
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 28
- FUXMTEKFGUWSNC-UHFFFAOYSA-N 2,3,4,5-tetrachlorobenzoic acid Chemical compound OC(=O)C1=CC(Cl)=C(Cl)C(Cl)=C1Cl FUXMTEKFGUWSNC-UHFFFAOYSA-N 0.000 claims abstract description 20
- MRUDNSFOFOQZDA-UHFFFAOYSA-N 2,6-dichlorobenzoic acid Chemical compound OC(=O)C1=C(Cl)C=CC=C1Cl MRUDNSFOFOQZDA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 20
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 101710194948 Protein phosphatase PhpP Proteins 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 20
- 229920001577 copolymer Polymers 0.000 claims abstract description 20
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims abstract description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 20
- 239000010452 phosphate Substances 0.000 claims abstract description 20
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 20
- 239000011591 potassium Substances 0.000 claims abstract description 20
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 20
- 239000011734 sodium Substances 0.000 claims abstract description 20
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims abstract description 20
- QRAOZQGIUIDZQZ-UHFFFAOYSA-N 4-methyl-7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2,3-dihydro-1,4-benzoxazine Chemical compound C=1C=C2N(C)CCOC2=CC=1B1OC(C)(C)C(C)(C)O1 QRAOZQGIUIDZQZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- -1 polyoxyethylene octylphenol Polymers 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- 150000007942 carboxylates Chemical class 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- PBULHKIPTBIZHO-UHFFFAOYSA-N dodecane-1-sulfonyl chloride Chemical compound CCCCCCCCCCCCS(Cl)(=O)=O PBULHKIPTBIZHO-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 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 abstract description 15
- 239000003063 flame retardant Substances 0.000 abstract description 15
- 238000009413 insulation Methods 0.000 abstract description 7
- 239000003973 paint Substances 0.000 description 19
- 239000011248 coating agent Substances 0.000 description 16
- 238000000576 coating method Methods 0.000 description 16
- 239000000463 material Substances 0.000 description 10
- 239000000049 pigment Substances 0.000 description 9
- LPAOLPKVGFMASA-UHFFFAOYSA-N C1=CC=C2C(=C1)N=CC(O2)Cl Chemical compound C1=CC=C2C(=C1)N=CC(O2)Cl LPAOLPKVGFMASA-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- 230000003245 working effect Effects 0.000 description 3
- 239000004606 Fillers/Extenders Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/324—Alkali metal phosphate
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a kind of anti-flaming dope and its preparation method, anti-flaming dope comprises the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 50��100 parts, 2,6-dichlorobenzoic acid 60��120 parts, 2,3,4,5-tetrachloro-benzoic acid 10��50 parts, 40��60 parts, tetracol phenixin, organotin copolymer 70��150 parts, Witco 1298 Soft Acid ammonium 120��130 parts, tripoly phosphate sodium STPP 20��60 parts, potassium primary phosphate 30��80 parts, chlorination K42��52 part, wetting agent 60��75 parts, pH adjusting agent 80��100 parts, solvent 100��200 parts. Preparation method is: by solvent, 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K mix even, drop into pH adjusting agent, add wetting agent, mixed even. Insulation resistance of the present invention is greater than 1.2 �� 1013��, flame retardant resistance reaches V-0 grade, 300 DEG C of baking ovens place 4 hours after weight rate between 0.08��0.11%.
Description
Technical field
The invention belongs to flame retardant area, particularly relate to a kind of anti-flaming dope and its preparation method.
Background technology
Coating is a kind of material, and this kind of material can be coated in article surface by different construction technologies, forms adhere well, has certain intensity, continuous print solid film. The film common name film formed like this, also known as paint film or coating. Coating has protection function, decoration functions and some other function. Protection function comprises anticorrosion, waterproof, grease proofing, chemicals-resistant, fast light, heatproof etc. Object is exposed among air, is subject to the erosion of oxygen, moisture etc., causes the breakoff phenomenons such as corrosion of metal, foxy, cement weathering. It is coated with coating at article surface, forms layer protecting film, it is possible to stop or postpone generation and the development of these breakoff phenomenons, the work-ing life of various material is extended. So, provide protection is a mainly effect of coating. Decoration functions comprises distinct colors, gloss, pattern and smooth property etc. The object of unlike material is coated with to be coated, and can obtain multicoloured, bright and colourful outward appearance, play the effect beautifying human habitat, and material life and cultural life to the mankind make the contribution that can not be ignored. In addition, coating also has the functions such as mark, antifouling, insulation.
Coating is generally all made up of filmogen, film forming subsidiary material matter and auxiliary film forming matter three kinds of base substances:
Filmogen: also claim binding agent, filmogen major part is that organic high molecular compound is such as mixes such as natural resin (rosin, lacquer), coating (tung oil, oleum lini, soya-bean oil, fish oil etc.), synthetic resins, become through pyroreaction, also the paint (as: inorganic zinc rich paint) of organic/inorganic substance combination. It is the main body forming paint, it is resolved that the performance of paint film. If not having filmogen, simple pigment and subsidiary material can not form paint film.
Film forming subsidiary material matter: comprise various pigment, pigment extender, rust-stabilising pigment. Pigment provides color and opacifying power for paint film, it is to increase the protective value of paint and decorative effect, the pigment of good weatherability can improve the work-ing life of paint. Pigment extender can increase the thickness of paint film, utilizes the performance of itself " sheet, needle-like " structure, folded multiple by the accumulation of pigment, forms the paint film of fish scale shape, it is to increase the work-ing life of paint film, it is to increase water-repellancy and rust-proof effect. Rust-stabilising pigment, by itself physics and chemistry rust inhibition, prevents body surface from being corroded by air, chemical substance, and metallic surface is by corrosion.
Auxiliary film forming matter: comprise various auxiliary agent, solvent. Various auxiliary agent is in the production process of paint, storage process, use procedure, and the forming process of paint film plays extremely important effect. Although the amount used is all little, but on the performance impact of paint film greatly, even can not form paint film as: do not do, sink to the bottom caking, skinning. Water-miscible paint more needs auxiliary agent could meet production, construction, storage and form paint film. Solvent also claims mainly be diluted to membrane substance and form thick liquid " dispersion medium " (comprising various organic solvent, water), so that producing and construction. Often the mixture of film forming base-material and dispersion medium is called paint vehicle.
The Chinese patent application that application number is 200910263366.7, denomination of invention is " thermal insulating coating " discloses a kind of thermal insulating coating, mixes by two kinds of components, and the coating application prepared is convenient, do not affect body of wall. But the flame retardant properties of this coating is general.
Application number is 200410012788.4, denomination of invention coating disclosed in the Chinese patent of " waterproof, heat insulation, anti-flaming dope ", comprise major ingredient, auxiliary material, this invention realizes the effect of water-proof thermal insulation flame retardant mainly through changing major ingredient composition, but influencing each other between composition, although the performance of each side all increases, but amplitude is little, particularly flame retardant properties, only slightly improve than prior art, and some coating is in use, flame retardant properties is required very high.
Summary of the invention
The present invention is in order to overcome the deficiencies in the prior art, it is provided that a kind of anti-flaming dope and its preparation method, the flame retardant properties of anti-flaming dope is good.
The present invention is by the following technical solutions:
A kind of anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 50��100 parts, 2,6-dichlorobenzoic acid 60��120 parts, 2,3,4,5-tetrachloro-benzoic acid 10��50 parts, 40��60 parts, tetracol phenixin, organotin copolymer 70��150 parts, Witco 1298 Soft Acid ammonium 120��130 parts, tripoly phosphate sodium STPP 20��60 parts, potassium primary phosphate 30��80 parts, chlorination K42��52 part, wetting agent 60��75 parts, pH adjusting agent 80��100 parts, solvent 100��200 parts.
As a further improvement on the present invention, anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 50��80 parts, 2,6-dichlorobenzoic acid 60��100 parts, 2,3,4,5-tetrachloro-benzoic acid 10��40 parts, 40��50 parts, tetracol phenixin, organotin copolymer 70��100 parts, Witco 1298 Soft Acid ammonium 120��125 parts, tripoly phosphate sodium STPP 20��50 parts, potassium primary phosphate 30��60 parts, chlorination K42��50 part, wetting agent 60��70 parts, pH adjusting agent 80��90 parts, solvent 100��150 parts.
As a further improvement on the present invention, anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 60 parts, 2,6-dichlorobenzoic acid 70 parts, 2,3,4,5-tetrachloro-benzoic acid 30 parts, 45 parts, tetracol phenixin, organotin copolymer 80 parts, Witco 1298 Soft Acid ammonium 123 parts, tripoly phosphate sodium STPP 30 parts, potassium primary phosphate 40 parts, 45 parts, Repone K, wetting agent 65 parts, pH adjusting agent 85 parts, solvent 120 parts.
As a further improvement on the present invention, additive is sulfonic chloride or dodecyl SULPHURYL CHLORIDE.
As a further improvement on the present invention, wetting agent is one or more in polyoxyethylene octylphenol ether, polyoxyethylene carboxylate, ammonium trideceth.
As a further improvement on the present invention, pH adjusting agent is sodium hydroxide or sodium carbonate.
As a further improvement on the present invention, solvent is the one in sherwood oil, normal heptane, octane, toluene or dimethylbenzene.
As a further improvement on the present invention, the mixture of the polyoxyethylene octylphenol ether of wetting agent to be weight ratio be 1:1:1, polyoxyethylene carboxylate, ammonium trideceth.
The preparation method of above-mentioned anti-flaming dope, comprise the following steps: by solvent, the chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K drop in container and fully mix, then drop into pH adjusting agent, adjust ph to 9��10, finally add wetting agent, mix.
As a further improvement on the present invention, pH value is 9.5.
Technique effect
The insulation resistance of obtained flame-retardant coating of the present invention is greater than 1.2 �� 1013��, flame retardant resistance reaches V-0 grade, 300 DEG C of baking ovens place 4 hours after weight rate between 0.08��0.11%.
Embodiment
Below by specific embodiment, the present invention is described further.
Embodiment 1
A kind of anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 50 parts, 2,6-dichlorobenzoic acid 60 parts, 2,3,4,5-tetrachloro-benzoic acid 10 parts, 40 parts, tetracol phenixin, organotin copolymer 70 parts, Witco 1298 Soft Acid ammonium 120 parts, tripoly phosphate sodium STPP 20 parts, potassium primary phosphate 30 parts, chlorination K42 part, wetting agent 60 parts, pH adjusting agent 80 parts, solvent 100 parts.
Wherein, additive is sulfonic chloride.
Wetting agent is polyoxyethylene octylphenol ether.
PH adjusting agent is sodium hydroxide.
Solvent is sherwood oil.
The preparation method of above-mentioned anti-flaming dope, comprise the following steps: by solvent, the chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K drop in container and fully mix, then drop into pH adjusting agent, adjust ph to 9, finally add wetting agent, mix.
Embodiment 2
A kind of anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 100 parts, 2,6-dichlorobenzoic acid 120 parts, 2,3,4,5-tetrachloro-benzoic acid 50 parts, 60 parts, tetracol phenixin, organotin copolymer 150 parts, Witco 1298 Soft Acid ammonium 130 parts, tripoly phosphate sodium STPP 60 parts, potassium primary phosphate 80 parts, 52 parts, Repone K, wetting agent 75 parts, pH adjusting agent 100 parts, solvent 200 parts.
Wherein, additive is dodecyl SULPHURYL CHLORIDE.
Wetting agent is the polyoxyethylene carboxylate of weight ratio 1:1 and the mixture of ammonium trideceth.
PH adjusting agent is sodium carbonate.
Solvent is octane.
The preparation method of above-mentioned anti-flaming dope, comprise the following steps: by solvent, the chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K drop in container and fully mix, then drop into pH adjusting agent, adjust ph to 10, finally add wetting agent, mix.
Embodiment 3
A kind of anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 60 parts, 2,6-dichlorobenzoic acid 70 parts, 2,3,4,5-tetrachloro-benzoic acid 30 parts, 45 parts, tetracol phenixin, organotin copolymer 80 parts, Witco 1298 Soft Acid ammonium 123 parts, tripoly phosphate sodium STPP 30 parts, potassium primary phosphate 40 parts, 45 parts, Repone K, wetting agent 65 parts, pH adjusting agent 85 parts, solvent 120 parts.
Wherein, additive is dodecyl SULPHURYL CHLORIDE.
PH adjusting agent is sodium hydroxide.
Solvent is normal heptane.
The mixture of the polyoxyethylene octylphenol ether of wetting agent to be weight ratio be 1:1:1, polyoxyethylene carboxylate, ammonium trideceth.
The preparation method of above-mentioned anti-flaming dope, comprise the following steps: by solvent, the chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K drop in container and fully mix, then drop into pH adjusting agent, adjust ph to 9.5, finally add wetting agent, mix.
Embodiment 4
A kind of anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 50 parts, 2,6-dichlorobenzoic acid 60 parts, 2,3,4,5-tetrachloro-benzoic acid 14 parts, 40 parts, tetracol phenixin, organotin copolymer 72 parts, Witco 1298 Soft Acid ammonium 122 parts, tripoly phosphate sodium STPP 30 parts, potassium primary phosphate 35 parts, 45 parts, Repone K, wetting agent 67 parts, pH adjusting agent 82 parts, solvent 110 parts.
Wherein, additive is dodecyl SULPHURYL CHLORIDE.
PH adjusting agent is sodium hydroxide.
Solvent is normal heptane.
The mixture of the polyoxyethylene octylphenol ether of wetting agent to be weight ratio be 1:1:1, polyoxyethylene carboxylate, ammonium trideceth.
The preparation method of above-mentioned anti-flaming dope, comprise the following steps: by solvent, the chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K drop in container and fully mix, then drop into pH adjusting agent, adjust ph to 9.5, finally add wetting agent, mix.
Embodiment 5
A kind of anti-flaming dope, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 80 parts, 2,6-dichlorobenzoic acid 90 parts, 2,3,4,5-tetrachloro-benzoic acid 30 parts, 48 parts, tetracol phenixin, organotin copolymer 95 parts, Witco 1298 Soft Acid ammonium 124 parts, tripoly phosphate sodium STPP 23 parts, potassium primary phosphate 52 parts, 48 parts, Repone K, wetting agent 70 parts, pH adjusting agent 88 parts, solvent 140 parts.
Wherein, additive is dodecyl SULPHURYL CHLORIDE.
PH adjusting agent is sodium hydroxide.
Solvent is normal heptane.
The mixture of the polyoxyethylene octylphenol ether of wetting agent to be weight ratio be 1:1:1, polyoxyethylene carboxylate, ammonium trideceth.
The preparation method of above-mentioned anti-flaming dope, comprise the following steps: by solvent, the chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K drop in container and fully mix, then drop into pH adjusting agent, adjust ph to 9.5, finally add wetting agent, mix.
Comparative example 1
Identical with embodiment 1, difference is: do not add the chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-.
Comparative example 2
Identical with embodiment 1, difference is: do not add pH adjusting agent.
Flame retardant properties is determined as follows:
V-0: after sample carries out twice combustion testings of 10 seconds, flame extinguished in 30 seconds. Combustionmaterial can not be had to fall down.
V-1: after sample carries out twice combustion testings of 10 seconds, flame extinguished in 60 seconds. Combustionmaterial can not be had to fall down.
V-2: after sample carries out twice combustion testings of 10 seconds, flame extinguished in 60 seconds. Combustionmaterial can be had to fall down.
Anti-flaming dope obtained to embodiment and comparative example is had the performance shown in following table 1 after tested:
Table 1
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Insulation resistance �� | 1.2��1013 | 1.3��1013 | 1.6��1013 | 1.6��1011 | 1.9��1012 |
| Flame retardant resistance UL-94-V-0 1.6mm | V-0 | V-0 | V-0 | V-2 | V-1 |
| Weight rate (300 DEG C of baking ovens place 4 hours) | 0.08% | 0.09% | 0.11% | 0.18% | 0.31% |
Conclusion: the insulation resistance of obtained flame-retardant coating of the present invention is greater than 1.2 �� 1013��, flame retardant resistance reaches V-0 grade, 300 DEG C of baking ovens place 4 hours after weight rate between 0.08��0.11%.
The chloro-2H-1,4-benzoxazine of 3-(4-bromophenyl)-6-can improve the flame retardant properties of anti-flaming dope greatly, and can strengthen insulating property further. In addition, flame retardant properties is also had a certain impact by pH adjusting agent, and experiment shows, the weight rate of the anti-flaming dope adding pH adjusting agent is less, good stability.
Claims (9)
1. an anti-flaming dope, it is characterized in that, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 50��100 parts, 2,6-dichlorobenzoic acid 60��120 parts, 2,3,4,5-tetrachloro-benzoic acid 10��50 parts, 40��60 parts, tetracol phenixin, organotin copolymer 70��150 parts, Witco 1298 Soft Acid ammonium 120��130 parts, tripoly phosphate sodium STPP 20��60 parts, potassium primary phosphate 30��80 parts, chlorination K42��52 part, wetting agent 60��75 parts, pH adjusting agent 80��100 parts, solvent 100��200 parts; Its preparation method comprises the following steps: by solvent, 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine, 2,6-dichlorobenzoic acid, 2,3,4,5-tetrachloro-benzoic acid, tetracol phenixin, organotin copolymer, Witco 1298 Soft Acid ammonium, tripoly phosphate sodium STPP, potassium primary phosphate, Repone K drop in container and fully mix, drop into pH adjusting agent again, adjust ph to 9��10, finally add wetting agent, mix.
2. anti-flaming dope according to claim 1, it is characterized in that, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 50��80 parts, 2,6-dichlorobenzoic acid 60��100 parts, 2,3,4,5-tetrachloro-benzoic acid 10��40 parts, 40��50 parts, tetracol phenixin, organotin copolymer 70��100 parts, Witco 1298 Soft Acid ammonium 120��125 parts, tripoly phosphate sodium STPP 20��50 parts, potassium primary phosphate 30��60 parts, chlorination K42��50 part, wetting agent 60��70 parts, pH adjusting agent 80��90 parts, solvent 100��150 parts.
3. anti-flaming dope according to claim 1, it is characterized in that, comprise the raw material of following parts by weight: 3-(4-bromophenyl) the chloro-2H-1 of-6-, 4-benzoxazine 60 parts, 2,6-dichlorobenzoic acid 70 parts, 2,3,4,5-tetrachloro-benzoic acid 30 parts, 45 parts, tetracol phenixin, organotin copolymer 80 parts, Witco 1298 Soft Acid ammonium 123 parts, tripoly phosphate sodium STPP 30 parts, potassium primary phosphate 40 parts, 45 parts, Repone K, wetting agent 65 parts, pH adjusting agent 85 parts, solvent 120 parts.
4. anti-flaming dope according to claim 1, it is characterised in that, additive is sulfonic chloride or dodecyl SULPHURYL CHLORIDE.
5. anti-flaming dope according to claim 1, it is characterised in that, wetting agent is one or more in polyoxyethylene octylphenol ether, polyoxyethylene carboxylate, ammonium trideceth.
6. anti-flaming dope according to claim 5, it is characterised in that, the mixture of the polyoxyethylene octylphenol ether of wetting agent to be weight ratio be 1:1:1, polyoxyethylene carboxylate, ammonium trideceth.
7. anti-flaming dope according to claim 1, it is characterised in that, pH adjusting agent is sodium hydroxide or sodium carbonate.
8. anti-flaming dope according to claim 1, it is characterised in that, solvent is the one in sherwood oil, normal heptane, octane, toluene or dimethylbenzene.
9. anti-flaming dope according to claim 1, it is characterised in that, pH value is 9.5.
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