CN109093803A - A kind of novel timber flame retardant composite material and preparation method thereof - Google Patents
A kind of novel timber flame retardant composite material and preparation method thereof Download PDFInfo
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- CN109093803A CN109093803A CN201810913010.2A CN201810913010A CN109093803A CN 109093803 A CN109093803 A CN 109093803A CN 201810913010 A CN201810913010 A CN 201810913010A CN 109093803 A CN109093803 A CN 109093803A
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- chlorosilane
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 35
- 239000002131 composite material Substances 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
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 36
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 16
- 229910000410 antimony oxide Inorganic materials 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 15
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 15
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 15
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 15
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 15
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 15
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 15
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 15
- 229940008099 dimethicone Drugs 0.000 claims abstract description 13
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 13
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 13
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 5
- -1 alkyl silyl dimethyl phosphonate Chemical compound 0.000 claims description 32
- 239000005046 Chlorosilane Substances 0.000 claims description 26
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 26
- 229920000877 Melamine resin Polymers 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 19
- MASBWURJQFFLOO-UHFFFAOYSA-N ammeline Chemical compound NC1=NC(N)=NC(O)=N1 MASBWURJQFFLOO-UHFFFAOYSA-N 0.000 claims description 16
- 239000011261 inert gas Substances 0.000 claims description 16
- YLFBFPXKTIQSSY-UHFFFAOYSA-N dimethoxy(oxo)phosphanium Chemical compound CO[P+](=O)OC YLFBFPXKTIQSSY-UHFFFAOYSA-N 0.000 claims description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- DCFKHNIGBAHNSS-UHFFFAOYSA-N chloro(triethyl)silane Chemical compound CC[Si](Cl)(CC)CC DCFKHNIGBAHNSS-UHFFFAOYSA-N 0.000 claims description 6
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 4
- ACTAPAGNZPZLEF-UHFFFAOYSA-N chloro(tripropyl)silane Chemical compound CCC[Si](Cl)(CCC)CCC ACTAPAGNZPZLEF-UHFFFAOYSA-N 0.000 claims description 3
- PDNUHAXBKKDGAM-UHFFFAOYSA-N chloro-diethyl-methylsilane Chemical compound CC[Si](C)(Cl)CC PDNUHAXBKKDGAM-UHFFFAOYSA-N 0.000 claims description 3
- HXVPUKPVLPTVCQ-UHFFFAOYSA-N chloro-dimethyl-propylsilane Chemical compound CCC[Si](C)(C)Cl HXVPUKPVLPTVCQ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 125000005103 alkyl silyl group Chemical group 0.000 claims 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims 1
- 229960001826 dimethylphthalate Drugs 0.000 claims 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims 1
- 239000000758 substrate Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 description 13
- 238000006116 polymerization reaction Methods 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- 230000004580 weight loss Effects 0.000 description 12
- 239000002023 wood Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 10
- 238000004079 fireproofing Methods 0.000 description 9
- 150000004702 methyl esters Chemical class 0.000 description 7
- 150000003009 phosphonic acids Chemical class 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000005829 trimerization reaction Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000004035 construction material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- GFTGHOJGGLNVMC-UHFFFAOYSA-N N=NC=NN.N=NC=NN.C(C=1C(C(=O)O)=CC=CC1)(=O)O Chemical compound N=NC=NN.N=NC=NN.C(C=1C(C(=O)O)=CC=CC1)(=O)O GFTGHOJGGLNVMC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- VNJCDDZVNHPVNM-UHFFFAOYSA-N chloro(ethyl)silane Chemical compound CC[SiH2]Cl VNJCDDZVNHPVNM-UHFFFAOYSA-N 0.000 description 1
- AVDUEHWPPXIAEB-UHFFFAOYSA-N chloro-ethyl-dimethylsilane Chemical group CC[Si](C)(C)Cl AVDUEHWPPXIAEB-UHFFFAOYSA-N 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
-
- 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
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K2240/00—Purpose of the treatment
- B27K2240/30—Fireproofing
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
- Fireproofing Substances (AREA)
Abstract
The present invention provides a kind of novel timber flame retardant composite materials, it is at least made of the components of following parts: 20-30 parts of the expanding flame-proof material of siliceous nitrogen phosphorus, 10-15 parts of aluminium hydroxide, 10-15 parts of antimony oxide, 5-10 parts of carboxymethyl cellulose, 3-8 parts of repefral, 1-2 parts of dispersing agent, 1.5-2 parts of defoaming agent, 0.5-1 parts of antioxidant, 30-50 parts of solvent naphtha, 5-15 parts of dimethicone.Novel timber flame retardant composite material preparation process is simple, and raw material is cheap and easy to get, is readily able to large-scale production, good flame retardation effect.
Description
Technical field
The invention belongs to fire proofing fields, and in particular to an a kind of novel timber flame retardant composite material and its preparation side
Method.
Background technique
With economic fast development, demand of the people to various construction materials is increasing.Wood materials are big as four
One of construction material (steel, cement, timber, plastics) is unique reproducible green, environment-friendly materials.And since timber is excellent
Different natural characteristic, the deep favor by people.
But wood-based product is inflammable, is calamity source and the communication media of a variety of fire.Not only daily life is brought
Potential danger, and timber is limited in the application in many fields.Fire-retardant fireproof is the important of relationship people life property safety
Project.In various disasters, fire is most frequently, most generally threatens one of public security and the major casualty of social development.
It is counted according to the Fire Department of Ministry of Public Security, 2015, the whole nation is informed of a case fire 33.8 ten thousand altogether, causes 1742 people death, 1112 people injured, directly
Connect 39.5 hundred million yuan of property loss.On May 25th, 2015, Pingdingshan City, Henan Province Lushan County health and happiness garden apartment for elderly people occur especially heavy
Conflagration accident causes 39 people death, 6 people injured, 745.8 square metres of burnt area, 2064.5 ten thousand yuan of direct economic loss, makes
At extremely severe social influence.Casualties caused by the fire of room is especially heavy, home fire 11.1 ten thousand in 2015,
Cause 1213 people dead, although fire number only accounts for 32.9%, death toll accounting reaches 69.6%.Small fire causes high fire
Calamity is the universal law of room fire occurrence and development.Wood materials are largely used in house decoration, while displayying a large amount of wood
Matter furniture and fibre cause fire load in house very big, once fire occurs, will fiercely burn, and spread rapidly.System
Meter shows that wood materials are the principal combustible objects in house, and fire load calorific value ratio is more than 50%.Timber is not only inflammable,
And a large amount of thermal energy is released when burning, the mean calorie of timber is 18kJ/g, accelerates sprawling and the fire intensity of fire.Cause
This, the generation and sprawling of many fire are all related with wood materials.
Therefore, carrying out flame retardant treatment to inflammable timber fills it to improve and improve its certain timber feature
Divide, rationally, efficiently utilize, is to adapt to economic development requirement.Have existed since ancient times for fire-retarding of wood, but fire-retarding of wood research is existing not
Few problem.
The common fire retardant for the treatment of of wood industry, including inorganic based flame retardant and organic based flame retardant.Inorganic based flame retardant
Small toxicity, at low cost but easy precipitation, influence the final flame retardant effect of timber.In recent years, with sound, the Yi Jiren of regulation law
Environmental consciousness enhancing, intumescent organic fire-retardant has climbed up the arena of history, but common wood products are not belonging to high consumption product,
Fire retardant higher cost limits its extensive use.In addition, there is also destroy wood characteristics such as toughness, intensity.Timber
Fire-retardant research be a system engineering research, it includes the pretreatment (i.e. improvement permeability) of timber, fire retardant processing wood
Material and performance handle the problem of three aspects of re-dry of material.It includes coating and impregnating two methods that fire retardant, which handles timber,.By
In some natural defects of timber, such as there is pit blocking, exists and invade the disadvantages of filling out object, influence impregnating depth and fire retardant
Molecular diameter size, influence whether treatment fluid reaches in cell wall, can lasting factors such as fire-retardant.
Summary of the invention
Goal of the invention: mesh of the invention is to provide a kind of novel timber flame retardant composite material and preparation method thereof.
Technical solution: for achieving the above object, the present invention provides a kind of novel timber flame retardant composite materials, special
Sign is: being at least made of the components of following parts: 20-30 parts of the expanding flame-proof material of siliceous nitrogen phosphorus, aluminium hydroxide 10-
15 parts, 10-15 parts of antimony oxide, 5-10 parts of carboxymethyl cellulose, 3-8 parts of repefral, 1-2 parts of dispersing agent,
1.5-2 parts of defoaming agent, 0.5-1 parts of antioxidant, 30-50 parts of solvent naphtha, 5-15 parts of dimethicone,
Wherein, the structural formula of the expanding flame-proof material of siliceous nitrogen phosphorus are as follows:
In formula, integer of the n between 460-990；R is alkyl.
Preferably, the novel timber flame retardant composite material is at least made of the components of following parts: siliceous nitrogen phosphorus
It is 24-26 parts of expanding flame-proof material, 12-14 parts of aluminium hydroxide, 12-14 parts of antimony oxide, 6-8 parts of carboxymethyl cellulose, adjacent
4-6 parts of rutgers, 1-2 parts of dispersing agent, 1.5-2 parts of defoaming agent, 0.5-1 parts of antioxidant, 30-50 parts of solvent naphtha, two
8-12 parts of methyl-silicone oil.
Preferably, the novel timber flame retardant composite material is at least made of the components of following parts: siliceous nitrogen phosphorus
25 parts of expanding flame-proof material, 13 parts of aluminium hydroxide, 13 parts of antimony oxide, 7 parts of carboxymethyl cellulose, phthalic acid diformazan
5 parts of ester, 1.5 parts of dispersing agent, 1.7 parts of defoaming agent, 0.8 part of antioxidant, 40 parts of solvent naphtha, 10 parts of dimethicone.
Preferably, integer of the n between 590-800；R is selected from methyl, ethyl, propyl and isopropyl.
The present invention also provides the preparation methods of above-mentioned novel timber flame retardant composite material, comprising the following steps:
(1) preparation of the expanding flame-proof material of siliceous nitrogen phosphorus shown in Formulas I:
(1.1) in the protection of inert gas, under room temperature, chlorosilane and dimethyl phosphonate are reacted, alkyl silicon is made
Base dimethyl phosphonate；
(1.2) at the protection of inert gas, 350~400 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate
It is reacted under the action of catalyst with melamine, is cooled to 300 DEG C；
(1.3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 1-3h, it is cooling,
It is dried in vacuo to obtain the final product；
(2) preparation of novel timber flame retardant composite material: raw material is weighed by formula ratio；By dispersing agent, defoaming agent, antioxygen
Agent, dimethicone sequentially add in solvent naphtha, mix, obtain in mixed liquor；By expanding flame-proof material, the hydrogen-oxygen of siliceous nitrogen phosphorus
Change aluminium, antimony oxide, carboxymethyl cellulose, repefral to crush respectively, sequentially add in mixed liquor, mixes,
To obtain the final product.
In step (1.1), the chlorosilane is selected from trim,ethylchlorosilane, chlorotriethyl silane, tripropyl chlorosilane, diformazan
Base ethyl chlorosilane, dimethyl propyl chlorosilane and diethylmethyl chlorosilane；Mole of the chlorosilane and dimethyl phosphonate
Than being 1: (3~4)；Reaction time is 2-4h；The solvent that dimethyl phosphonate is reacted with chlorosilane is selected from methylene chloride, chloroform and third
Ketone.
In step (1.2), catalyst is selected from one or more of anhydrous magnesium chloride, triphenyl phosphate, triethylamine；Step
(1) molar ratio of gains alkyl silyl dimethyl phosphonate and melamine is 1: (1~1.2)；Reaction time is 3-5h.
In step (1.3), the dosage of ammeline is 1-1.2 times of melamine, in terms of molal quantity.
The utility model has the advantages that the present invention provides, fire proofing molecular weight is big, thermal stability is good, with solvent naphtha and other macromolecule materials
There is preferable compatibility between material, combined with other compositions and prepare fireproof coating etc., is not easy to be precipitated；Contain organosilicon knot in molecule
Structure, has good at charcoal effect, and when burning will form the inorganic oxygen barrier heat-insulating protective layer of silicon oxygen or silicon-carbon bonds, both organize to burn
Decomposition product leaks, and inhibits further thermal decomposition；Nitrogenous and phosphorus in molecular structure can play the work of coagulating agent in burning
With in carbide surface formation protective film, isolation air；The fire proofing synthesis technology is simple, and raw material is cheap and easy to get, Neng Gouyi
In large-scale production.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the present invention
Protection scope.
Embodiment 1
The preparation method of the expanding flame-proof material of siliceous nitrogen phosphorus, includes the following steps:
(1) in the protection of inert gas, under room temperature, the solvent of reaction is methylene chloride, by chlorosilane and phosphonic acids two
Methyl esters reacts 3h, and alkyl silyl dimethyl phosphonate is made；The chlorosilane is trim,ethylchlorosilane；The chlorosilane and phosphonic acids two
The molar ratio of methyl esters is 1: 3.5；
(2) at the protection of inert gas, 370 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate and melamine
Amine reacts 4h under anhydrous magnesium chloride effect, is cooled to 300 DEG C；Step (1) gains alkyl silyl dimethyl phosphonate and trimerization
The molar ratio of cyanamide is 1: 1.1；
Sampling, washing, drying and crushing, the product degree of polymerization 750,1% thermal weight loss decomposition temperature are 247.6 DEG C.
(3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 2h, cooling, vacuum
It is drying to obtain；The dosage of ammeline is 1.1 times of melamine, in terms of molal quantity.
Washing, drying and crushing are 269.5 to get the fire proofing, the degree of polymerization 750,1% thermal weight loss decomposition temperature
℃。
Embodiment 2
The preparation method of the expanding flame-proof material of siliceous nitrogen phosphorus, includes the following steps:
(1) in the protection of inert gas, under room temperature, the solvent of reaction is methylene chloride, by chlorosilane and phosphonic acids two
Methyl esters reacts 3h, and alkyl silyl dimethyl phosphonate is made；The chlorosilane is chlorotriethyl silane；The chlorosilane and phosphonic acids two
The molar ratio of methyl esters is 1: 3；
(2) at the protection of inert gas, 350 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate and melamine
Amine reacts 4h under anhydrous magnesium chloride effect, is cooled to 300 DEG C；Step (1) gains alkyl silyl dimethyl phosphonate and trimerization
The molar ratio of cyanamide is 1: 1.1.
Sampling, washing, drying and crushing, the product degree of polymerization 990,1% thermal weight loss decomposition temperature are 235.7 DEG C.
(3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 2h, cooling, vacuum
It is drying to obtain；The dosage of ammeline is 1.1 times of melamine, in terms of molal quantity.
Washing, drying and crushing are 258.4 to get the fire proofing, the degree of polymerization 990,1% thermal weight loss decomposition temperature
℃。
Embodiment 3
The preparation method of the expanding flame-proof material of siliceous nitrogen phosphorus, includes the following steps:
(1) in the protection of inert gas, under room temperature, the solvent of reaction is chloroform, by chlorosilane and dimethyl phosphonate
2h is reacted, alkyl silyl dimethyl phosphonate is made；The chlorosilane is tripropyl chlorosilane；The chlorosilane and dimethyl phosphonate
Molar ratio be 1: 4；
(2) at the protection of inert gas, 350 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate and melamine
Amine reacts 3h under triphenyl phosphate effect, is cooled to 300 DEG C；Step (1) gains alkyl silyl dimethyl phosphonate and trimerization
The molar ratio of cyanamide is 1: 1.1.
Sampling, washing, drying and crushing, the product degree of polymerization 800,1% thermal weight loss decomposition temperature are 237.6 DEG C.
(3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 3h, cooling, vacuum
It is drying to obtain；The dosage of ammeline is 1 times of melamine, in terms of molal quantity.
Washing, drying and crushing are 257.5 to get the fire proofing, the degree of polymerization 800,1% thermal weight loss decomposition temperature
℃。
Embodiment 4
The preparation method of the expanding flame-proof material of siliceous nitrogen phosphorus, includes the following steps:
(1) in the protection of inert gas, under room temperature, the solvent of reaction is acetone, by chlorosilane and dimethyl phosphonate
2h is reacted, alkyl silyl dimethyl phosphonate is made；The chlorosilane is dimethyl ethyl chlorosilane；The chlorosilane and phosphonic acids two
The molar ratio of methyl esters is 1: 3.2；
(2) at the protection of inert gas, 360 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate and melamine
Amine reacts 3h under triphenyl phosphate effect, is cooled to 300 DEG C；Step (1) gains alkyl silyl dimethyl phosphonate and trimerization
The molar ratio of cyanamide is 1: 1.
Sampling, washing, drying and crushing, the product degree of polymerization 460,1% thermal weight loss decomposition temperature are 219.1 DEG C.
(3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 3h, cooling, vacuum
It is drying to obtain；The dosage of ammeline is 1 times of melamine, in terms of molal quantity.
Washing, drying and crushing are 253.6 to get the fire proofing, the degree of polymerization 460,1% thermal weight loss decomposition temperature
℃。
Embodiment 5
The preparation method of the expanding flame-proof material of siliceous nitrogen phosphorus, includes the following steps:
(1) in the protection of inert gas, under room temperature, the solvent of reaction is acetone, by chlorosilane and dimethyl phosphonate
4h is reacted, alkyl silyl dimethyl phosphonate is made；The chlorosilane is diethylmethyl chlorosilane；The chlorosilane and phosphonic acids two
The molar ratio of methyl esters is 1: 3.8；
(2) at the protection of inert gas, 390 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate and melamine
Amine reacts 5h under triethylamine effect, is cooled to 300 DEG C；Step (1) gains alkyl silyl dimethyl phosphonate and melamine
Molar ratio be 1: 1.2.
Sampling, washing, drying and crushing, the product degree of polymerization 680,1% thermal weight loss decomposition temperature are 231.2 DEG C.
(3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 1h, cooling, vacuum
It is drying to obtain；The dosage of ammeline is 1.2 times of melamine, in terms of molal quantity.
Washing, drying and crushing are 259.4 to get the fire proofing, the degree of polymerization 680,1% thermal weight loss decomposition temperature
℃。
Embodiment 6
The preparation method of the expanding flame-proof material of siliceous nitrogen phosphorus, includes the following steps:
(1) in the protection of inert gas, under room temperature, the solvent of reaction is acetone, by chlorosilane and dimethyl phosphonate
4h is reacted, alkyl silyl dimethyl phosphonate is made；The chlorosilane is dimethyl propyl chlorosilane；The chlorosilane and phosphonic acids two
The molar ratio of methyl esters is 1: 3.5；
(2) at the protection of inert gas, 380 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate and melamine
Amine reacts 5h under triethylamine effect, is cooled to 300 DEG C；Step (1) gains alkyl silyl dimethyl phosphonate and melamine
Molar ratio be 1: 1.1.
Sampling, washing, drying and crushing, the product degree of polymerization 590,1% thermal weight loss decomposition temperature are 229.0 DEG C.
(3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 1h, cooling, vacuum
It is drying to obtain；The dosage of ammeline is 1.2 times of melamine, in terms of molal quantity.
Washing, drying and crushing are 260.2 to get the fire proofing, the degree of polymerization 590,1% thermal weight loss decomposition temperature
℃。
Novel timber flame retardant composite material, method are prepared using the expanding flame-proof material of the siliceous nitrogen phosphorus of embodiment 1 to 6
It is as follows: to weigh raw material by formula ratio；Dispersing agent, defoaming agent, antioxidant, dimethicone are sequentially added in solvent naphtha, mixed,
It obtains in mixed liquor；By the expanding flame-proof material of siliceous nitrogen phosphorus, aluminium hydroxide, antimony oxide, carboxymethyl cellulose, adjacent benzene two
Formic acid dimethyl ester crushes respectively, sequentially adds in mixed liquor, mix to get.
A batch composite material is made, component is as follows:
Composite material 1: it is made of the components of following parts: the expanding flame-proof material 25 of the siliceous nitrogen phosphorus of embodiment 1
Part, 13 parts of aluminium hydroxide, 13 parts of antimony oxide, 7 parts of carboxymethyl cellulose, 5 parts of repefral, dispersing agent 1.5
Part, 1.7 parts of defoaming agent, 0.8 part of antioxidant, 40 parts of solvent naphtha, 10 parts of dimethicone.
Composite material 2: it is made of the components of following parts: the expanding flame-proof material 25 of the siliceous nitrogen phosphorus of embodiment 2
Part, 13 parts of aluminium hydroxide, 13 parts of antimony oxide, 7 parts of carboxymethyl cellulose, 5 parts of repefral, dispersing agent 1.5
Part, 1.7 parts of defoaming agent, 0.8 part of antioxidant, 40 parts of solvent naphtha, 10 parts of dimethicone.
Composite material 3: it is made of the components of following parts: the expanding flame-proof material 24 of the siliceous nitrogen phosphorus of embodiment 3
Part, 12 parts of aluminium hydroxide, 14 parts of antimony oxide, 6 parts of carboxymethyl cellulose, 6 parts of repefral, 1 part of dispersing agent,
1.5 parts of defoaming agent, 0.5 part of antioxidant, 50 parts of solvent naphtha, 8 parts of dimethicone.
Composite material 4: it is made of the components of following parts: the expanding flame-proof material 26 of the siliceous nitrogen phosphorus of embodiment 4
Part, 14 parts of aluminium hydroxide, 12 parts of antimony oxide, 8 parts of carboxymethyl cellulose, 4 parts of repefral, 2 parts of dispersing agent,
2 parts of defoaming agent, 1 part of antioxidant, 30 parts of solvent naphtha, 2 parts of dimethicone.
Composite material 5: it is made of the components of following parts: the expanding flame-proof material 20 of the siliceous nitrogen phosphorus of embodiment 5
Part, 10 parts of aluminium hydroxide, 10 parts of antimony oxide, 5 parts of carboxymethyl cellulose, 8 parts of repefral, 2 parts of dispersing agent,
2 parts of defoaming agent, 0.5 part of antioxidant, 30 parts of solvent naphtha, 5 parts of dimethicone.
Composite material 6: it is made of the components of following parts: the expanding flame-proof material 30 of the siliceous nitrogen phosphorus of embodiment 6
Part, 15 parts of aluminium hydroxide, 15 parts of antimony oxide, 10 parts of carboxymethyl cellulose, 3 parts of repefral, dispersing agent 1
Part, 1.5 parts of defoaming agent, 1 part of antioxidant, 50 parts of solvent naphtha, 15 parts of dimethicone.
Timber sample is respectively placed in the composite material of composite material 1 to 6 immersion treatment for 24 hours, and carries out combustion experiment,
In 12 seconds, untreated timber sample burning reaches 65% or more, and uses the combustion of the composite material processing of composite material 1 to 6
Burning degree is respectively as follows:
Claims (8)
1. a kind of novel timber flame retardant composite material, it is characterised in that: be at least made of the components of following parts: siliceous nitrogen phosphorus
20-30 parts of expanding flame-proof material, 10-15 parts of aluminium hydroxide, 10-15 parts of antimony oxide, 5-10 parts of carboxymethyl cellulose,
3-8 parts of repefral, 1-2 parts of dispersing agent, 1.5-2 parts of defoaming agent, 0.5-1 parts of antioxidant, 30-50 parts of solvent naphtha,
5-15 parts of dimethicone,
Wherein, the structural formula of the expanding flame-proof material of siliceous nitrogen phosphorus are as follows:
In formula, integer of the n between 460-990；R is alkyl.
2. a kind of novel timber flame retardant composite material according to claim 1, it is characterised in that: at least by following parts by weight
Component be made: 24-26 parts of the expanding flame-proof material of siliceous nitrogen phosphorus, 12-14 parts of aluminium hydroxide, 12-14 parts of antimony oxide,
6-8 parts of carboxymethyl cellulose, 4-6 parts of repefral, 1-2 parts of dispersing agent, 1.5-2 parts of defoaming agent, antioxidant 0.5-1
Part, 30-50 parts of solvent naphtha, 8-12 parts of dimethicone.
3. a kind of novel timber flame retardant composite material according to claim 1, it is characterised in that: at least by following parts by weight
Component be made: 25 parts of the expanding flame-proof material of siliceous nitrogen phosphorus, 13 parts of aluminium hydroxide, 13 parts of antimony oxide, carboxymethyl is fine
7 parts of dimension element, 5 parts of repefral, 1.5 parts of dispersing agent, 1.7 parts of defoaming agent, 0.8 part of antioxidant, 40 parts of solvent naphtha, two
10 parts of methyl-silicone oil.
4. a kind of novel timber flame retardant composite material according to claim 1, it is characterised in that: n is between 590-800
Integer；R is selected from methyl, ethyl, propyl and isopropyl.
5. a kind of preparation method of novel timber flame retardant composite material described in Claims 1-4, it is characterised in that: including with
Lower step:
(1) preparation of the expanding flame-proof material of siliceous nitrogen phosphorus shown in Formulas I:
(1.1) in the protection of inert gas, under room temperature, chlorosilane and dimethyl phosphonate are reacted, alkyl silyl phosphine is made
Dimethyl phthalate；
(1.2) at the protection of inert gas, 350~400 DEG C, by step (1) gains alkyl silyl dimethyl phosphonate and three
Poly cyanamid reacts under the action of catalyst, is cooled to 300 DEG C；
(1.3) 250 DEG C are cooled to the speed of 10 DEG C/h, while ammeline is added；Constant temperature 1-3h, cooling, vacuum
It is drying to obtain；
(2) preparation of novel timber flame retardant composite material: raw material is weighed by formula ratio；By dispersing agent, defoaming agent, antioxidant, two
Methyl-silicone oil sequentially adds in solvent naphtha, mixes, obtains in mixed liquor；By the expanding flame-proof material of siliceous nitrogen phosphorus, aluminium hydroxide,
Antimony oxide, carboxymethyl cellulose, repefral crush respectively, sequentially add in mixed liquor, mix to get.
6. a kind of preparation method of novel timber flame retardant composite material according to claim 5, it is characterised in that: step
(1.1) in, the chlorosilane is selected from trim,ethylchlorosilane, chlorotriethyl silane, tripropyl chlorosilane, dimethyl ethyl chlorine silicon
Alkane, dimethyl propyl chlorosilane and diethylmethyl chlorosilane；The molar ratio of the chlorosilane and dimethyl phosphonate is 1: (3~
4)；Reaction time is 2-4h；The solvent that dimethyl phosphonate is reacted with chlorosilane is selected from methylene chloride, chloroform and acetone.
7. a kind of preparation method of novel timber flame retardant composite material according to claim 5, it is characterised in that: step
(1.2) in, catalyst is selected from one or more of anhydrous magnesium chloride, triphenyl phosphate, triethylamine；Step (1) gains alkane
The molar ratio of base silicon substrate dimethyl phosphonate and melamine is 1: (1~1.2)；Reaction time is 3-5h.
8. a kind of preparation method of novel timber flame retardant composite material according to claim 5, it is characterised in that: step
(1.3) in, the dosage of ammeline is 1-1.2 times of melamine, in terms of molal quantity.
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