CN107973885A - Tough fire retardant agent and preparation method thereof - Google Patents
Tough fire retardant agent and preparation method thereof Download PDFInfo
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- CN107973885A CN107973885A CN201711451353.3A CN201711451353A CN107973885A CN 107973885 A CN107973885 A CN 107973885A CN 201711451353 A CN201711451353 A CN 201711451353A CN 107973885 A CN107973885 A CN 107973885A
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- retardant agent
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 64
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229920005610 lignin Polymers 0.000 claims abstract description 95
- 239000011347 resin Substances 0.000 claims abstract description 59
- 229920005989 resin Polymers 0.000 claims abstract description 59
- 239000000376 reactant Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229940117958 vinyl acetate Drugs 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000012662 bulk polymerization Methods 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 69
- 238000005406 washing Methods 0.000 claims description 35
- 238000001914 filtration Methods 0.000 claims description 31
- 239000006166 lysate Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 239000003513 alkali Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000011065 in-situ storage Methods 0.000 claims description 12
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 claims 1
- UQXKXGWGFRWILX-UHFFFAOYSA-N ethylene glycol dinitrate Chemical compound O=N(=O)OCCON(=O)=O UQXKXGWGFRWILX-UHFFFAOYSA-N 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 abstract description 3
- 238000007334 copolymerization reaction Methods 0.000 abstract description 3
- 239000012153 distilled water Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 235000019400 benzoyl peroxide Nutrition 0.000 description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- -1 glycol dimethyl ethers Chemical class 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- PVEOYINWKBTPIZ-UHFFFAOYSA-N but-3-enoic acid Chemical class OC(=O)CC=C PVEOYINWKBTPIZ-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920002689 polyvinyl acetate Polymers 0.000 description 4
- 239000011118 polyvinyl acetate Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 239000003607 modifier Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- PGLOXGDCEWLIQB-UHFFFAOYSA-N 3-hydroxyprop-1-enyl acetate Chemical group C(C)(=O)OC=CCO PGLOXGDCEWLIQB-UHFFFAOYSA-N 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229920002988 biodegradable polymer Polymers 0.000 description 1
- 239000004621 biodegradable polymer Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000010893 paper waste Substances 0.000 description 1
- VWSUVZVPDQDVRT-UHFFFAOYSA-N phenylperoxybenzene Chemical compound C=1C=CC=CC=1OOC1=CC=CC=C1 VWSUVZVPDQDVRT-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application provides a kind of tough fire retardant agent and preparation method thereof, which comprises the following steps：The modified lignin resin of initiator, the vinylacetate of 100 mass parts and 2~25 mass parts is mixed, reaction, obtains reactant；The reactant is purified, obtains tough fire retardant agent.The preparation method of above-mentioned tough fire retardant agent, it was bulk polymerization originally that vinylacetate occurs with modified lignin resin, free radicals copolymerization reaction occurs using the C=C keys in modified lignin resin and vinylacetate, generate tough fire retardant agent, since modified lignin resin has well into carbon in combustion, material can be prevented to burn away, therefore, the tough fire retardant agent of generation has good anti-flammability, it may be used as high molecular material fire retardant, the application field of lignin is expanded, improves the utilization rate of lignin.
Description
Technical field
The present invention relates to biodegradable polymer technical field, more particularly to tough fire retardant agent and its preparation side
Method
Background technology
Lignin is a kind of degradable environmental-friendly resource, is mainly derived from the waste water of industrial pulping and paper-making.The whole world is every
Year as accessory substance generation lignin utilization rate less than 5%, most of to be all discharged into as fertilizer in the Nature, not only dirt
Environment is contaminated, wastes resource.Therefore, the application field of lignin how is expanded, improving the utilization rate of lignin becomes research
The problem that person becomes more concerned with.
Lignin is modified, assigns lignin new function, it is to realize then to prepare new material using modified lignin resin
Expand lignin application field, improve the effective way of lignin utilization rate.
The content of the invention
Based on this, it is necessary to provide a kind of tough fire retardant agent prepared using modified lignin resin.
In addition, the application also provides a kind of preparation method of above-mentioned tough fire retardant agent.
A kind of preparation method of tough fire retardant agent, comprises the following steps：
The modified lignin resin of initiator, the vinylacetate of 100 mass parts and 2~25 mass parts is mixed, is occurred in situ
Bulk polymerization, obtains reactant；
The reactant is purified, obtains the tough fire retardant agent.
In one of the embodiments, the initiator is dibenzoyl peroxide or azodiisobutyronitrile.
In one of the embodiments, the dosage of the initiator is the vinylacetate and modified lignin resin gross mass
0.5%~1%.
In one of the embodiments, the modified lignin resin is prepared by following methods：
The maleic anhydride of glycol dimethyl ether, the alkali lignin of 100 mass parts and 10~50 mass parts is mixed, at 80 DEG C
When~90 DEG C of reactions 2~8 are small, cooling, filtering, washing, obtain thick modified lignin resin；
The thick modified lignin resin and methanol are mixed, dissolved 30 minutes at 50 DEG C~80 DEG C, cooling, filtering, washing, obtain
To filtrate；
The solid that the filtrate is distilled is mixed with water, filtering, washing, drying, obtain the modified lignin resin.
In one of the embodiments, the dosage of the relatively described alkali lignin of the glycol dimethyl ether is 4~5ml/g alkali
Lignin.
In one of the embodiments, the reaction temperature that bulk polymerization in situ occurs is 60 DEG C~100 DEG C, instead
When being 2~8 small between seasonable.
In one of the embodiments, the reaction temperature that bulk polymerization in situ occurs is 70 DEG C~90 DEG C, instead
When being 4~6 small between seasonable.
In one of the embodiments, the step of reactant being purified, obtaining the tough fire retardant agent be specially：Will
Reactant and the methanol mixing, in 60 DEG C of stirrings to being completely dissolved, obtains lysate；
The lysate is mixed with water, filtering, washing, drying, obtain the tough fire retardant agent.
In one of the embodiments, the dosage of the methanol is 2.5~3.5 times of the reactant quality.
Tough fire retardant agent prepared by a kind of preparation method of tough fire retardant agent using described in any of the above-described.
With modified lignin resin bulk polymerization in situ occurs for the preparation method of above-mentioned tough fire retardant agent, vinylacetate,
Free radicals copolymerization reaction occurs using the C=C keys in modified lignin resin and vinylacetate, tough fire retardant agent is generated, due to changing
Property lignin in combustion have well into carbon, material can be prevented to burn away, therefore, the tough fire retardant agent of generation
With good anti-flammability, high molecular material fire retardant is may be used as, the application field of lignin is expanded, improves lignin
Utilization rate.
In addition, what vinylacetate formed on tough fire retardant agent molecule chain is unformed high-elastic molecule segment, therefore,
Above-mentioned tough fire retardant agent also has good toughness.
Embodiment
For the ease of understand the present invention, the present invention will be described more fully below, and give the present invention compared with
Good embodiment.But the present invention can realize in many different forms, however it is not limited to embodiment described herein.Phase
Instead, there is provided the purpose of these embodiments is the understanding more thorough and comprehensive made to the disclosure.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The normally understood implication of technical staff is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
The arbitrary and all combination of the Listed Items of pass.
The preparation method of the tough fire retardant agent of one embodiment, comprises the following steps S110~S120：
S110, the modified lignin resin mixing by initiator, the vinylacetate of 100 mass parts and 2~25 mass parts, occur
Bulk polymerization in situ, obtains reactant.
Wherein, the reaction temperature that bulk polymerization in situ occurs is 60 DEG C~100 DEG C.Preferably, body in situ occurs
The reaction temperature of polymerisation is 70 DEG C~90 DEG C.
When the reaction time that bulk polymerization in situ occurs is 2~8 small.Preferably, bulk polymerization in situ occurs
Reaction time for 4~6 it is small when.
Further, the dosage of initiator is the 0.5%~1% of vinylacetate and modified lignin resin gross mass.
Preferably, the dosage of initiator is the 0.6%~0.8% of vinylacetate and modified lignin resin gross mass.
Further, initiator is dibenzoyl peroxide (BPO) or azodiisobutyronitrile (AIBN).
Further, the vinylacetate of vinylacetate purification.
Further, modified lignin resin is prepared by following methods：
(1) maleic anhydride of glycol dimethyl ether, the alkali lignin of 100 mass parts and 10~50 mass parts is mixed,
When 80 DEG C~90 DEG C reactions 2~8 are small, cooling, filtering, washing, obtain thick modified lignin resin.
Wherein, alkali lignin comes from commercial paper waste liquid, is utilized, and not only reduces above-mentioned modified polyvinylalcohol material
The production cost of material, also expands the application field of lignin, reduces pollution of the papermaking wastewater to environment.
Preferably, alkali lignin is dry alkali lignin.
Further, glycol dimethyl ether is 4~5ml/g alkali lignins with respect to the dosage of alkali lignin.
(2) the thick modified lignin resin and methanol are mixed, is dissolved 30 minutes at 50 DEG C~80 DEG C, cooling, filtering, washing,
Obtain filtrate.
(3) solid that the filtrate is distilled is mixed with water, filtering, washing, drying, obtain modified lignin resin.
Specifically, the solid which distilled is added in distilled water, and quick stirring 2 minutes, filtering, wash, is dry
It is dry, obtain modified lignin resin.
Self-catalysis occurs in glycol dimethyl ether for the preparation method of above-mentioned modified lignin resin, alkali lignin and maleic anhydride
Ring-opening reaction is acted on, is generated in reaction process without small-molecule substance.
S120, purify the reactant, obtains tough fire retardant agent.
Specifically, the reactant and methanol are mixed, in 60 DEG C of stirrings to being completely dissolved, obtains lysate；
The lysate is mixed with water, filtering, washing, drying, obtain tough fire retardant agent.
Wherein, the dosage of methanol is 2.5~3.5 times of reactant quality.
It should be noted that the dosage of methanol is not limited to 2.5~3.5 times of the reactant quality that present embodiment is enumerated,
As long as reactant can be dissolved.
With modified lignin resin bulk polymerization in situ occurs for the preparation method of above-mentioned tough fire retardant agent, vinylacetate,
Free radicals copolymerization reaction occurs using the C=C keys in modified lignin resin and vinylacetate, tough fire retardant agent is generated, due to changing
Property lignin in combustion have well into carbon, material can be prevented to burn away, therefore, the tough fire retardant agent of generation
With good anti-flammability, high molecular material fire retardant is may be used as, the application field of lignin is expanded, improves lignin
Utilization rate.
In addition, what vinylacetate formed on tough fire retardant agent molecule chain is unformed high-elastic molecule segment, therefore,
Above-mentioned tough fire retardant agent also has good toughness.
Further, due to containing the various polarity groups such as carboxyl, hydroxyl, methylol, vinyl acetate in modified lignin resin
Also ester group is contained in ester, therefore, above-mentioned tough fire retardant agent is while with fire retardation, moreover it is possible to is used as compatilizer.
Further, due to containing rigid radical phenyl in modified lignin resin, heat endurance is good, therefore, above-mentioned fire retardant
It is also used as polymer heat resistance modifier.
Further, since the tough fire retardant agent of the application is amorphous macromolecule material, at a lower temperature with regard to energy
Softening, and then flow, and since containing a large amount of different types of polar groups, other corresponding polarity or nonpolar can be driven
Sub-chain motion, therefore the tough fire retardant agent of the application can also do Process Technology of Polymer flow ability modifying agent.
Further, since modified lignin resin is a kind of degradable environment friendly material, it is introduced into and enhances tough fire retardant
The degradability of agent, meets the requirement of national green economic development.
The preparation method of above-mentioned tough fire retardant agent, technique is simple, environmentally protective, low production cost, and production efficiency is high, easily
Industrialized in realizing.
In addition, also act as toughener, heat-proof modifier, compatilizer, height using tough fire retardant agent prepared by the above method
The processing aids such as molecular material processing flow ability modifying agent.
It is specific embodiment below.
Embodiment 1
(1) modified lignin resin is prepared：The alkali lignin of 100g, the maleic anhydride of 10g and 400ml glycol dimethyl ethers are mixed
Close, when 80 DEG C of reactions 2 are small, cooling, filtering, washing, obtain thick modified lignin resin.The thick modified lignin resin and methanol are mixed
Close, dissolved 30 minutes at 50 DEG C, cooling, filtering, washing, obtain filtrate.The solid that the filtrate is distilled is mixed with water, mistake
Filter, washing, drying, obtain modified lignin resin.
(2) tough fire retardant agent is prepared：By two isobutyl of azo of the vinylacetate of 50g, the modified lignin resin of 1g and 0.51g
Nitrile mixes, and when 70 DEG C of reactions 6 are small, obtains reactant.The reactant is added in 158g methanol, is stirred at 60 DEG C to completely molten
Solution, obtains lysate.The lysate is poured into distilled water, filtering, washing, drying, obtain 31.2g tough fire retardant agent.
Embodiment 2
(1) modified lignin resin is prepared：The alkali lignin of 100g, the maleic anhydride of 50g and 500ml glycol dimethyl ethers are mixed
Close, when 90 DEG C of reactions 8 are small, cooling, filtering, washing, obtain thick modified lignin resin.The thick modified lignin resin and methanol are mixed
Close, dissolved 30 minutes at 80 DEG C, cooling, filtering, washing, obtain filtrate.The solid that the filtrate is distilled is mixed with water, mistake
Filter, washing, drying, obtain modified lignin resin.
(2) tough fire retardant agent is prepared：50g vinylacetates, 4g modified lignin resins and 0.432g azodiisobutyronitriles are mixed
Close, when 68 DEG C of reactions 4 are small, obtain reactant.The reactant is added in 165g methanol, in 60 DEG C of stirrings to being completely dissolved,
Obtain lysate.The lysate is poured into distilled water, filtering, washing, drying, obtain 36.6g tough fire retardant agent.
Embodiment 3
(1) modified lignin resin is prepared：The alkali lignin of 100g, the maleic anhydride of 20g and 450ml glycol dimethyl ethers are mixed
Close, when 85 DEG C of reactions 5 are small, cooling, filtering, washing, obtain thick modified lignin resin.The thick modified lignin resin and methanol are mixed
Close, dissolved 30 minutes at 75 DEG C, cooling, filtering, washing, obtain filtrate.The solid that the filtrate is distilled is mixed with water, mistake
Filter, washing, drying, obtain modified lignin resin.
(2) tough fire retardant agent is prepared：By 50g vinylacetates, 9g modified lignin resins and 0.354g dibenzoyl peroxides
Mixing, when 90 DEG C of reactions 8 are small, obtains reactant.The reactant is added in 165g methanol, is stirred at 60 DEG C to completely molten
Solution, obtains lysate.The lysate is poured into distilled water, filtering, washing, drying, obtain 41.3g tough fire retardant agent.
Embodiment 4
(1) modified lignin resin is prepared：The alkali lignin of 100g, the maleic anhydride of 30g and 480ml glycol dimethyl ethers are mixed
Close, when 85 DEG C of reactions 6 are small, cooling, filtering, washing, obtain thick modified lignin resin.The thick modified lignin resin and methanol are mixed
Close, dissolved 30 minutes at 75 DEG C, cooling, filtering, washing, obtain filtrate.The solid that the filtrate is distilled is mixed with water, mistake
Filter, washing, drying, obtain modified lignin resin.
(2) tough fire retardant agent is prepared：By 50g vinylacetates, 7.25g modified lignin resins and 0.46g diphenyl peroxide first
Acyl mixes, and when 95 DEG C of reactions 6 are small, obtains reactant.The reactant is added in 170g methanol, is stirred at 60 DEG C to completely molten
Solution, obtains lysate.The lysate is poured into distilled water, filtering, washing, drying, obtain 39.5g tough fire retardant agent.
Embodiment 5
(1) modified lignin resin is prepared：The alkali lignin of 100g, the maleic anhydride of 40g and 500ml glycol dimethyl ethers are mixed
Close, when 85 DEG C of reactions 7 are small, cooling, filtering, washing, obtain thick modified lignin resin.The thick modified lignin resin and methanol are mixed
Close, dissolved 30 minutes at 75 DEG C, cooling, filtering, washing, obtain filtrate.The solid that the filtrate is distilled is mixed with water, mistake
Filter, washing, drying, obtain modified lignin resin.
(2) tough fire retardant agent is prepared：By 50g vinylacetates, 12.5g modified lignin resins and 0.313g azodiisobutyronitriles
Mixing, when 75 DEG C of reactions 8 are small, obtains reactant.The reactant is added in 180g methanol, is stirred at 60 DEG C to completely molten
Solution, obtains lysate.The lysate is poured into distilled water, filtering, washing, drying, obtain 41.6g tough fire retardant agent.
Comparative example 1
The azodiisobutyronitrile of the vinylacetate of 50g and 0.34g are mixed, when 70 DEG C of reactions 3 are small, reacted
Thing.The reactant is added in 160g methanol, in 60 DEG C of stirrings to being completely dissolved, obtains lysate.The lysate is poured into steaming
In distilled water, filtering, washing, drying, obtain 40.5g polyvinyl acetate.
Comparative example 2
The dibenzoyl peroxide of the vinylacetate of 50g and 0.40g are mixed, when 92 DEG C of reactions 5 are small, reacted
Thing.The reactant is added in 160g methanol, in 60 DEG C of stirrings to being completely dissolved, obtains lysate.The lysate is poured into steaming
In distilled water, filtering, washing, drying, obtain 39.7g polyvinyl acetate.
Comparative example 3
The dibenzoyl peroxide of the vinylacetate of 50g and 0.25g are mixed, when 95 DEG C of reactions 6 are small, reacted
Thing.The reactant is added in 160g methanol, in 60 DEG C of stirrings to being completely dissolved, obtains lysate.The lysate is poured into steaming
In distilled water, filtering, washing, drying, obtain 38.3g polyvinyl acetate.
Material prepared by embodiment 1~5 and comparative example 1~3 is subjected to oxygen index (OI) test respectively, the results are shown in Table 1.
1 oxygen index (OI) of table tests table
| Sample | LOI (%) |
| Embodiment 1 | 22.4 |
| Embodiment 2 | 24.1 |
| Embodiment 3 | 24.4 |
| Embodiment 4 | 26.2 |
| Embodiment 5 | 28.1 |
| Comparative example 1 | 18.6 |
| Comparative example 2 | 19.2 |
| Comparative example 3 | 19.0 |
As known from Table 1, the oxygen index (OI) of tough fire retardant agent prepared by embodiment 1~5 is prepared apparently higher than comparative example 1~3
Polyvinyl acetate, illustrating the tough fire retardant agent of the application has good anti-flammability, and having opened up one for lignin new makes
Use approach.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, its description is more specific and detailed, but simultaneously
Cannot therefore it be construed as limiting the scope of the patent.It should be pointed out that come for those of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of tough fire retardant agent, it is characterised in that comprise the following steps：
The modified lignin resin of initiator, the vinylacetate of 100 mass parts and 2~25 mass parts is mixed, body in situ occurs
Polymerisation, obtains reactant；
The reactant is purified, obtains the tough fire retardant agent.
2. the preparation method of tough fire retardant agent according to claim 1, it is characterised in that the initiator is peroxidating two
Benzoyl or azodiisobutyronitrile.
3. the preparation method of tough fire retardant agent according to claim 1, it is characterised in that the dosage of the initiator is institute
State the 0.5%~1% of vinylacetate and modified lignin resin gross mass.
4. the preparation method of tough fire retardant agent according to claim 1, it is characterised in that the modified lignin resin is by following
It is prepared by method：
The maleic anhydride of glycol dimethyl ether, the alkali lignin of 100 mass parts and 10~50 mass parts is mixed, 80 DEG C~90
DEG C reaction 2~8 it is small when, cooling, filtering, washing, obtain thick modified lignin resin；
The thick modified lignin resin and methanol are mixed, dissolved 30 minutes at 50 DEG C~80 DEG C, cooling, filtering, washing, are filtered
Liquid；
The solid that the filtrate is distilled is mixed with water, filtering, washing, drying, obtain the modified lignin resin.
5. the preparation method of modified polyvinylalcohol material according to claim 4, it is characterised in that the glycol dinitrate
The dosage of the relatively described alkali lignin of ether is 4~5ml/g alkali lignins.
6. according to the preparation method of Claims 1 to 5 any one of them tough fire retardant agent, it is characterised in that described that original occurs
The reaction temperature of position bulk polymerization is 60 DEG C~100 DEG C, when the reaction time is 2~8 small.
7. the preparation method of tough fire retardant agent according to claim 6, it is characterised in that described that polymerisation in bulk in situ occurs
The reaction temperature of reaction is 70 DEG C~90 DEG C, when the reaction time is 4~6 small.
8. according to the preparation method of Claims 1 to 5 any one of them tough fire retardant agent, it is characterised in that by the reaction
Thing purifies, and the step of obtaining the tough fire retardant agent is specially：The reactant and methanol are mixed, stirred at 60 DEG C to complete
Dissolving, obtains lysate；
The lysate is mixed with water, filtering, washing, drying, obtain the tough fire retardant agent.
9. the preparation method of tough fire retardant agent according to claim 8, it is characterised in that the dosage of the methanol is described
2.5~3.5 times of reactant quality.
A kind of 10. tough fire retardant agent prepared by preparation method using claim 1~9 any one of them tough fire retardant agent.
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| CN109503860A (en) * | 2018-12-13 | 2019-03-22 | 湖南绿燊环保科技有限公司 | Modified lignin resin for expansion type flame retardant and preparation method thereof, expansion type flame retardant and preparation method thereof |
| CN109593282A (en) * | 2018-12-12 | 2019-04-09 | 湖南绿燊环保科技有限公司 | For the fire retardant of polystyrene, fire retardant polystyrene material and preparation method thereof |
| CN110804119A (en) * | 2019-12-09 | 2020-02-18 | 怀化学院 | Modified polyvinyl alcohol and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109593282A (en) * | 2018-12-12 | 2019-04-09 | 湖南绿燊环保科技有限公司 | For the fire retardant of polystyrene, fire retardant polystyrene material and preparation method thereof |
| CN109593282B (en) * | 2018-12-12 | 2021-07-09 | 苏州博之顺材料科技有限公司 | Flame retardant for polystyrene, flame-retardant polystyrene material and preparation method thereof |
| CN109503860A (en) * | 2018-12-13 | 2019-03-22 | 湖南绿燊环保科技有限公司 | Modified lignin resin for expansion type flame retardant and preparation method thereof, expansion type flame retardant and preparation method thereof |
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