CN107973885B - Tough fire retardant agent and preparation method thereof - Google Patents
Tough fire retardant agent and preparation method thereof Download PDFInfo
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- CN107973885B CN107973885B CN201711451353.3A CN201711451353A CN107973885B CN 107973885 B CN107973885 B CN 107973885B CN 201711451353 A CN201711451353 A CN 201711451353A CN 107973885 B CN107973885 B CN 107973885B
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- retardant agent
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- modified lignin
- tough fire
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 66
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229920005610 lignin Polymers 0.000 claims abstract description 99
- 239000011347 resin Substances 0.000 claims abstract description 62
- 229920005989 resin Polymers 0.000 claims abstract description 62
- 239000000376 reactant Substances 0.000 claims abstract description 30
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229940117958 vinyl acetate Drugs 0.000 claims abstract description 26
- 238000012662 bulk polymerization Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction 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 72
- 239000006166 lysate Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000003513 alkali Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 17
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 13
- 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 10
- 238000000034 method Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 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 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000002023 wood Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 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
- 238000001035 drying Methods 0.000 description 5
- 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
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 229920000642 polymer Polymers 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
- 239000006227 byproduct 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
- 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
- 239000000126 substance Substances 0.000 description 1
- 239000012745 toughening agent 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, and for the preparation method the following steps are included: 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, tough fire retardant agent is obtained.The preparation method of above-mentioned tough fire retardant agent, vinylacetate and modified lignin resin generation are bulk polymerization originally, utilize the C=C key and vinylacetate generation free radicals copolymerization reaction in modified lignin resin, generate tough fire retardant agent, since modified lignin resin has well in combustion into carbon, 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 for expanding lignin improves the utilization rate of lignin.
Description
Technical field
The present invention relates to biodegradable polymer technical fields, more particularly to tough fire retardant agent and its preparation side
Method.
Background technique
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
The lignin utilization rate year generated as by-product is less than 5%, most of to be all discharged into the Nature as fertilizer, not only dirt
Environment is contaminated, resource is wasted.Therefore, the application field for how expanding lignin, the utilization rate for improving lignin become research
The project that person becomes more concerned with.
Lignin is modified, lignin new function is assigned, then preparing new material using modified lignin resin is to realize
The effective way for expanding lignin application field, improving lignin utilization rate.
Summary 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, comprising 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, the tough fire retardant agent is obtained.
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 in one of the embodiments,
0.5%~1%.
The modified lignin resin is prepared by following methods in one of the embodiments:
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
~90 DEG C are reacted 2~8 hours, cooling, are filtered, washed, are obtained thick modified lignin resin；
The thick modified lignin resin and methanol are mixed, dissolved 30 minutes at 50 DEG C~80 DEG C, it is cooling, it is filtered, washed, obtains
To filtrate；
The solid that the filtrate is distilled is mixed with water, is filtered, washed, dries, obtains the modified lignin resin.
The dosage of the relatively described alkali lignin of the glycol dimethyl ether is 4~5ml/g alkali in one of the embodiments,
Lignin.
The reaction temperature that bulk polymerization in situ occurs is 60 DEG C~100 DEG C in one of the embodiments, instead
It is 2~8 hours between seasonable.
The reaction temperature that bulk polymerization in situ occurs is 70 DEG C~90 DEG C in one of the embodiments, instead
It is 4~6 hours between seasonable.
The step of reactant is purified in one of the embodiments, obtains the tough fire retardant agent specifically: will
The reactant and methanol mixing obtain lysate in 60 DEG C of stirrings to being completely dissolved；
The lysate is mixed with water, is filtered, washed, dries, obtains the tough fire retardant agent.
The dosage of the methanol is 2.5~3.5 times of the reactant quality in one of the embodiments,.
A kind of tough fire retardant agent prepared by the preparation method using tough fire retardant agent described in any of the above embodiments.
Bulk polymerization in situ occurs for the preparation method of above-mentioned tough fire retardant agent, vinylacetate and modified lignin resin,
Using the C=C key and vinylacetate generation free radicals copolymerization reaction in modified lignin resin, tough fire retardant agent is generated, due to changing
Property lignin has well in combustion into carbon, and material can be prevented to burn away, therefore, the tough fire retardant agent of generation
With good anti-flammability, high molecular material fire retardant may be used as, expand the application field of lignin, improve lignin
Utilization rate.
In addition, vinylacetate formed on tough fire retardant agent molecule chain be amorphous high-elastic molecule segment, therefore,
Above-mentioned tough fire retardant agent also has good toughness.
Specific embodiment
To facilitate the understanding of the present invention, below will to invention is more fully described, and give it is of the invention compared with
Good embodiment.But the invention can be realized in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention 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
Any and all combinations of the listed item of pass.
The preparation method of the tough fire retardant agent of one embodiment, includes the following steps S110~S120:
S110, the modified lignin resin of initiator, the vinylacetate of 100 mass parts and 2~25 mass parts is mixed, is occurred
Bulk polymerization in situ, obtains reactant.
Wherein, the reaction temperature that bulk polymerization in situ occurs is 60 DEG C~100 DEG C.Preferably, ontology in situ occurs
The reaction temperature of polymerization reaction is 70 DEG C~90 DEG C.
The reaction time that bulk polymerization in situ occurs is 2~8 hours.Preferably, bulk polymerization in situ occurs
Reaction time be 4~6 hours.
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,
80 DEG C~90 DEG C are reacted 2~8 hours, cooling, are filtered, washed, are obtained thick modified lignin resin.
Wherein, alkali lignin is utilized from commercial paper waste liquid, not only reduces the life of above-mentioned tough fire retardant agent
Cost is produced, the application field of lignin is also expanded, reduces pollution of the papermaking wastewater to environment.
Preferably, alkali lignin is dry alkali lignin.
Further, glycol dimethyl ether is 4~5ml/g alkali lignin 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, it is cooling, it is filtered, washed,
Obtain filtrate.
(3) solid that the filtrate is distilled is mixed with water, is filtered, washed, dries, obtains modified lignin resin.
Specifically, the solid which distilled is added in distilled water, and quickly stirring 2 minutes, are filtered, washed, do
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, the reactant is purified, 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, is filtered, washed, dries, 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.
Bulk polymerization in situ occurs for the preparation method of above-mentioned tough fire retardant agent, vinylacetate and modified lignin resin,
Using the C=C key and vinylacetate generation free radicals copolymerization reaction in modified lignin resin, tough fire retardant agent is generated, due to changing
Property lignin has well in combustion into carbon, and material can be prevented to burn away, therefore, the tough fire retardant agent of generation
With good anti-flammability, high molecular material fire retardant may be used as, expand the application field of lignin, improve lignin
Utilization rate.
In addition, vinylacetate formed on tough fire retardant agent molecule chain be amorphous high-elastic molecule segment, therefore,
Above-mentioned tough fire retardant agent also has good toughness.
Further, due to containing the various polarities groups such as carboxyl, hydroxyl, methylol, vinyl acetate in modified lignin resin
Also contain ester group in ester, therefore, above-mentioned tough fire retardant agent is while with fire retardation, moreover it is possible to use as compatilizer.
Further, due to containing rigid radical phenyl in modified lignin resin, thermal stability 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 energy
Softening, and then flow, and due to being able to drive other corresponding polarity or nonpolar containing a large amount of different types of polar groups
Sub-chain motion, therefore the tough fire retardant agent of the application can also do Process Technology of Polymer flow ability modifying agent.
Further, it since modified lignin resin is a kind of degradable environment friendly material, 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, simple process is environmentally protective, low production cost, high production efficiency, easily
It is industrialized in realizing.
In addition, also acting as toughener, heat-proof modifier, compatilizer, height using tough fire retardant agent prepared by the above method
Molecular material processes the processing aids such as flow ability modifying agent.
The following are specific embodiments.
Embodiment 1
(1) it prepares modified lignin resin: the alkali lignin of 100g, the maleic anhydride of 10g and 400ml glycol dimethyl ether is mixed
It closes, is reacted 2 hours at 80 DEG C, it is cooling, it is filtered, washed, obtains thick modified lignin resin.The thick modified lignin resin and methanol are mixed
It closes, is dissolved 30 minutes at 50 DEG C, it is cooling, it is filtered, washed, obtains 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 mixing, reacts 6 hours at 70 DEG C, 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, is filtered, washed, dries, obtains 31.2g tough fire retardant agent.
Embodiment 2
(1) it prepares modified lignin resin: the alkali lignin of 100g, the maleic anhydride of 50g and 500ml glycol dimethyl ether is mixed
It closes, is reacted 8 hours at 90 DEG C, it is cooling, it is filtered, washed, obtains thick modified lignin resin.The thick modified lignin resin and methanol are mixed
It closes, is dissolved 30 minutes at 80 DEG C, it is cooling, it is filtered, washed, obtains filtrate.The solid that the filtrate is distilled is mixed with water, mistake
Filter, washing, drying, obtain modified lignin resin.
(2) it prepares tough fire retardant agent: 50g vinylacetate, 4g modified lignin resin and 0.432g azodiisobutyronitrile is mixed
It closes, is reacted 4 hours at 68 DEG C, 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, is filtered, washed, dries, obtains 36.6g tough fire retardant agent.
Embodiment 3
(1) it prepares modified lignin resin: the alkali lignin of 100g, the maleic anhydride of 20g and 450ml glycol dimethyl ether is mixed
It closes, is reacted 5 hours at 85 DEG C, it is cooling, it is filtered, washed, obtains thick modified lignin resin.The thick modified lignin resin and methanol are mixed
It closes, is dissolved 30 minutes at 75 DEG C, it is cooling, it is filtered, washed, obtains 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 vinylacetate, 9g modified lignin resin and 0.354g dibenzoyl peroxide
Mixing reacts 8 hours at 90 DEG C, 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, is filtered, washed, dries, obtains 41.3g tough fire retardant agent.
Embodiment 4
(1) it prepares modified lignin resin: the alkali lignin of 100g, the maleic anhydride of 30g and 480ml glycol dimethyl ether is mixed
It closes, is reacted 6 hours at 85 DEG C, it is cooling, it is filtered, washed, obtains thick modified lignin resin.The thick modified lignin resin and methanol are mixed
It closes, is dissolved 30 minutes at 75 DEG C, it is cooling, it is filtered, washed, obtains 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 vinylacetate, 7.25g modified lignin resin and 0.46g diphenyl peroxide first
Acyl mixing, reacts 6 hours at 95 DEG C, 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, is filtered, washed, dries, obtains 39.5g tough fire retardant agent.
Embodiment 5
(1) it prepares modified lignin resin: the alkali lignin of 100g, the maleic anhydride of 40g and 500ml glycol dimethyl ether is mixed
It closes, is reacted 7 hours at 85 DEG C, it is cooling, it is filtered, washed, obtains thick modified lignin resin.The thick modified lignin resin and methanol are mixed
It closes, is dissolved 30 minutes at 75 DEG C, it is cooling, it is filtered, washed, obtains 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 vinylacetate, 12.5g modified lignin resin and 0.313g azodiisobutyronitrile
Mixing reacts 8 hours at 75 DEG C, 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, is filtered, washed, dries, obtains 41.6g tough fire retardant agent.
Comparative example 1
The azodiisobutyronitrile of the vinylacetate of 50g and 0.34g are mixed, reacts 3 hours, is reacted at 70 DEG C
Object.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
It in distilled water, is filtered, washed, dries, obtain 40.5g polyvinyl acetate.
Comparative example 2
The dibenzoyl peroxide of the vinylacetate of 50g and 0.40g are mixed, reacts 5 hours, is reacted at 92 DEG C
Object.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
It in distilled water, is filtered, washed, dries, obtain 39.7g polyvinyl acetate.
Comparative example 3
The dibenzoyl peroxide of the vinylacetate of 50g and 0.25g are mixed, reacts 6 hours, is reacted at 95 DEG C
Object.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
It in distilled water, is filtered, washed, dries, obtain 38.3g polyvinyl acetate.
Material prepared by Examples 1 to 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 the tough fire retardant agent of Examples 1 to 5 preparation is apparently higher than the preparation of comparative example 1~3
Polyvinyl acetate illustrates that 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, for simplicity of description, not to above-mentioned reality
It applies 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, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of tough fire retardant agent, which comprises the following steps:
The modified lignin resin of initiator, the vinylacetate of 100 mass parts and 2~25 mass parts is mixed, ontology in situ occurs
Polymerization reaction obtains reactant；The modified lignin resin is prepared by following methods: by glycol dimethyl ether, the alkali of 100 mass parts
Lignin and the mixing of the maleic anhydride of 10~50 mass parts, react 2~8 hours at 80 DEG C~90 DEG C, cooling, are filtered, washed, obtain
To thick modified lignin resin；The thick modified lignin resin and methanol are mixed, dissolved 30 minutes at 50 DEG C~80 DEG C, it is cooling, filtering,
Washing, obtains filtrate；The solid that the filtrate is distilled is mixed with water, is filtered, washed, dries, obtains the innovation wood
Quality；
The reactant is purified, the tough fire retardant agent is obtained.
2. the preparation method of tough fire retardant agent according to claim 1, which is characterized in that the initiator is peroxidating two
Benzoyl or azodiisobutyronitrile.
3. the preparation method of tough fire retardant agent according to claim 1, which is characterized 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, which is characterized in that the modified lignin resin is by following
Method preparation:
The maleic anhydride of glycol dimethyl ether, the alkali lignin of 100 mass parts and 30~40 mass parts is mixed, 80 DEG C~90
It is DEG C reaction 2~8 hours, cooling, it is filtered, washed, obtains thick modified lignin resin；
The thick modified lignin resin and methanol are mixed, dissolved 30 minutes at 50 DEG C~80 DEG C, it is cooling, it is filtered, washed, is filtered
Liquid；
The solid that the filtrate is distilled is mixed with water, is filtered, washed, dries, obtains the modified lignin resin.
5. the preparation method of tough fire retardant agent according to claim 4, which is characterized in that the glycol dimethyl ether is opposite
The dosage of the alkali lignin is 4~5ml/g alkali lignin.
6. the preparation method of described in any item tough fire retardant agent according to claim 1~5, which is characterized in that the generation is former
The reaction temperature of position bulk polymerization is 60 DEG C~100 DEG C, and the reaction time is 2~8 hours.
7. the preparation method of tough fire retardant agent according to claim 6, which is characterized in that generation bulk polymerization in situ
The reaction temperature of reaction is 70 DEG C~90 DEG C, and the reaction time is 4~6 hours.
8. the preparation method of described in any item tough fire retardant agent according to claim 1~5, which is characterized in that by the reaction
The step of object purifies, and obtains the tough fire retardant agent specifically: the reactant and methanol are mixed, stirred at 60 DEG C to complete
Dissolution, obtains lysate；
The lysate is mixed with water, is filtered, washed, dries, obtains the tough fire retardant agent.
9. the preparation method of tough fire retardant agent according to claim 8, which is characterized in that the dosage of the methanol is described
2.5~3.5 times of reactant quality.
10. a kind of tough fire retardant agent prepared by the preparation method using according to any one of claims 1 to 99 described in any item tough fire retardant agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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