CN104403603A - Flame-retardant cross-linked polyvinyl alcohol binder and preparation method thereof - Google Patents
Flame-retardant cross-linked polyvinyl alcohol binder and preparation method thereof Download PDFInfo
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- CN104403603A CN104403603A CN201410568626.2A CN201410568626A CN104403603A CN 104403603 A CN104403603 A CN 104403603A CN 201410568626 A CN201410568626 A CN 201410568626A CN 104403603 A CN104403603 A CN 104403603A
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Abstract
The invention relates to a flame retardant cross-linked polyvinyl alcohol binder and a preparation method thereof. The binder comprises the components in parts by weight: 100 parts of water, 3-20 parts of polyvinyl alcohol, 1.6-18 parts of an inorganic composite flame retardant, 0.2-1.2 parts of an inorganic crosslinking agent, 0.01-0.2 part of emulsified silicone oil, and 0.2-3 parts of an anti-mildew agent. The inorganic composite flame retardant is composed of ammonium polyphosphate and zinc sulfate according to the mass ratio of 1:0.006-0.02. The method adopts a compound having active groups to be subjected to a reaction with hydroxyl on polyvinyl alcohol molecules to form a crosslinked product, the hydroxyl on the polyvinyl alcohol molecules is sealed, the water absorption of polyvinyl alcohol is reduced, and the water resistant level of polyvinyl alcohol is improved.
Description
Technical field
The present invention relates to a kind of polyvinyl alcohol adhesive and preparation method thereof, particularly a kind of flame-proof cross-linking type polyvinyl alcohol adhesive and preparation method thereof.
Background technology
Polyvinyl alcohol (PVA) is a kind of high molecular weight water soluble polymer of excellent property, and its physical properties is tasteless, colourless, nontoxic, non-corrosiveness, have easily by biological decomposition, and performance is between plastics and rubber, and purposes is quite extensive.Because it has unique strong adherence, epithelium snappiness, smoothness, oil-proofness, solvent resistance, protective colloid, barrier properties for gases, wear resistance, except making vinylon fibre, also by a large amount of for the production of coating, tackiness agent, paper product machining agent, emulsifying agent, dispersion agent, photosensitive resin, paper grade (stock) finishing agent, industry slurry, makeup, the products such as solar cell backboard component composition and film, range of application is throughout weaving, food, medicine, building, wood working, paper industry, printing, agricultural, building, iron and steel, the industries such as macromolecule chemical industry, there is very wide application prospect.Have more oh group in PVA, cause it to have stronger wetting ability, poor water tolerance and stability, these weakness greatly limit its in the industry further genralrlization application.The hydrophilic immanent cause of polyvinyl alcohol is that molecular chain exists great amount of hydroxy group, it is the group that absorbs water by force, want to improve its water tolerance, the hydroxyl in PVA molecule must be sheltered, or make hydroxyl be combined with other material the material generating and be insoluble in water.This hydroxyl on polyvinyl alcohol molecule is also a very active chemical group; it can with many chemical substance generation chemical reactions, if react with numerous compounds such as aldehydes, HDI or TDI, boric acid, urea, organosilicon radical, epoxy resin, Vinyl Acetate Copolymer, ACRYLIC EMULSION and amines.By these reactions, not only shelter oh group, improved the water tolerance of polyvinyl alcohol, the modified polyvinyl alcohol that performance is various can also be obtained, strengthen its range of application.
Polyvinyl alcohol as a binder, a film forming agent, toughening and reinforcing a wide range of potential applications in the construction, transportation, marine drilling platform, garage storage, steel works, but its highly hydrophilic limited its promotion in these areas.Modification is carried out to polyvinyl alcohol, improves its water tolerance, can greatly advance it in the application in these fields.
On the other hand, being used in the problem that the material in construction work abstains from most is incendivity.For macromolecular material, the charring rate of material is high, and its oxygen index also can be higher.Charring rate reaches the polymer of 40-50%, and its oxygen index can higher than 30%, and the polymer that charring rate is lower, its oxygen index is no more than 20%.Polyvinyl alcohol is macromolecular material, the same with other most of macromolecular material, is the material that charring rate is lower, and its limiting oxygen index(LOI) (LOI) is lower than 20%, and be easy to burning, flame retardant properties difference is its maximum shortcoming, has a strong impact on its application.The application of polyvinyl alcohol to be promoted at building field, first will become the material of flame retardant resistance.Up to now, had a lot of reports to the fire-retardant research of PVA material, it mainly contains following three kinds of methods: 1. blending fire retardant modification, 2. copolymerization is flame-retardant modified, and 3. sol-gel method prepares PVA/Si0
2hybrid material, the technique of wherein blending fire retardant modification is the simplest, and relative price is also lower.This patent selects blending fire retardant method of modifying.
According to composition, additive flame retardant mainly comprises inorganic combustion inhibitor (aluminium hydroxide, magnesium hydroxide etc.), halogenated flame retardant (organic chloride and organic bromide), phosphorus flame retardant (red phosphorus, phosphoric acid ester and halogenated phosphate etc.) and nitrogenated flame retardant etc.
And the environment friendly flame retardant of Halogen, low cigarette, low toxicity is the target that people pursue always.Phosphorus flame retardant has three kinds of fire-retardant effects in macromolecular material, and as dewatering agent, promote that polymer becomes charcoal, the generation of charcoal reduces the thermal conduction from flame to condensed phase; Phosphoric acid can absorb heat, because it is prevented that CO is oxidized to CO
2, reduce heat-processed; Condensed phase is formed to the glass or liquid protective layer of thin layer; because this reducing oxygen diffusion and the heat between gas phase and solid phase and mass transfer; inhibit char combustion process, reduce phosphonium flame retardant decomposes and following change occurs: phosphorus flame retardant → metaphosphoric acid → phosphoric acid → poly-metaphosphoric acid.Poly-metaphosphoric acid is not volatile stable compound, has high dehydrated, at polymkeric substance table compound and air exclusion; The heat that the moisture sorption of deviating from is a large amount of, makes polymer surfaces fire retardant decomposes discharge volatility phosphide.
Nitrogenated flame retardant is a kind of new and effective fire retardant, after it has been generally acknowledged that nitrogenated flame retardant decomposes, the non-flammable gases such as easy releasing ammonia, nitrogen, degree of depth oxynitride, water vapor, the generation of non-flammable gases and fire retardant divide heat of desorption (comprising the distillation heat absorption of a part of fire retardant) to take away most of heat, greatly reduce the surface temperature of polymkeric substance.Non-flammable gas, as nitrogen, not only serve the effect that oxygen in diluent air and superpolymer decomposes produce the concentration of inflammable gas, the oxide compound of nitrogen, water and the degree of depth can also be generated with oxygen reaction in air, while the oxygen of consumable material surface, reach good flame retardant effect.Nitrogenated flame retardant mainly comprises 3 large classes: trimeric cyanamide, Dyhard RU 100, flesh salt (carbonic acid flesh, phosphoric acid flesh, condensed phosphoric acid flesh and thionamic acid flesh) and their derivative, particularly phosphoric acid salt derivative.
Summary of the invention
An object of the present invention is the flame-proof cross-linking type polyvinyl alcohol adhesive providing a kind of applicable building engineering field application.
Two of object of the present invention is the preparation method providing this binding agent.
Due to the polyhydroxy structure of polyvinyl alcohol adhesive, make this binding agent become aqueous solution systems, meet the theory of environmental protection.For meeting fire prevention and the ecological requirements of construction work, the present invention selects inorganic phosphorus flame retardant, and it can impel polyvinyl alcohol to become charcoal, improves the flame retardant resistance of binding agent.The water tolerance of binding agent when building engineering field uses, also extremely important, inorganic solidification agent is as inorganic salt such as borate, Titanium hydrochlorate or chromic salt, and not only having the hydroxyl sheltered on binding agent molecule, is also favourable to the flame retardant resistance of binding agent.The modification of polyvinyl alcohol adhesive in water tolerance and flame retardant resistance improves, and contributes to very much expanding it and uses at building engineering field.
Can be used as polyvinyl alcohol of the present invention is a kind of excellent property, broad-spectrum commodity polymer material, and the structural formula of its molecule is as follows:
Its alcoholysis degree is the important indicator weighing hydrophilic hydroxy group and hydrophobicity ethanoyl number in polyvinyl alcohol molecule, and it has material impact to the product performance of PVA.Along with the reduction of alcoholysis degree, in polyvinyl alcohol molecule, hydrophilic hydroxy group quantity reduces, and the ability of polyvinyl alcohol molecule formation hydrogen bond is also corresponding to be weakened, and the corresponding increase of hydrophobic ethanoyl quantity.This change that is hydrophilic, hydrophobic grouping quantity result in polyvinyl alcohol performance great changes will take place just.Usually, along with the reduction of alcoholysis degree, the emulsion dispersion ability of polyvinyl alcohol, hydrophobic material bounding force, water dissolution performance, stable viscosity performance to be improved, and the corresponding reduction of film toughness, water tolerance, and whipability and conglomeration trend are obviously.The polymerization degree of polyvinyl alcohol commodity differs greatly, having that the polymerization degree is little is hundreds of, and large having is thousands of, has a significant impact the viscosity of polyvinyl alcohol water solution, the alcoholysis degree scope of the polyvinyl alcohol that the present invention selects is between 50%-99%, and preferred polyvinyl alcohol alcoholysis degree is between 88%-99%.The polymerization degree of polyvinyl alcohol can adopt between 800-2000, preferably selects the polymerization degree between 1200-1700.
For achieving the above object, the present invention adopts following technical scheme:
A kind of flame-proof cross-linking type polyvinyl alcohol adhesive, is characterized in that the composition of this binding agent and parts by weight are:
100 parts, water;
Polyvinyl alcohol 3 ~ 20 parts;
Inorganic composite flame retardants 1.6-18 part;
Inorganic crosslinking agent 0.2-1.2 part;
Silicone emulsion 0.01-0.2 part;
Mould inhibitor 0.2-3 part;
Described electrodeless composite flame-retardant agent is mixed by the mass ratio of 1:0.006 ~ 0.02 by ammonium polyphosphate and zinc sulfate.
The alcoholysis degree scope of above-mentioned polyvinyl alcohol is between 50% ~ 99%, and its polymerization degree is between 800 ~ 2000.
Above-mentioned polyvinyl alcohol alcoholysis degree is 88% ~ 99%, and its polymerization degree is between 1200 ~ 1700.
Above-mentioned inorganic crosslinking agent is: the complex compound of sodium sulfate, zinc sulfate, boric acid, borax, dichromate, chromium nitrate, chromium, cuprammonium oxyhydroxide or organic titanate.
Above-mentioned mould inhibitor is phenylformic acid, Sodium Benzoate, propionic acid and its esters, Sorbic Acid and its esters, dehydro-acetic acid, citric acid and Trisodium Citrate hydroxybenzoate, sodium Diacetate or dimethyl fumarate.
Prepare a method for above-mentioned flame-proof cross-linking type polyvinyl alcohol adhesive, it is characterized in that the concrete steps of the method are:
A. polyvinyl alcohol is added to the water, then adds silicone emulsion and mould inhibitor, at 70 DEG C ~ 95 DEG C temperature, be stirred to polyvinyl alcohol all dissolve; Add composite flame-retardant agent again, 25 DEG C condition under stirring and dissolving, namely form flame retardant polyethylene alcohol binding agent;
B. the pH value of regulating step a obtained flame-retardant polyvinyl alcohol adhesive is to 5 ~ 9, then at 20 DEG C of-100 DEG C of temperature, is added dropwise to inorganic crosslinking agent, obtains the flame retardant polyethylene alcohol binding agent of crosslinked shape structure.
Present method adopts the compound and the hydroxyl reaction on polyvinyl alcohol molecule with active group, forms cross-linking products, seals the hydroxyl on polyvinyl alcohol molecule, reduce the water-absorbent of polyvinyl alcohol, the water-fast grade of raising polyvinyl alcohol.Polyvinyl alcohol is nonpoisonous and tasteless aqueous high molecular material, the binding agent of a kind of green that to take water as solvent be.Particularly the important point, as the binding agent of building trade, polyvinyl alcohol can be degraded by microorganisms in physical environment, and final product is carbon, hydrogen, oxygen and water, very environmental protection.Containing great amount of hydroxy group on polyvinyl alcohol molecule, so it and cement and gypsum material have very strong cohesiveness, also with other material of construction as the materials such as iron and steel, glass natural fiber also have good cohesive strength.The maximum feature of binding agent of the present invention is, after appropriate interpolation linking agent, is that part of hydroxyl is sealed, and is that the water tolerance of polyvinyl alcohol improves; The existence of fire retardant in formula is that the oxygen index of product reaches about 35.
Embodiment
Be below the limiting examples that the present invention prepares flame-proof cross-linking type polyvinyl alcohol adhesive solution, these examples have further described and demonstrated the embodiment in the scope of the invention.The embodiment provided only for illustration of object, do not form any restriction to the present invention, can carry out various change to its concentration under the condition not deviating from spirit and scope of the invention, all concentration listed in embodiment are weight part.
Embodiment 1: the water 8 parts of granule of polyvinyl alcohol materials, 0.02 part of silicone emulsion and 0.05 Sodium Benzoate being put into 70 DEG C-95 DEG C, heated and stirred 3 hours, until granule of polyvinyl alcohol all dissolves.3.5 parts of composite flame-retardant agents (ammonium polyphosphate/zinc sulfate is 1:0.008) are made the aqueous solution, joins in polyvinyl alcohol water solution, stir at normal temperatures and can form flame retardant polyethylene alcohol binder solution.Proper ammonia or sulfuric acid (98%) are added at normal temperatures the flame retardant polyethylene alcohol binder solution stirred, the pH value of regulator solution is 7.When rapid stirring, the temperature of reaction of solution is adjusted to 60 DEG C, and being added drop-wise in reactor containing 0.09 part of sodium tetraborate aqueous solution, reacting 2 hours, can obtain and there is the more limpid aqueous solution of fire-retardant water-resistant polyvinyl alcohol binding agent.This binding agent is made solid sample, and through flame retardant resistance test, its flame retardant resistance is 35, and state of cure is 68.54.
Embodiment 2: change following condition, other condition is with embodiment 1.Proper ammonia or sulfuric acid (98%) are added at normal temperatures the flame retardant polyethylene alcohol binder solution stirred, the pH value of regulator solution is 5.Compared with the sample of embodiment 1 gained, there is gelatin phenomenon in the aqueous solution of this sample.
Embodiment 3: change following condition, other condition is with embodiment 1.When rapid stirring, the temperature of reaction of solution is adjusted to 50 DEG C, and being added drop-wise in reactor containing 0.09 part of sodium tetraborate aqueous solution, reacting 2 hours, can obtain and there is the more limpid aqueous solution of fire-retardant water-resistant polyvinyl alcohol binding agent.After tested, its state of cure is 61.43 to this formula
Embodiment 4: change following condition, other condition is with embodiment 1.3.5 parts of composite flame-retardant agents (ammonium polyphosphate/zinc sulfate is 1:0.002) are made the aqueous solution, joins in polyvinyl alcohol water solution, stir at normal temperatures and can form flame retardant polyethylene alcohol binder solution.This binding agent is made solid sample, and through flame retardant resistance test, its oxygen index is 34.
Embodiment 5: change following condition, other condition is with embodiment 1.3.5 parts of composite flame-retardant agents (ammonium polyphosphate/zinc sulfate is 1:0.006) are made the aqueous solution, joins in polyvinyl alcohol water solution, stir at normal temperatures and can form flame retardant polyethylene alcohol binder solution.This binding agent is made solid sample, and through flame retardant resistance test, its oxygen index is 36.
Embodiment 6: change following condition, other condition is with embodiment 1.3.5 parts of composite flame-retardant agents (ammonium polyphosphate/zinc sulfate is 1:0.01) are made the aqueous solution, joins in polyvinyl alcohol water solution, stir at normal temperatures and can form flame retardant polyethylene alcohol binder solution.This binding agent is made solid sample, and through flame retardant resistance test, its oxygen index is 34.
Embodiment 7: change following condition, other condition is with embodiment 1.3.5 parts of composite flame-retardant agents (ammonium polyphosphate/zinc sulfate is 1:0.02) are made the aqueous solution, joins in polyvinyl alcohol water solution, stir at normal temperatures and can form flame retardant polyethylene alcohol binder solution.This binding agent is made solid sample, and through flame retardant resistance test, its oxygen index is 29.
Claims (6)
1. a flame-proof cross-linking type polyvinyl alcohol adhesive, is characterized in that the composition of this binding agent and parts by weight are:
100 parts, water;
Polyvinyl alcohol 3 ~ 20 parts;
Inorganic composite flame retardants 1.6-18 part;
Inorganic crosslinking agent 0.2-1.2 part;
Silicone emulsion 0.01-0.2 part;
Mould inhibitor 0.2-3 part;
Described electrodeless composite flame-retardant agent is mixed by the mass ratio of 1:0.006 ~ 0.02 by ammonium polyphosphate and zinc sulfate.
2. flame-proof cross-linking type polyvinyl alcohol adhesive according to claim 1, it is characterized in that the alcoholysis degree scope of described polyvinyl alcohol is between 50% ~ 99%, its polymerization degree is between 800 ~ 2000.
3. flame-proof cross-linking type polyvinyl alcohol adhesive according to claim 2, it is characterized in that described polyvinyl alcohol alcoholysis degree is 88% ~ 99%, its polymerization degree is between 1200 ~ 1700.
4. flame-proof cross-linking type polyvinyl alcohol adhesive according to claim 1, is characterized in that described inorganic crosslinking agent is: the complex compound of sodium sulfate, zinc sulfate, boric acid, borax, dichromate, chromium nitrate, chromium, cuprammonium oxyhydroxide or organic titanate.
5. flame-proof cross-linking type polyvinyl alcohol adhesive according to claim 1, is characterized in that described mould inhibitor is phenylformic acid, Sodium Benzoate, propionic acid and its esters, Sorbic Acid and its esters, dehydro-acetic acid, citric acid and Trisodium Citrate hydroxybenzoate, sodium Diacetate or dimethyl fumarate.
6. prepare a method for the flame-proof cross-linking type polyvinyl alcohol adhesive according to any one of claim 1-5, it is characterized in that the concrete steps of the method are:
A. polyvinyl alcohol is added to the water, then adds silicone emulsion and mould inhibitor, at 70 DEG C ~ 95 DEG C temperature, be stirred to polyvinyl alcohol all dissolve; Add composite flame-retardant agent again, 25 DEG C condition under stirring and dissolving, namely form flame retardant polyethylene alcohol binding agent;
B. the pH value of regulating step a obtained flame-retardant polyvinyl alcohol adhesive is to 5 ~ 9, then at 20 DEG C of-100 DEG C of temperature, is added dropwise to inorganic crosslinking agent, obtains the flame retardant polyethylene alcohol binding agent of crosslinked shape structure.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106928869A (en) * | 2017-05-02 | 2017-07-07 | 南通沪望塑料科技发展有限公司 | A kind of polyethylene is anti-, drain plate binding agent |
| CN108192256A (en) * | 2017-12-19 | 2018-06-22 | 常州市阿曼特化工有限公司 | A kind of preparation method of the resin expanded glue of composition polymer |
| CN109004220A (en) * | 2018-07-19 | 2018-12-14 | 苏州大学 | A kind of boronic acid compounds modification lithium ion battery silicium cathode and preparation method thereof |
| CN111909615A (en) * | 2020-08-14 | 2020-11-10 | 江西龙泰新材料股份有限公司 | Water-based flame-retardant coating for fireproof cotton textile rope |
| CN112143148A (en) * | 2020-09-25 | 2020-12-29 | 湖南安翔科技有限公司 | Polyvinyl alcohol film and preparation method thereof |
| CN112341957A (en) * | 2020-10-21 | 2021-02-09 | 齐皓宇 | Metal complex type high-strength polyvinyl alcohol glue and preparation method thereof |
| CN112824470A (en) * | 2019-11-21 | 2021-05-21 | 江西佳银科技有限公司 | Organic binder based on phosphorus-containing high polymer resin and preparation method and application thereof |
| CN113004578A (en) * | 2021-04-02 | 2021-06-22 | 江苏恒尚节能科技股份有限公司 | Waterproof heat-insulation curtain wall and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928869A (en) * | 2017-05-02 | 2017-07-07 | 南通沪望塑料科技发展有限公司 | A kind of polyethylene is anti-, drain plate binding agent |
| CN108192256A (en) * | 2017-12-19 | 2018-06-22 | 常州市阿曼特化工有限公司 | A kind of preparation method of the resin expanded glue of composition polymer |
| CN109004220A (en) * | 2018-07-19 | 2018-12-14 | 苏州大学 | A kind of boronic acid compounds modification lithium ion battery silicium cathode and preparation method thereof |
| CN109004220B (en) * | 2018-07-19 | 2021-07-20 | 苏州大学 | Boric acid compound modified lithium ion battery silicon cathode and preparation method thereof |
| CN112824470A (en) * | 2019-11-21 | 2021-05-21 | 江西佳银科技有限公司 | Organic binder based on phosphorus-containing high polymer resin and preparation method and application thereof |
| CN112824470B (en) * | 2019-11-21 | 2023-07-21 | 江西佳银科技有限公司 | Organic binder based on phosphorus-containing polymer resin and preparation method and application thereof |
| CN111909615A (en) * | 2020-08-14 | 2020-11-10 | 江西龙泰新材料股份有限公司 | Water-based flame-retardant coating for fireproof cotton textile rope |
| CN111909615B (en) * | 2020-08-14 | 2021-12-03 | 江西龙泰新材料股份有限公司 | Water-based flame-retardant coating for fireproof cotton textile rope |
| CN112143148A (en) * | 2020-09-25 | 2020-12-29 | 湖南安翔科技有限公司 | Polyvinyl alcohol film and preparation method thereof |
| CN112341957A (en) * | 2020-10-21 | 2021-02-09 | 齐皓宇 | Metal complex type high-strength polyvinyl alcohol glue and preparation method thereof |
| CN113004578A (en) * | 2021-04-02 | 2021-06-22 | 江苏恒尚节能科技股份有限公司 | Waterproof heat-insulation curtain wall and preparation method thereof |
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Application publication date: 20150311 |