CN107325260A - A kind of modified phosphorus nitrogen expansion type combustion inhibitor fire-retardant polyurethane foam and preparation method - Google Patents
A kind of modified phosphorus nitrogen expansion type combustion inhibitor fire-retardant polyurethane foam and preparation method Download PDFInfo
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- CN107325260A CN107325260A CN201710671442.2A CN201710671442A CN107325260A CN 107325260 A CN107325260 A CN 107325260A CN 201710671442 A CN201710671442 A CN 201710671442A CN 107325260 A CN107325260 A CN 107325260A
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- expansion type
- type combustion
- combustion inhibitor
- polyurethane foam
- nitrogen expansion
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- 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
- C08G2101/00—Manufacture of cellular products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
Abstract
The invention discloses a kind of modified phosphorus nitrogen expansion type combustion inhibitor fire-retardant polyurethane foam and preparation method.The foam is to be modified phosphorus nitrogen expansion type combustion inhibitor as dispersed phase, a kind of flame-proof composite material by continuous phase of polyurathamc, specifically three components such as the acid source of phosphorus nitrogen expansion type combustion inhibitor, source of the gas and charcoal source are mixed, surface modification is carried out with nonionic surfactant and polyacrylate elastomer emulsion, obtains being modified phosphorus nitrogen expansion type combustion inhibitor；Modified phosphorus nitrogen expansion type combustion inhibitor is added and is uniformly dispersed in dihydric alcohol, diisocyanate and blowing promotor are added thereto, continues to stir more than 1 minute, material is poured into mould, foaming and curing process are completed, the fire-retardant polyurethane foam of modified phosphorus nitrogen expansion type combustion inhibitor is obtained.It is modified to phosphorus nitrogen expansion type combustion inhibitor surface, generation and the performance of polyurethane foam are not influenceed, and the polyurethane foam that the modification phosphorus nitrogen expansion type combustion inhibitor of acquisition is fire-retardant has good combination property.
Description
Technical field
The present invention relates to phosphor-nitrogen expansion type combustion inhibitor technical field, specifically a kind of modified phosphor-nitrogen expansion type combustion inhibitor resistance
The polyurethane foam and preparation method of combustion.
Background technology
Polyurethane foam is a kind of high polymer material of superior performance.Because the thermal insulation of materials effect is good, high mechanical strength,
Electric property, chemical resistance and soundproof effect are excellent, thus in furniture, automotive trim, aero seat, building heat preservation, family
It is irreplaceable and be widely applied that there is other materials in the fields such as electricity, especially in terms of building energy conservation heat insulation.Due to
World energy sources shortage and the demand of energy-conservation, polyurethane foam have been widely used at present as the insulation material of function admirable.
China enforced in the city of Beijing, Tianjin, Dalian, Qingdao, Shenzhen, Shanghai etc. six and built since 2006
The standard of energy-conservation 65%, the provinces and cities such as Gansu, Henan also just progressively carry out this work.But, because polyurethane foam density is small,
Specific surface area is big, is easily ignited and burns, and burns rapid and fierce, is difficult to be extinguished, and produce largely has in combustion
Poisonous gas and smog, easily cause personnel's death by suffocation.Fire, 2009 4 occur for CCTV's new address BeiPeiLou within 2 9th, 2009
Month Nanjing middle ring International Square on the 19th also there occurs similar fire, including the Jinan Olympic Sports Center in recent years, Beijing Qiao Bo are slided
It is all architecture exterior wall insulating materials polyurethane foam to avenge the fire fire positions such as shop, Beijing University's table tennis training hall.2010 October 15 on days
Day, Shanghai Jing'an District Jiangzhou road teacher apartment is on fire, and the intensity of a fire is swift and violent, with poly- ammonia used in " external wall energy-saving comprehensive improvement " project
Ester cellular insulant is relevant.2 months 3 midnights in 2011 shortly past, be referred to as the high building of Shenyang first feudal dynasty ten thousand prosperous mansion because combustion
Putting on fireworks and firecrackers initiation fire, building alien invasion on fire has substantial amounts of inflammable polyurethane foam heat insulation material, is to cause fire
One of major reason of calamity.Whole building, which can be spread to, after this insulation material burning from fire location quickly forms three-dimensional combustion
Burn, and this insulation material is used in China much builds at present.How the fire prevention of architecture exterior wall insulating materials is improved
Safety turns into the important topic concerning people's livelihood safety.
Traditional halogen containing flame-retardant, mainly organic bromide/Sb2O3Fire proofing, tool fire-retardant for high polymer material
There is good fire resistance, but the gas of a large amount of poisonous and harmful strong and stimulatings can be produced during the burning of this fire proofing, to people
Healthy and environment cause direct, potential and permanent harm.Particularly trigger bioxin therefrom
(Dioxin) problem so that halogen containing flame-retardant is treated by the discretion of people.In some new high-tech industries, this kind of material
Using being restricted.What European Union put into effect《Rohs is instructed》Clear and definite limitation has been made in use to brominated flame-retardant.The U.S., Japan
And China has also promulgated the decree of correlation in succession, the use to brominated flame-retardant is equally limited.Therefore, people actively seek
Ask Halogen, low cigarette and environment-friendly new and effective fire proofing.IFR has good anti-flammability and security, meets health
The requirement of environmental protection, so its application prospect is good, it is the ideal chose of following substitution halogen containing flame-retardant.
Phosphor-nitrogen expansion type combustion inhibitor includes three kinds of Main Ingredients and Appearances：（1）Acid source.Acid source produces acid in heating.（2）Charcoal source.
Charcoal source is the compound rich in charcoal atom, and charcoal is dehydrated under the action of an acid.（3）Source of the gas.Source of the gas discharges volatilization when heated
Property product, generally amine or amide compound.Amine or acid amides also play catalytic action to the reaction for forming charcoal.Vapor can also be produced
Raw bubble effect.Typical expansion type flame retardant is APP（APP）/ melamine（MA）/ pentaerythrite（PER）Or season penta
Tetrol phosphate（PEPA）And its derivative.Because the decomposition of the thermal decomposition of acid source, the dehydration carbonization in charcoal source, source of foaming produces gas
The body synergy such as expand layer of charcoal, surface forms the layer of charcoal of one layer of bulk multi-hole, barrier when the flame-retardant polymer is burnt
Heat transfer and O2Diffusion, effectively delay and prevent the thermal degradation of polymer, it is suppressed that the production of volatile combustible component
It is raw, so as to reach fire-retardant purpose.The release of fuel gas and smog is reduced just because of foamed char, is simultaneously effective hindered
Polymer combustion is stopped and has produced melting drip phenomenon, so as to prevent flame transmission.
Existing phosphor-nitrogen expansion type combustion inhibitor has that bad dispersibility, foaminess be poor, mechanical property for polyurethane foam system
Can low deficiency.The modified phosphor-nitrogen expansion type combustion inhibitor resistance combustion polyurethane foam of the present invention, can effectively solve the above problems.
The content of the invention
It is an object of the invention to provide a kind of fire-retardant polyurethane foam of modified phosphor-nitrogen expansion type combustion inhibitor and preparation side
Method.The fire-retardant polyurethane foam of the modified phosphor-nitrogen expansion type combustion inhibitor, is a kind of flame-proof composite material, swollen to be modified phosphorus-nitrogen
Swollen type fire retardant is dispersed phase, using polyurethane foam as continuous phase（Matrix phase）.The preparation method, its key technology is pair
Phosphor-nitrogen expansion type combustion inhibitor surface is modified, and phosphor-nitrogen expansion type combustion inhibitor is not influenceed poly- ammonia when being prepared for polyurethane foam
The generation of ester foam and performance, obtain the fire-retardant polyurethane foam of the phosphor-nitrogen expansion type combustion inhibitor with good combination property.
Realizing the technical scheme of the object of the invention is：
A kind of fire-retardant polyurethane foam of modified phosphor-nitrogen expansion type combustion inhibitor, its architectural feature is with modified phosphor-nitrogen expansion type
Fire retardant is dispersed phase, using polyurethane foam as the flame-proof composite material of continuous phase.
A kind of preparation method of the fire-retardant polyurethane foam of modified phosphor-nitrogen expansion type combustion inhibitor, specifically includes following steps：
1）The preparation of modified phosphor-nitrogen expansion type combustion inhibitor：By the acid source of phosphor-nitrogen expansion type combustion inhibitor, source of the gas and the component of charcoal source three
By 1.5-3.5：0.5-1.5：0.5-1.5 ratio mixing, under high speed peptizaiton, successively adds nonionic surfactant
And polyacrylate elastomer emulsion, it is scattered more than 30 minutes at a high speed, the phosphor-nitrogen expansion type combustion inhibitor that surface is modified is made；
2）The preparation of the fire-retardant polyurethane foam of modified phosphor-nitrogen expansion type combustion inhibitor：By step 1）The phosphorus that obtained surface is modified-
Nitrogen expansion type combustion inhibitor is added in dihydric alcohol, after stirring more than 30 minutes, adds diisocyanate and polyurethane foam auxiliary agent,
Continue to stir 2-4 minutes, well mixed material is poured into mould, complete foaming and curing process, modified phosphorus-nitrogen is made swollen
The swollen flame retardant polyurethane foam of type；Phosphor-nitrogen expansion type combustion inhibitor is wherein modified in its fire-retardant polyurethane foam
Mass percent be more than 20%.
Step 1）In, described acid source is ammonium phosphate or ammonium polyphosphate；Described source of the gas is melamine, melamine
It is a kind of in phosphate or MCA；Described charcoal source is polyalcohol or PAPE.
Step 1）In, described nonionic surfactant is APEO series of surfactants, department's Pan's series of tables
One kind in face activating agent or TWEEN Series surfactant.
Step 1）In, the addition of described nonionic surfactant is that acid source, source of the gas and the constituent mass of charcoal source three are total
The 0.50-5.00% of sum；The addition of described polyacrylate elastomer emulsion is acid source, source of the gas and the constituent mass of charcoal source three
The 1.00-6.00% of summation.
Step 2）In, described dihydric alcohol is polyester diol or polyether Glycols.
Step 2）In, described diisocyanate is toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, different Fo Er
One kind in ketone diisocyanate or its performed polymer.
Step 2）In, described dihydric alcohol and the mass ratio of diisocyanate are 1.0-3.0：1.0.
Step 2）In, described polyurethane foam auxiliary agent is stannous octoate, dibutyl tin laurate, triethylene diamine
At least one of and organic silicon surfactant, polyurethane foam auxiliary dosage is dihydric alcohol and diisocyanate quality sum
0.20-0.80%.
Beneficial effect：By carrying out surface modification to phosphor-nitrogen expansion type combustion inhibitor, the fire retardant is set to disperse in dihydric alcohol
Property it is good, while the fire retardant does not influence raw material to foam and cure, obtained flame-retardant polyurethane foam has good anti-flammability, color
And other performances of items are suitable with pure polyurethane foam.
Embodiment
The present invention is further elaborated with reference to embodiment, but is not limitation of the invention.
Embodiment 1：
A kind of modified phosphor-nitrogen expansion type combustion inhibitor fire-retardant polyurethane foam and preparation method, specifically include following steps：
1）The preparation of modified phosphor-nitrogen expansion type combustion inhibitor：In the material pot of high-speed mixer, ammonium polyphosphate is added
120.0g, melamine 40.0g and pentaerythrite 40.0g, under stirring, being first slowly added to 10mL mass fractions is
After the 10.7% OP-10 aqueous solution, 10mL mass fractions are added for 28.6% polyacrylate elastomer emulsion；Add
Finish, continue to stir 30 minutes, material pot temperature control releases material below 80 degrees Celsius, as modified phosphorus-nitrogen expansion
Type fire retardant.
2）The preparation of phosphor-nitrogen expansion type combustion inhibitor resistance combustion polyurethane foam：In the material pot of high speed dispersor, add
150.0g molecular weight is 3000g/mol polyester diol, under high-speed stirred effect, is slowly added to 100.0g and is modified phosphorus-nitrogen
Expansion type flame retardant, after fire retardant addition is finished, continues to stir 30 minutes, adds 150.0g toluene di-isocyanate(TDI)s, 1.2g
Stannous octoate, 1.2g triethylene diamines and 1.2g organic silicon surfactants, high-speed stirred 2.0 minutes, resulting material is poured into
In mould, foam at room temperature, 10 minutes i.e. it is expandable finish, formed hard polyurethane foams.The modified flame-retardant agent is to poly- ammonia
The combination property of ester foaming and polyurethane foam has not significant impact.After testing, prepared resistance combustion polyurethane foam anti-flammability
Can be the V-0 levels of UL-94 standards.
Claims (9)
1. the fire-retardant polyurethane foam of a kind of modified phosphor-nitrogen expansion type combustion inhibitor, it is characterised in that its architectural feature is with modification
Phosphor-nitrogen expansion type combustion inhibitor be dispersed phase, the flame-proof composite material constituted using polyurethane foam as continuous phase.
2. a kind of preparation method of the fire-retardant polyurethane foam of modified phosphor-nitrogen expansion type combustion inhibitor, specifically includes following steps：
1）The preparation of modified phosphor-nitrogen expansion type combustion inhibitor：By the acid source of phosphor-nitrogen expansion type combustion inhibitor, source of the gas and the component of charcoal source three
By 1.5-3.5：0.5-1.5：0.5-1.5 ratio mixing, under high speed peptizaiton, successively adds nonionic surfactant
And polyacrylate elastomer emulsion, it is scattered more than 30 minutes at a high speed, the phosphor-nitrogen expansion type combustion inhibitor that surface is modified is made；
2）The preparation of the fire-retardant polyurethane foam of modified phosphor-nitrogen expansion type combustion inhibitor：By step 1）The phosphorus that obtained surface is modified-
Nitrogen expansion type combustion inhibitor is added in dihydric alcohol, after stirring more than 30 minutes, adds diisocyanate and polyurethane foam auxiliary agent,
Continue to stir 2-4 minutes, well mixed material is poured into mould, complete foaming and curing process, modified phosphorus-nitrogen is made swollen
The swollen flame retardant polyurethane foam of type；Phosphor-nitrogen expansion type combustion inhibitor is wherein modified in its fire-retardant polyurethane foam
Mass percent be more than 20%.
3. preparation method according to claim 2, it is characterised in that step 1）In, described acid source is ammonium phosphate or many
APP；Described source of the gas is one kind in melamine, melamine phosphate or MCA；Described charcoal
Source is polyalcohol or PAPE.
4. preparation method according to claim 2, it is characterised in that step 1）In, described nonionic surfactant,
For one kind in APEO series of surfactants, department's Pan's series of surfactants or TWEEN Series surfactant.
5. preparation method according to claim 2, it is characterised in that step 1）In, described nonionic surfactant
Addition be acid source, source of the gas and the constituent mass summation of charcoal source three 0.50-5.00%；Described polyacrylate elastomer breast
The addition of liquid is the 1.00-6.00% of acid source, source of the gas and the constituent mass summation of charcoal source three.
6. preparation method according to claim 2, it is characterised in that step 2）In, described dihydric alcohol is polyester binary
Alcohol or polyether Glycols.
7. preparation method according to claim 2, it is characterised in that step 2）In, described diisocyanate is toluene
One kind in diisocyanate, methyl diphenylene diisocyanate, IPDI or its performed polymer.
8. preparation method according to claim 2, it is characterised in that step 2）In, described dihydric alcohol and two isocyanic acids
The mass ratio of ester is 1.0-3.0：1.0.
9. preparation method according to claim 2, it is characterised in that step 2）In, described polyurethane foam auxiliary agent is
At least one of stannous octoate, dibutyl tin laurate, triethylene diamine and organic silicon surfactant, polyurethane foam
Auxiliary dosage is dihydric alcohol and the 0.20-0.80% of diisocyanate quality sum.
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| CN201710671442.2A CN107325260A (en) | 2017-08-08 | 2017-08-08 | A kind of modified phosphorus nitrogen expansion type combustion inhibitor fire-retardant polyurethane foam and preparation method |
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| CN201710671442.2A CN107325260A (en) | 2017-08-08 | 2017-08-08 | A kind of modified phosphorus nitrogen expansion type combustion inhibitor fire-retardant polyurethane foam and preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109337037A (en) * | 2018-09-30 | 2019-02-15 | 长春顺风新材料有限公司 | A kind of preparation method of rapid UV-curing polyurethane-acrylate emulsion |
| CN112143193A (en) * | 2019-06-26 | 2020-12-29 | 向红建 | Halogen-free nitrogen-phosphorus-containing macromolecular intumescent flame retardant and preparation method thereof |
| CN113817170A (en) * | 2021-09-14 | 2021-12-21 | 厦门理工学院 | Phosphorus-nitrogen-silicon-containing intumescent flame retardant, preparation method thereof and application thereof in rigid polyurethane foam |
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| CN113817170A (en) * | 2021-09-14 | 2021-12-21 | 厦门理工学院 | Phosphorus-nitrogen-silicon-containing intumescent flame retardant, preparation method thereof and application thereof in rigid polyurethane foam |
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