CN107722908B - A kind of preparation method of polyurethane fireproof glue for building - Google Patents
A kind of preparation method of polyurethane fireproof glue for building Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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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
- C08G18/28—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
- C08G18/44—Polycarbonates
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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
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K3/2279—Oxides; Hydroxides of metals of antimony
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
- C08K7/12—Asbestos
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to a kind of preparation methods of polyurethane fireproof glue for building, it is mixed with by pre-polymer component and polyol component, wherein, pre-polymer component is obtained by diisocyanate, antimony oxide, asbestos fibre, poly (propylene carbonate) polyalcohol, catalyst preparation, polyol component is prepared by poly (propylene carbonate) polyalcohol, chain extender, crosslinking agent, bromine-containing polyols.Wherein, antimony oxide, asbestos fibre, bromine-containing polyols have the effect of cooperative flame retardant, and obtained fireproof gum can combine flame retardant property, fire-retardant persistence, mechanical property.
Description
Technical field
The present invention relates to polyurethane fireproof glue field, in particular to one kind can combine flame retardant property, it is fire-retardant persistently
Property, polyurethane fireproof glue for building of mechanical property and preparation method thereof.
Background technique
Adhesive for polyurethane has the performances such as excellent elastic, low temperature resistant, wear-resisting and good bonding.Therefore, it answers extensively
For building, the fields such as automobile, house ornamentation, waterproof and ship.
However, adhesive for polyurethane is inflammable, and when being burnt by external heat source, big, burning velocity that there are flames
Fastly, drippage is serious, produce thick smoke and the problems such as toxic gas, seriously threatens people's security of the lives and property.As people are to building
The raising that field fire protecting performance requires, the flame retardant property of polyurethane fireproof glue are increasingly taken seriously.
In the prior art, in order to prepare polyurethane fireproof glue, flame retardant property is improved, generallys use and adds during the preparation process
It is disclosed in the additive flame retardants, such as CN105504354A such as metal hydroxide combustion inhibitor, red phosphorus combustion inhibitor, zinc borate, APP
A kind of pressure sensitive adhesive efficient halogen-free element fire retardant combination comprising: aluminium hydroxide 25-90%.CN104893641A is disclosed
A kind of preparation method of high-strength fire-retarding polyurethane sealant, the sealant are made of A, B component, are indicated with parts by weight,
Middle component A is made of following component: 60-70 parts of polyurethane prepolymer, 3-5 parts of stearic acid, -200 22-24 parts of mesh silica are received
12-14 parts of titanium dioxide of rice, -400 18-20 parts of mesh zirconium dioxides, 6-8 parts of plasticizer, 12-14 parts of tackifier, fire-retardant aluminium hydroxide
3-5 parts, it is zinc borate 5-7 parts fire-retardant, 6-8 parts of melamine cyanurate.The fire-retardant effect of traditional inorganic hydroxide fire retardant
Rate is low, and very big additive amount is needed to can be only achieved fire-retardant purpose.Common additive flame retardant is easily precipitated, and flame retardant property is with making
It can be lost with the extension of process.
Reactive flame retardant can participate in reaction as a kind of reacted constituent, and it is good to be conducive to obtain fire-retardant persistence
Polyurethane fireproof glue, such as CN106221654A is related to a kind of flame retardant bicomponent adhesive for polyurethane and preparation method thereof,
In, the method for being total to flame-retardant modified polyurethane using soft and hard segments prepares isocyanate group component A and polyalcohol B component respectively,
In, component A is made of diisocyanate, the polyalcohol containing fire-retardant group, reactive flame retardant；B component is by chain extender, crosslinking
Agent, the polyalcohol containing fire-retardant group, reactive flame retardant composition, obtain one after A, B bi-component are mixed in a certain ratio, are solidified
The kind good adhesive for polyurethane material of flame retardant property.CN104232006A provide a kind of novel flame-retardant polyurethane adhesive and
Preparation method, the polyurethane adhesive is by polytetrahydrofuran diol 1000, toluene di-isocyanate(TDI), reaction-type flame-retarding
Agent, chain extender and crosslinking agent are prepared, and the reactive flame retardant is dibromoneopentyl glycol, and the chain extender is Isosorbide-5-Nitrae-
Butanediol, the crosslinking agent are trimethylolpropane.But reactive flame retardant is used completely, and it is at high cost, influence polyurethane
Proportion, and certain influence can be generated on performance.
Traditional adhesive for polyurethane mostly uses greatly polyether polyol as polyol component, with the excellent of hydrolysis
Point, but flame retardant property is not so good as polyester polyol, selects polyester polyol the problem of facing solution not resistant to water again, has had at present
It is some report point out poly (propylene carbonate) polyalcohol have excellent anti-hydrolytic performance, such as CN105482068A,
CN1865311A, CN106589300A etc., but document is attempted poly (propylene carbonate) polyalcohol being used to prepare building not yet
With polyurethane fireproof glue.
In conclusion providing a kind of poly- ammonia for building that can combine flame retardant property, fire-retardant persistence, mechanical property
Ester fireproof gum has critically important application value.
Summary of the invention
The purpose of the present invention essentially consists in the deficiency avoided in existing polyurethane fireproof glue technology, and providing one kind can be simultaneously
Take into account the polyurethane fireproof glue for building and preparation method thereof of flame retardant property, fire-retardant persistence, mechanical property.
Polyurethane fireproof glue for building of the invention is achieved through the following technical solutions:
A kind of polyurethane fireproof glue for building, the fireproof gum are made of pre-polymer component and polyol component, wherein pre-
Copolymer component is by diisocyanate 30-70 mass parts, antimony oxide 1-5 mass parts, asbestos fibre 1-5 mass parts, poly- carbonic acid
Sub- propyl ester polyalcohol 5-30 mass parts, catalyst 0.01-0.2 mass parts composition, polyol component are polynary by poly (propylene carbonate)
Alcohol 50-80 mass parts, chain extender 3-7 mass parts, crosslinking agent 2-4 mass parts, 5-10 parts of bromine-containing polyols compositions.
Wherein, the poly (propylene carbonate) polyalcohol in the pre-polymer component is the poly- carbon of number-average molecular weight 1000-2000
Sour Asia propyl ester glycol.
The polymerized thylene carbonate third that poly (propylene carbonate) polyalcohol in the polyol component is number-average molecular weight 5000-6000
Esterdiol.
The diisocyanate can be toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, the more methylenes of more phenyl
One or more of Quito isocyanates, preferably polyphenyl polymethylene polyisocyanates (such as PM-100, PM-200 etc.).
The bromine-containing polyols are firemaster 520, bromine content 46.0%, hydroxyl value 195-217mgKOH/g.
The chain extender is one of 1,4- butanediol, 1,6-HD.
The crosslinking agent is one of glycerol, trimethylolpropane.
The catalyst is one of dibutyl tin dilaurate, stannous octoate.
When pre-polymer component and polyol component mix, pre-polymer component mass fraction is about 40%-50%, polyol component
About 60%-50%.
Diisocyanate dosage is preferably 60-70 mass parts in pre-polymer component, and poly (propylene carbonate) polyalcohol dosage is excellent
It is selected as 5-10 mass parts.
Poly (propylene carbonate) polyalcohol dosage is preferably that 50-60 mass parts, chain extender dosage are preferably in polyol component
3-4 mass parts, dosage of crosslinking agent are preferably 2-3 mass parts, and bromine-containing polyols dosage is preferably 5-8 mass parts.
The method for preparing polyurethane fireproof glue, comprising the following steps:
(1) preparation of pre-polymer component: by poly (propylene carbonate) polyalcohol 5-30 mass parts, vacuum is done at 90-100 DEG C
Dry 1-3 hours water removal, is added diisocyanate 30-70 mass parts, antimony oxide 1-5 mass parts, stone after being cooled to 60-80 DEG C
Cotton fiber 1-5 mass parts, catalyst 0.01-0.2 mass parts, are stirred, and reaction obtained prepolymer after 2-6 hours；
(2) poly (propylene carbonate) polyalcohol 50-80 mass parts, chain extender 3-7 mass the preparation of polyol component: are weighed
Part, crosslinking agent 2-4 mass parts, are uniformly mixed by 5-10 parts of bromine-containing polyols, obtain polyol component；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is about 40%-50%, and polyol component is about 60%-50%.
The utility model has the advantages that
1, additive flame retardant is easily precipitated, and flame retardant property can lose with the extension of use process, and traditional inorganic
The flame retarding efficiency of hydroxide flame retardant is low, and very big additive amount is needed to can be only achieved fire-retardant purpose；Reactive flame retardant conduct
A kind of reacted constituent can participate in reaction, but use reactive flame retardant completely, at high cost, influence the proportion of polyurethane,
And certain influence can be generated on performance.In order to obtain the effect more balanced, the present invention selects bromine-containing polyols first, especially
It is to have screened firemaster 520, and for general flame-proof polyol, viscosity is lower, is more suitble to mixture；
Other than reactive flame retardant, it is matched that the present invention has also screened two kinds of inorganic additive flame retardants.Asbestos fibre can mention
The high temperature resistant and flame retardant property of high fireproof gum, and by its special pattern, it will help further increase flame retardant property；Three
It aoxidizes two antimony flame retardant property itself not protrude, but the present invention has found brominated by carrying out repeated screening to a large amount of fire retardants
Polyalcohol, asbestos fibre, antimony oxide three cooperation, flame retardant effect is very good, has the effect of cooperative flame retardant, this point from
The available confirmation of embodiment.
2, the antimony oxide, asbestos fibre, the bromine-containing polyols that play flame retardant effect are respectively put into soft and hard segments component,
Wherein, antimony oxide, asbestos fibre can wrap up in prepolymer in prepolymer preparation process, guarantee there is one in hard section
Dividing flame-retardant composition, bromine-containing polyols are placed in polyol component, and it is subsequent to enter polyurethane soft segment, finally guarantee entire polyurethane point
There are more flame-retardant compositions in son, and for being all mixed into a component, it can be ensured that more equal when mixing
It is even, and after preparing the flame-retardant composition later period can be uniformly distributed in polyurethane, and also have to flame retardant effect certain
It is promoted.
3, traditional adhesive for polyurethane mostly uses greatly polyether polyol as polyol component, with hydrolysis
Advantage, but flame retardant property is not so good as polyester polyol, selects polyester polyol the problem of facing solution not resistant to water again, at present
Have it is some report point out poly (propylene carbonate) polyalcohol have excellent anti-hydrolytic performance, such as CN105482068A,
CN1865311A, CN106589300A etc., but document is attempted poly (propylene carbonate) polyalcohol being used to prepare building not yet
With polyurethane fireproof glue, the present invention uses poly (propylene carbonate) polyalcohol, improves flame retardant property, overcome hydrolysis problem, and
And it finds in prepolymer preparation using the poly (propylene carbonate) glycol within the scope of number-average molecular weight 1000-2000, polyol component
The middle poly (propylene carbonate) glycol using number-average molecular weight 5000-6000, the impact of performance are best.
Specific embodiment
The present invention is described in further details below in conjunction with specific embodiment.It should be understood that these embodiments are for saying
The bright basic principles, principal features and advantages of the present invention, and the present invention is not by the scope limitation of following embodiment.It is adopted in embodiment
Implementation condition can do further adjustment according to specific requirement, and the implementation condition being not specified is usually the item in routine experiment
Part.
Embodiment 1
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 1000 100
It is dried in vacuo 3 hours and removes water at DEG C, 70 mass parts of polyphenyl polymethylene polyisocyanates, three oxidations are added after being cooled to 80 DEG C
Two antimony, 5 mass parts, 3 mass parts of asbestos fibre, 0.01 mass parts of stannous octoate, are stirred, and reaction obtained pre-polymerization after 5 hours
Object；
(2) preparation of polyol component: weigh number-average molecular weight 6000 60 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 4- butanediol, 2 mass parts of trimethylolpropane, are stirred by 520 5 parts of bromine-containing polyols firemaster
It is even, obtain polyol component；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
Embodiment 2
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 5 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 2000 100
It is dried in vacuo 2 hours and removes water at DEG C, 60 mass parts of polyphenyl polymethylene polyisocyanates, three oxidations are added after being cooled to 70 DEG C
Two antimony, 4 mass parts, 4 mass parts of asbestos fibre, 0.2 mass parts of dibutyl tin dilaurate, are stirred, after reaction 5 hours
To prepolymer；
(2) preparation of polyol component: weigh number-average molecular weight 6000 50 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 6- hexylene glycol, 2 mass parts of glycerol, 520 10 mass parts of bromine-containing polyols firemaster are uniformly mixed, obtain
Obtain polyol component；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 50%, and polyol component mass fraction is 50%.
Embodiment 3
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 1500 95
It is dried in vacuo 3 hours and removes water at DEG C, 70 mass parts of polyphenyl polymethylene polyisocyanates, three oxidations are added after being cooled to 80 DEG C
Two antimony, 5 mass parts, 4 mass parts of asbestos fibre, 0.1 mass parts of stannous octoate, are stirred, and reaction obtained prepolymer after 6 hours；
(2) preparation of polyol component: weigh number-average molecular weight 6000 60 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 4- butanediol, 3 mass parts of trimethylolpropane, 520 7 mass parts of bromine-containing polyols firemaster are stirred
Uniformly, polyol component is obtained；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
Comparative example 1
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 1000 100
It is dried in vacuo 3 hours and removes water at DEG C, 70 mass parts of polyphenyl polymethylene polyisocyanates, three oxidations are added after being cooled to 80 DEG C
Two antimony, 8 mass parts, 0.01 mass parts of stannous octoate, are stirred, and reaction obtained prepolymer after 5 hours；
(2) preparation of polyol component: weigh number-average molecular weight 6000 60 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 4- butanediol, 2 mass parts of trimethylolpropane, 520 5 mass parts of bromine-containing polyols firemaster are stirred
Uniformly, polyol component is obtained；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
Comparative example 2
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 1000 100
It is dried in vacuo 3 hours and removes water at DEG C, it is fine that 70 mass parts of polyphenyl polymethylene polyisocyanates, asbestos are added after being cooled to 80 DEG C
8 mass parts, 0.01 mass parts of stannous octoate are tieed up, are stirred, reaction obtained prepolymer after 5 hours；
(2) preparation of polyol component: weigh number-average molecular weight 6000 60 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 4- butanediol, 2 mass parts of trimethylolpropane, 520 5 mass parts of bromine-containing polyols firemaster are stirred
Uniformly, polyol component is obtained；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
Comparative example 3
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 1000 100
It is dried in vacuo 3 hours and removes water at DEG C, 70 mass parts of polyphenyl polymethylene polyisocyanates, zinc borate are added after being cooled to 80 DEG C
5 mass parts, 3 mass parts of asbestos fibre, 0.01 mass parts of stannous octoate, are stirred, and reaction obtained prepolymer after 5 hours；
(2) preparation of polyol component: weigh number-average molecular weight 6000 60 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 4- butanediol, 2 mass parts of trimethylolpropane, 520 5 mass parts of bromine-containing polyols firemaster are stirred
Uniformly, polyol component is obtained；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
Comparative example 4
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 1000 100
It is dried in vacuo 3 hours and removes water at DEG C, 70 mass parts of polyphenyl polymethylene polyisocyanates, three oxidations are added after being cooled to 80 DEG C
Two antimony, 5 mass parts, 3 mass parts of asbestos fibre, 0.01 mass parts of stannous octoate, are stirred, and reaction obtained pre-polymerization after 5 hours
Object；
(2) preparation of polyol component: weigh number-average molecular weight 6000 60 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 4- butanediol, 2 mass parts of trimethylolpropane, are uniformly mixed by 5 parts of dimethyl methyl phosphonate, obtain polyalcohol
Component；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
Comparative example 5
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 5 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 2000 100
It is dried in vacuo 2 hours and removes water at DEG C, 60 mass parts of polyphenyl polymethylene polyisocyanates, two laurels are added after being cooled to 70 DEG C
Sour 0.2 mass parts of dibutyl tin, are stirred, and reaction obtained prepolymer after 5 hours；
(2) preparation of polyol component: weigh number-average molecular weight 6000 50 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 6- hexylene glycol, 2 mass parts of glycerol, 520 10 mass parts of bromine-containing polyols firemaster, 4 mass of antimony oxide
Part, 4 mass parts of asbestos fibre are uniformly mixed, and obtain polyol component；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 50%, and polyol component mass fraction is 50%.
Comparative example 6
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of poly (propylene carbonate) dihydric alcohol of number-average molecular weight 7000 95
It is dried in vacuo 3 hours and removes water at DEG C, 70 mass parts of polyphenyl polymethylene polyisocyanates, three oxidations are added after being cooled to 80 DEG C
Two antimony, 5 mass parts, 4 mass parts of asbestos fibre, 0. 1 mass parts of stannous octoate, are stirred, and reaction obtained pre-polymerization after 6 hours
Object；
(2) preparation of polyol component: weigh number-average molecular weight 1000 60 mass parts of poly (propylene carbonate) dihydric alcohol, 1,
3 mass parts of 4- butanediol, 3 mass parts of trimethylolpropane, 520 7 mass parts of bromine-containing polyols firemaster are stirred
Uniformly, polyol component is obtained；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
Comparative example 7
A kind of polyurethane fireproof glue for building is prepared as follows:
(1) preparation of pre-polymer component: by 10 mass parts of Polyoxypropylene diol of number-average molecular weight 1500 at 95 DEG C
Lower vacuum drying removes water for 3 hours, and 70 mass parts of polyphenyl polymethylene polyisocyanates, three oxidations two are added after being cooled to 80 DEG C
5 mass parts of antimony, 4 mass parts of asbestos fibre, 0. 1 mass parts of stannous octoate, are stirred, and reaction obtained prepolymer after 6 hours；
(2) 60 mass parts of Polyoxypropylene diol, the 1,4- of number-average molecular weight 6000 preparation of polyol component: are weighed
3 mass parts of butanediol, 3 mass parts of trimethylolpropane, 520 7 mass parts of bromine-containing polyols firemaster are stirred
It is even, obtain polyol component；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain is mixed
It closes, obtains fireproof gum, wherein pre-polymer component mass fraction is 40%, and polyol component mass fraction is 60%.
1 polyurethane fireproof glue the performance test results of table
The present invention is described in detail above, the explanation of embodiment be merely used to help understand method of the invention and
Its core concept, its object is to allow the personage for being familiar with this field technology to can understand the content of the present invention and implement it accordingly, and
The protection scope that the present invention cannot be limited in this way.Any equivalent change or modification in accordance with the spirit of the invention should all be contained
Lid is within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of polyurethane fireproof glue for building, it is characterised in that the following steps are included: (1) pre-polymer component
Preparation: poly (propylene carbonate) polyalcohol 5-30 mass parts are dried in vacuo 1-3 hours at 90-100 DEG C and are removed water, be cooled to 60-
Diisocyanate 30-70 mass parts, antimony oxide 1-5 mass parts, asbestos fibre 1-5 mass parts, catalyst are added after 80 DEG C
0.01-0.2 mass parts, are stirred, and reaction obtained pre-polymer component after 2-6 hours；
(2) preparation of polyol component: poly (propylene carbonate) polyalcohol 50-80 mass parts are weighed, chain extender 3-7 mass parts, are handed over
Join agent 2-4 mass parts, 5-10 parts of bromine-containing polyols, be uniformly mixed, obtains polyol component；
(3) preparation of fireproof gum: the polyol component that the pre-polymer component and step (2) that step (1) is obtained obtain mixes, and obtains
To fireproof gum, wherein pre-polymer component mass fraction is 40%-50%, polyol component 60%-50%；
The poly (propylene carbonate) two that poly (propylene carbonate) polyalcohol in the pre-polymer component is number-average molecular weight 1000-2000
Alcohol；
The poly (propylene carbonate) two that poly (propylene carbonate) polyalcohol in the polyol component is number-average molecular weight 5000-6000
Alcohol.
2. the preparation method of polyurethane fireproof glue for building according to claim 1, it is characterised in that: the diisocyanate
Ester is one of toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, polyphenyl polymethylene polyisocyanates or several
Kind.
3. the preparation method of polyurethane fireproof glue for building according to claim 1, it is characterised in that: described brominated polynary
Alcohol is firemaster 520.
4. the preparation method of polyurethane fireproof glue for building according to claim 1, it is characterised in that: the chain extender is
One of 1,4- butanediol, 1,6-HD.
5. the preparation method of polyurethane fireproof glue for building according to claim 1, it is characterised in that: the crosslinking agent is
One of glycerol, trimethylolpropane.
6. the preparation method of polyurethane fireproof glue for building according to claim 1, it is characterised in that: the prepolymer group
When dividing with polyol component mixing, pre-polymer component mass fraction is 40%-50%, polyol component 60%-50%.
7. the preparation method of polyurethane fireproof glue for building according to claim 1, it is characterised in that: the prepolymer group
Diisocyanate is 60-70 mass parts in point, and poly (propylene carbonate) polyalcohol is 5-10 mass parts.
8. the preparation method of polyurethane fireproof glue for building according to claim 1, it is characterised in that: the polyalcohol group
Point in poly (propylene carbonate) polyalcohol be 50-60 mass parts, chain extender 3-4 mass parts, crosslinking agent 2-3 mass parts, it is brominated polynary
Alcohol 5-8 mass parts.
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| CN111073587B (en) * | 2019-12-19 | 2021-10-29 | 上海华峰新材料研发科技有限公司 | Ultralow temperature-resistant environment-friendly double-component polyurethane adhesive and preparation and application thereof |
| CN112048274A (en) * | 2020-07-29 | 2020-12-08 | 东风汽车集团有限公司 | Bi-component flame-retardant polyurethane adhesive for bonding and sealing power battery and preparation method thereof |
| CN112724909A (en) * | 2020-12-30 | 2021-04-30 | 广州集泰化工股份有限公司 | High-shear-strength two-component polyurethane corner adhesive and preparation method thereof |
| EP4359460A1 (en) * | 2021-06-23 | 2024-05-01 | Saudi Aramco Technologies Company | Polyol compositions and methods |
| CN114456761B (en) * | 2021-12-23 | 2024-04-26 | 广州集泰化工股份有限公司 | Polyurethane section sealant and preparation method thereof |
| CN114395360A (en) * | 2022-02-23 | 2022-04-26 | 杭州得力科技股份有限公司 | Flame-retardant bi-component polyurethane adhesive and preparation method thereof |
| CN115030335B (en) * | 2022-07-06 | 2023-04-18 | 徐州市晶鑫新材料有限公司 | Composite insulation board for building outer wall and preparation method thereof |
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