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CN106010415B - A kind of full water foamed cold-curing foam fireproof gap-filling glue and preparation method thereof - Google Patents

A kind of full water foamed cold-curing foam fireproof gap-filling glue and preparation method thereof Download PDF

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Publication number
CN106010415B
CN106010415B CN201610351761.0A CN201610351761A CN106010415B CN 106010415 B CN106010415 B CN 106010415B CN 201610351761 A CN201610351761 A CN 201610351761A CN 106010415 B CN106010415 B CN 106010415B
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parts
filling glue
component
catalyst
gap
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CN106010415A (en
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胡涛
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Jilin Zawa new materials Co., Ltd.
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JILIN GENERAL CHEMICAL SCIENCE AND TECHNOLOGY DEVELOPMENT Co Ltd
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    • C—CHEMISTRY; METALLURGY
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    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
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    • C08G18/18—Catalysts containing secondary or tertiary amines or salts thereof
    • C08G18/20—Heterocyclic amines; Salts thereof
    • C08G18/2045—Heterocyclic amines; Salts thereof containing condensed heterocyclic rings
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  • Chemical & Material Sciences (AREA)
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  • Health & Medical Sciences (AREA)
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  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Fireproofing Substances (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Sealing Material Composition (AREA)

Abstract

The present invention relates to a kind of full water foamed cold-curing foam fireproof gap-filling glue and preparation method thereof, belong to fire-proof sealing material technical field.Including 100 parts of polyalcohol, 38 50 parts of liquid phosphorus acid esters fire retardant, 110 120 parts of powder fire retardant, 25 parts of pigment, 1.8 4 parts of deionized water, 0.5 1.8 parts of tertiary amine catalyst, 1.8 2.4 parts of the temperature sensitive catalyst of hydrolysis, 1.8 2.5 parts of chain extender, 0.4 0.6 parts of high-activity silicon oil, 2.76 11 parts of catalyst activator, 0.8 1.8 parts of coupling agent；64 169 parts of polyisocyanates.Beneficial effect：With more excellent base material adhesive force, demand that can be in terms of ensureing to take into account environmental protection while lighting；And meet do not possess the onsite application demand of heating condition using the temperature sensitive catalyst of quaternary ammonium salt as the gel catalyst of hydrolysis in the present invention；The foaming layer of formation not only itself has excellent anti-flammability, also occurs that expansion forms solid fine and close carbon-coating concrete on fire occurs, and plays a part of preventing flame skewered from spreading and preventing calorie spread.

Description

A kind of full water foamed cold-curing foam fireproof gap-filling glue and preparation method thereof
Technical field
The present invention relates to fire-proof sealing material technical field, is specifically related to a kind of full water foamed cold-curing foam fireproof and fills out Stitch glue and preparation method thereof.
Background technology
Fire prevention gap-filling glue is formed when being mainly used in cable, crane span structure, groove box, airduct, material delivery pipe etc. through wall, floor Through hole fire separation.Traditional fire-proof sealing material such as fire protection plaster, fire-proof mud, back-fire relief bag are compared, there is construction party Just, using term of validity length, good weatherability, antidetonation cracking resistance, it is good to most of base material adhesive force, do not corrode the advantages such as cable.
Fire prevention gap-filling glue on the market with using based on silicone system or aqueous acrylamide acid system, exist hardening time it is long, Anti-mildew becomes the deficiencies of performance is not bad, good enough to some base material adhesive force.Although and polyurethane resin these aspects possess it is obvious excellent Gesture, and two-component foaming system is easily made to mitigate overall structure weight, as industry in terms of environmental protection for requiring increasingly Improve, it is full water foamed to compare traditional freon class foaming and more received by market.But due to being catalyzed usually as gel The organo-metallic catalyst of agent is very easy to hydrolysis, can be declined to a great extent in the next all left and right catalysis efficiencies of full water foamed system straight To occur do not solidify, it is difficult to for a long time preserve, and if using the temperature sensitive catalyst of quaternary ammonium salt, although catalyst can be solved The problem of hydrolysis, but because temperature sensitive catalyst requires very harsh for reaction temperature, catalysis efficiency is very low under normal temperature, and adds Catalysis efficiency can improve several times to tens times after heat, therefore be difficult to be used as the catalyst of cold curing polyurethane, be made with it Product is restricted in the job site use of no heating condition.
The content of the invention
The present invention provides a kind of full water foamed cold-curing foam gap-filling glue and preparation method thereof, it is therefore an objective to overcomes existing fire prevention The deficiency of gap-filling glue, there is provided a kind of solidification of two-component short time, it is full water foamed, can be in no heating and the construction of stirring condition Manual, long-time storage stable performance the polyurethane foam fire prevention gap-filling glue in scene.
The technical solution adopted by the present invention is：
A kind of full water foamed cold-curing foam fireproof gap-filling glue, include the raw material of following parts by weight：
Component A：100 parts of polyalcohol, liquid phosphorus acid esters fire retardant 38-50 parts, powder fire retardant 110-120 parts, pigment 2-5 Part, deionized water 1.8-4 parts, tertiary amine catalyst 0.5-1.8 parts, the temperature sensitive catalyst 1.8-2.4 parts of hydrolysis, chain extender 1.8- 2.5 parts, high-activity silicon oil 0.4-0.6 parts, catalyst activator 2.76-11 parts, coupling agent 0.8-1.8 parts；
B component：Polyisocyanates 64-169 parts；
The ratio of component A and B component is 100：22.8 or 100：32.8 or 100：41.4 or 100：60.
Polyalcohol of the present invention includes hydroxyl value 28-336mgKOH/g dihydroxy PPOX ether, trihydroxy polyoxy Change two kinds in propylene ether, polycaprolactone diols, polycaprolactone trihydroxylic alcohol, polymer grafted polyether polyol；
Liquid phosphorus acid esters fire retardant of the present invention include dimethyl methyl phosphonate, three (β-chloroethyl) phosphates, three (β- Chloropropyl) phosphate, one kind in 2,3- dichloro propyl phosphates；
Powder fire retardant of the present invention includes n>1000 II types ammonium polyphosphate, aluminium hydroxide, magnesium hydroxide, can be swollen Three kinds in swollen graphite, melamine, melamine cyanurate, pentaerythrite, bipentaerythrite, Firebrake ZB, ammonium octamolybdate with On；
Chain extender of the present invention includes ethylene glycol, BDO, in 2 methyl pentamethylenediamine, diethanol amine, hexylene glycol One or two；
Catalyst activator of the present invention includes one in 2- ethylaminoethanols, aminopropanol, amino butanol, amino-hexanol Kind；
The temperature sensitive catalyst of hydrolysis of the present invention includes the carbon -7- alkene phenolate of 1,8- diazabicylos 11,1,8- bis- One kind in the carbon -7- alkene caprylates of azabicyclic 11；
Tertiary amine catalyst of the present invention includes triethylene diamine, double (dimethylaminoethyl) ethers, N, N- dimethyl ethanols Amine, N, one kind in N- dimethyl benzylamines；
Coupling agent of the present invention includes gamma-aminopropyl-triethoxy-silane, γ-methacryloxypropyl trimethoxy One kind in base silane, phytane acid type monoalkoxy class titanate esters, phosphatic type monoalkoxy class titanate esters；
Polyisocyanates of the present invention includes poly methylene poly phenyl poly isocyanate, Carbodiimide-Modified diphenyl One or both of methane diisocyanate, 3- isocyanates methylene -3,5,5- trimethylcyclohexylisocyanates.
A kind of preparation method of full water foamed cold-curing foam fireproof gap-filling glue of the present invention, comprises the following steps：
(1) recipe ingredient is pressed, takes 100 parts of polyalcohol, liquid phosphorus acid esters fire retardant 38-50 parts, deionized water 1.8-4 Part, high-activity silicon oil 0.4-0.6 parts, tertiary amine catalyst 0.5-1.8 parts, the temperature sensitive catalyst 1.8-2.4 parts of hydrolysis, chain extender 1.8-2.5 parts, catalyst activator 2.76-11 parts are added in agitator tank, are stirred 30 minutes under 500 turns/min；
(2) recipe ingredient is pressed, powder fire retardant 110-120 parts, pigment 2-5 parts are added in graphite dryer, side The coupling agent 0.8-1.8 parts diluted with petroleum ether are uniformly sprayed in dryer by stirring side, and normal temperature and pressure mixes 30 Minute, it is then heated at 60-80 DEG C and vacuumizes 1 hour removing petroleum ether；
(3) the powder fire retardant and pigment handled well are added in agitator tank and continues stirring 1 hour, be the foam fireproof The component A of gap-filling glue；
(4) polyisocyanates is added in agitator tank stir 30 minutes by the formula component and discharged, as B component；
(5) ratio of component A and B component is pressed 100：22.8 or 100：32.8 or 100：41.4 or 100：60 weigh, bag Dress, it is intumescent two-component fire prevention gap-filling glue.
The present invention has the advantages that：Polyurethane-based foam fire prevention gap-filling glue, than with organic siliconresin or water-based by third Olefin(e) acid resin is the fire prevention gap-filling glue of base-material, has more excellent base material adhesive force, compares for aluminium section bar, polyethylene etc. The substrate surface of hardly possible attachment, can adhere to well, and the formula design of two-component causes its hardening time to greatly shorten again, carries High efficiency of construction；Compared in general polyurethane foam glue gap filling, due to being full water foamed system, lighting can ensured While take into account demand in terms of environmental protection；And it is catalyzed in the present invention using the temperature sensitive catalyst of quaternary ammonium salt as the gel of hydrolysis Agent, using mono amino alcohol compound as catalyst activator, the aminoterminal of such compound and the isocyanate groups of B component are anti- Should be active very high, reaction can release amount of heat to improve the catalysis efficiency of temperature sensitive catalyst, and it is steady can to solve catalyst hydrolysis Contradiction between catalysis efficiency is low under qualitative difference and normal temperature；And the hydroxyl reaction activity of the other end is relatively low, viscosity will not be made to increase It is too fast to cause the difficulty that job site is stirred by hand, stirring and the dumping time of more than 5 minutes can be achieved, satisfaction does not possess heating The onsite application demand of condition；The foaming layer of formation not only itself has excellent anti-flammability, can also be sent out concrete on fire occurs Raw expansion forms solid fine and close carbon-coating, plays a part of preventing flame skewered from spreading and preventing calorie spread.
Embodiment
Embodiment 1
Hydroxyl value 336mgKOH/g 15 parts of trihydroxy PPOX ether, hydroxyl value 112mgKOH/g dihydroxy PPOXs 85 parts of ether, 50 parts of dimethyl methyl phosphonate, 0.4 part of high-activity silicon oil, 2.9 parts of deionized water, 2 parts of diethanol amine, 2- amino second 2.76 parts of alcohol, 1,8- diazabicylo 11,2 parts of carbon -7- alkene phenolate, 0.5 part of triethylene diamine, 25 parts of expansible graphite, iron Red 2 parts, 20 parts of aluminium hydroxide, 5 parts of Firebrake ZB, 40 parts of II types ammonium polyphosphate, 15 parts of melamine, 12 parts of pentaerythrite, γ- 1.2 parts of aminopropyl triethoxysilane, 47 parts of carbodiimide modified diphenylmethane diisocyanate, polymethylene polyphenyl 45 parts of polyisocyanates.
Described expansion fire-proof gap-filling glue, its preparation method are：By trihydroxy PPOX ether, dihydroxy polyoxygenated Propylene ether, dimethyl methyl phosphonate, high-activity silicon oil, deionized water, diethanol amine, 2- ethylaminoethanols, 1,8- diazabicylos 11 carbon -7- alkene phenolates, triethylene diamine are added in agitator tank and stirred 30 minutes；By expansible graphite, iron oxide red, hydroxide Aluminium, Firebrake ZB, II types ammonium polyphosphate, melamine, pentaerythrite are added in graphite dryer, are sprayed while stirring under normal temperature The gamma-aminopropyl-triethoxy-silane 30min diluted with petroleum ether, it is then heated at 60 DEG C and vacuumizes 1h removing oil Ether；Mixed powder after processing is added in agitator tank and continues to stir 1h, discharging is component A；By Carbodiimide-Modified two It is B that methylenebis phenyl isocyanate, poly methylene poly phenyl poly isocyanate, which put into stirring 30min dischargings in another agitator tank, Component；A, B component are pressed 100：32.8 is canned.
Embodiment 2
Hydroxyl value 37mgKOH/g 90 parts of trihydroxy PPOX ether, hydroxyl value 28mgKOH/g polymer graft polyol 10 parts, three 38 parts of (β-chloroethyl) phosphates, 0.5 part of high-activity silicon oil, 3.5 parts of deionized water, 1.8 parts of ethylene glycol, aminopropan 8.47 parts of alcohol, 1,8- diazabicylo 11,2.2 parts of carbon -7- alkene caprylate, double 0.9 part of (dimethylaminoethyl) ethers, it may expand 30 parts of graphite, 5 parts of iron oxide red, 10 parts of magnesium hydroxide, 5 parts of ammonium octamolybdate, 45 parts of II types ammonium polyphosphate, melamine cyanurate 10 Part, 10 parts of bipentaerythrite, 0.8 part of γ-aminopropyltrimethoxysilane, Carbodiimide-Modified diphenylmethane diisocyanate 84 parts of ester, 3- isocyanates methylenes -3,5,32.5 parts of 5- trimethylcyclohexylisocyanates.
Described expansion fire-proof gap-filling glue, its preparation method are：Trihydroxy PPOX ether, polymer grafting is more First alcohol, three (β-chloroethyl) phosphates, high-activity silicon oil, deionized water, ethylene glycol, aminopropanol, 1,8- diazabicylos ten One carbon -7- alkene caprylate, double (dimethylaminoethyl) ethers are added in agitator tank and stirred 30 minutes；By expansible graphite, iron oxide red, hydrogen Magnesia, ammonium octamolybdate, II types ammonium polyphosphate, melamine cyanurate, bipentaerythrite are added in graphite dryer, normal temperature Under the γ-aminopropyltrimethoxysilane 30min that was diluted with petroleum ether of sprinkling while stirring, be then heated at 80 DEG C take out it is true Empty 1h removes petroleum ether；Mixed powder after processing is added in agitator tank and continues to stir 1h, discharging is component A；Will carbonization Diimine modified diphenylmethane diisocyanate, 3- isocyanates methylene -3,5,5- trimethylcyclohexylisocyanates It is B component to put into stirring 30min dischargings in another agitator tank；A, B component are pressed 100：41.4 is canned.
Embodiment 3
Hydroxyl value 168mgKOH/g 30 parts of trihydroxy PPOX ether, hydroxyl value 56mgKOH/g polycaprolactone diols 70 parts, three 44 parts of (β-chloropropyl) phosphates, 0.6 part of high-activity silicon oil, 1.8 parts of deionized water, 2 parts of hexylene glycol, 2- methylpents 0.5 part of diamines, 6.88 parts of amino butanol, 1,8- diazabicylo 11,1.8 parts, N of carbon -7- alkene caprylate, N- dimethyl ethanols 1.5 parts of amine, 35 parts of expansible graphite, 3.530 parts of iron oxide red, 15 parts of magnesium hydroxide, 5 parts of aluminium hydroxide, 6 parts of Firebrake ZB, eight molybdic acids 8 parts of ammonium, 30 parts of II types ammonium polyphosphate, 8 parts of melamine, 3 parts of bipentaerythrite, phytane acid type monoalkoxy class titanate esters 1.8 parts, 57 parts of poly methylene poly phenyl poly isocyanate, 3- isocyanates methylenes -3,5,5- trimethylcyclohexyl isocyanides 7 parts of acid esters.
Described expansion fire-proof gap-filling glue, its preparation method are：By trihydroxy PPOX ether, polycaprolactone binary Alcohol, three (β-chloropropyl) phosphates, high-activity silicon oil, deionized water, hexylene glycol, 2 methyl pentamethylenediamine, amino butanol, 1,8- bis- Carbon -7- alkene the caprylate of azabicyclic 11, N, N- dimethylethanolamines are added in agitator tank and stirred 30 minutes；By inflatable stone Ink, iron oxide red, magnesium hydroxide, aluminium hydroxide, II types ammonium polyphosphate, melamine, bipentaerythrite are added in graphite dryer, The phytane acid type monoalkoxy class titanate esters 30min that sprinkling while stirring was diluted with petroleum ether under normal temperature, is then heated to 70 1h removing petroleum ethers are vacuumized at DEG C；Mixed powder after processing is added in agitator tank and continues to stir 1h, discharging is A groups Point；Poly methylene poly phenyl poly isocyanate, 3- isocyanates methylene -3,5,5- trimethylcyclohexylisocyanates are thrown It is B component to enter stirring 30min dischargings in another agitator tank；A, B component are pressed 100：22.8 is canned.
Embodiment 4
Hydroxyl value 112mgKOH/g 80 parts of dihydroxy PPOX ether, hydroxyl value 336mgKOH/g polycaprolactone trihydroxylic alcohol 20 parts, 2,3- 38 parts of dichloro propyl phosphates, 0.4 part of high-activity silicon oil, 4 parts of deionized water, 2.2 parts of BDO, amino 11 parts of hexanol, 1,8- diazabicylo 11,2.4 parts, N of carbon -7- alkene phenolate, 1.8 parts of N- dimethyl benzylamines, expansible graphite 42 parts, 2.5 parts of iron oxide red, 10 parts of aluminium hydroxide, 50 parts of II types ammonium polyphosphate, 8 parts of melamine cyanurate, pentaerythrite 10 Part, 1 part of phosphatic type monoalkoxy class titanate esters, 169 parts of poly methylene poly phenyl poly isocyanate.
Described expansion fire-proof gap-filling glue, its preparation method are：By dihydroxy PPOX ether, polycaprolactone ternary Alcohol, 2,3- dichloros propyl phosphate, high-activity silicon oil, deionized water, butanediol, amino-hexanol, 1,8- diazabicylos 11 Carbon -7- alkene phenolate, N, N- dimethyl benzylamines are added in agitator tank and stirred 30 minutes；By expansible graphite, iron oxide red, hydroxide Aluminium, II types ammonium polyphosphate, melamine cyanurate, pentaerythrite are added in graphite dryer, are sprayed while stirring under normal temperature The phosphatic type monoalkoxy class titanate esters 30min diluted with petroleum ether, it is then heated at 75 DEG C and vacuumizes 1h removing oil Ether；Mixed powder after processing is added in agitator tank and continues to stir 1h, discharging is component A；Polymethylene polyphenyl polyisocyanate Cyanate is B component；A, B component are pressed 100：60 is canned.
Test case：
Blob of viscose is made by GB 23864-2009 in above example and comparative example, detects its density, corrosion resistance, expansion respectively Performance, fire endurance；Batten is made by GB/T 8624, measures fire resistance grade respectively；Pressed using omnipotent mechanics machine GB/T 13477 measures glue-line and peels off caking property；Example and comparative example are positioned over 20h at -20 DEG C, are being positioned over normal temperature Solidify respectively after 4h, simulate the accumulating performance under its low temperature, above testing result is shown in Table 1.
The properties of product test result of table 1
Note：Comparative example 1 is a kind of expanded silicone fireproof gap-filling glue, and comparative example 2 is a kind of polyurethane fireproof gap-filling glue.
According to 1 every testing result of table, the present invention gap-filling glue product more common than in the market is in curing rate, corrosion resistance Energy, fire endurance and low temperature accumulating performance are had a clear superiority, and density is lower, and the load-carrying that can effectively reduce closure hole is born Lotus.

Claims (9)

1. a kind of full water foamed cold-curing foam fireproof gap-filling glue, it is characterised in that include the raw material of following parts by weight：
Component A：100 parts of polyalcohol, liquid phosphorus acid esters fire retardant 38-50 parts, powder fire retardant 110-120 parts, pigment 2-5 parts, Deionized water 1.8-4 parts, tertiary amine catalyst 0.5-1.8 parts, the temperature sensitive catalyst 1.8-2.4 parts of hydrolysis, chain extender 1.8-2.5 Part, high-activity silicon oil 0.4-0.6 parts, catalyst activator 2.76-11 parts, coupling agent 0.8-1.8 parts；
The catalyst activator includes one kind in 2- ethylaminoethanols, aminopropanol, amino butanol, amino-hexanol；
B component：Polyisocyanates 64-169 parts；
The polyisocyanates includes poly methylene poly phenyl poly isocyanate, the isocyanide of Carbodiimide-Modified diphenyl methane two One or both of acid esters, 3- isocyanates methylene -3,5,5- trimethylcyclohexylisocyanates；
The ratio of component A and B component is 100：22.8 or 100：32.8 or 100：41.4 or 100：60.
2. a kind of full water foamed cold-curing foam fireproof gap-filling glue according to claim 1, it is characterised in that described polynary Alcohol includes hydroxyl value 28-336mgKOH/g dihydroxy PPOX ether, trihydroxy PPOX ether, polycaprolactone binary Two kinds in alcohol, polycaprolactone trihydroxylic alcohol, polymer grafted polyether polyol.
A kind of 3. full water foamed cold-curing foam fireproof gap-filling glue according to claim 1, it is characterised in that the liquid Phosphate flame retardant includes dimethyl methyl phosphonate, three (β-chloroethyl) phosphates, three (β-chloropropyl) phosphates, 2,3- dichloros One kind in propyl phosphate.
A kind of 4. full water foamed cold-curing foam fireproof gap-filling glue according to claim 1, it is characterised in that the powder Fire retardant includes n>1000 II types ammonium polyphosphate, aluminium hydroxide, magnesium hydroxide, expansible graphite, melamine, melamine More than three kinds in aminuria hydrochlorate, pentaerythrite, bipentaerythrite, Firebrake ZB, ammonium octamolybdate.
A kind of 5. full water foamed cold-curing foam fireproof gap-filling glue according to claim 1, it is characterised in that the chain extension Agent includes ethylene glycol, one or both of BDO, 2 methyl pentamethylenediamine, diethanol amine, hexylene glycol.
6. a kind of full water foamed cold-curing foam fireproof gap-filling glue according to claim 1, it is characterised in that described water-fast Solving temperature sensitive catalyst includes the carbon -7- alkene phenolate of 1,8- diazabicylos 11, the carbon -7- alkene of 1,8- diazabicylos 11 octanoic acid One kind in salt.
A kind of 7. full water foamed cold-curing foam fireproof gap-filling glue according to claim 1, it is characterised in that the tertiary amine Catalyst includes triethylene diamine, double (dimethylaminoethyl) ethers, N, N- dimethylethanolamines, N, and one in N- dimethyl benzylamines Kind.
A kind of 8. full water foamed cold-curing foam fireproof gap-filling glue according to claim 1, it is characterised in that the coupling Agent includes gamma-aminopropyl-triethoxy-silane, γ-methacryloxypropyl trimethoxy silane, phytane acid type list alcoxyl One kind in base class titanate esters, phosphatic type monoalkoxy class titanate esters.
9. a kind of preparation method of full water foamed cold-curing foam fireproof gap-filling glue as described in claim 1~8, including it is following Step：
(1) press the recipe ingredient, take 100 parts of polyalcohol, liquid phosphorus acid esters fire retardant 38-50 parts, deionized water 1.8-4 parts, High-activity silicon oil 0.4-0.6 parts, tertiary amine catalyst 0.5-1.8 parts, the temperature sensitive catalyst 1.8-2.4 parts of hydrolysis, chain extender 1.8- 2.5 parts, catalyst activator 2.76-11 parts add agitator tank in, stirred 30 minutes under 500 turns/min；
(2) recipe ingredient is pressed, powder fire retardant 110-120 parts, pigment 2-5 parts are added in graphite dryer, side stirring While the coupling agent 0.8-1.8 parts diluted with petroleum ether are uniformly sprayed in dryer, normal temperature and pressure mixes 30 minutes, It is then heated at 60-80 DEG C and vacuumizes 1 hour removing petroleum ether；
(3) the powder fire retardant and pigment handled well are added in agitator tank and continues stirring 1 hour, be the foam fireproof joint filling The component A of glue；
(4) polyisocyanates is added in agitator tank stir 30 minutes by the formula component and discharged, as B component；
(5) ratio of component A and B component is pressed 100：22.8 or 100：32.8 or 100：41.4 or 100：60 weigh, packaging, i.e., For intumescent two-component fire prevention gap-filling glue.
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