CN106243632A - A kind of preparation method of fire proofing material - Google Patents

A kind of preparation method of fire proofing material Download PDF

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Publication number
CN106243632A
CN106243632A CN201610631874.6A CN201610631874A CN106243632A CN 106243632 A CN106243632 A CN 106243632A CN 201610631874 A CN201610631874 A CN 201610631874A CN 106243632 A CN106243632 A CN 106243632A
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epoxy resin
product
mass ratio
diluent
powder
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CN201610631874.6A
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CN106243632B (en
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吴美燕
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Shantou Tianling Security Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Building Environments (AREA)

Abstract

The present invention relates to the preparation method of a kind of fire proofing material, by defoamer and dispersant according to certain mass than joining the powder being stirring evenly and then adding into certain mass in the High shear device filling diluent, high speed shear to powder is fully dispersed in diluent, alicyclic based epoxy resin and modifying agent are joined in the diluent of scattered powder, stirring to epoxy resin and modifying agent is fully dispersed in diluent, add water and firming agent, i.e. obtain fire proofing material.The present invention can effectively prevent the disaster hidden-trouble in building construction process.

Description

A kind of preparation method of fire proofing material
Technical field
The present invention relates to the preparation method of a kind of fire proofing material.
Background technology
Due to the generation of the most a lot of building heat preservation event of fire, cause the thinking of each bound pair insulated fire, insulation The beyond example great attention causing all circles in the industry of the fire protecting performance of material.But, a lot of insulation materials are on fire be all Work progress produces, such as: electric welding, naked light, bad construction custom.What these materials the most constantly produced melts Dripping thing and toxic smoke, the harm of environment also can not be neglected by the gas such as the Chlorofluorocarbons (CFCs) simultaneously discharged, hydrofluorocarbons, freon Depending on.Fire proofing material arises at the historic moment.
Fire proofing material is mainly based on incombustible at present, and binding agent is auxiliary, needs to smear certain thickness, and this increases the most greatly Add the weight of fire proofing material, bring the biggest trouble to carrying and construction.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of fire proofing material, and the present invention can construct Facilitate and can effectively prevent the disaster hidden-trouble in building construction process.
In order to solve above-mentioned technical problem, present invention employs techniques below scheme:
The preparation method of a kind of fire proofing material, it is characterised in that follow the steps below:
1) product A is made: defoamer, dispersant and fire retardant certain mass ratio is joined the high shear filling diluent In equipment, it is stirring evenly and then adding into the powder of certain mass, the mass ratio of defoamer, dispersant, fire retardant, powder and diluent It is 0.5~3:0.5~3:0.5~3:200~500:1000, high speed shear 20min~60min, is fully dispersed in powder dilute Release in agent, obtain product A;
2), product B is made: join in product A by epoxy resin and modifying agent according to certain mass ratio, epoxy resin, modification The mass ratio of agent and product A is 60~89:1~10:10~30, and stirring to epoxy resin and modifying agent is fully dispersed in diluent In, obtain product B;
3), make fire proofing material: according to will add water and firming agent join in product B according to certain mass ratio, mix homogeneously, The mass ratio of water, firming agent and product B is 2~6:30~50:30~50, i.e. obtains fire proofing material;
Described dispersant is triethyl group hexyl phosphoric acid, methyl anyl alcohol, vinyl bis-stearamides, glycerol monostearate, poly-second A kind of or arbitrary proportion in glycol and mono alkenyl succimide two or more;
Described defoamer is to join in the Guangdong bought on tributyl phosphate, phenethanol oleate, polydimethylsiloxane and market A kind of or arbitrary proportion in the middle federal special defoamer of B458 oiliness that Fine Chemical Co., Ltd of nation produces two or more;
Described fire retardant is the two or more of a kind of or arbitrary proportion in tripolyphosphate ammonium, boric acid and Borax;
Described powder is the two or more of a kind of or arbitrary proportion in calcium carbonate, aluminium hydroxide, aluminium oxide, potter's clay and cement;
Described diluent is methacrylic acid-beta-hydroxy ethyl ester, expoxy propane lauryl ether, butyl glycidyl ether, 1,4-fourth A kind of or arbitrary proportion in Hexanediol diglycidyl ether, benzyl glycidyl ether and ethyl acetate two or more;
Described modifying agent is the one in 1,6 hexanediol diacrylate, end carboxyl propylene glycol polyethers and polybutadiene or any Ratio two or more;
Described epoxy resin is alicyclic based epoxy resin, propane type epoxy resin of di phenolic group and glycidyl ester epoxy resin In a kind of or arbitrary proportion two or more;
Described firming agent be the one in triethylene tetramine, ethylenediamine, maleic anhydride and phthalic anhydride or arbitrarily than Example two or more.
Described powder fineness requirement is 1200 mesh~3000 mesh.
Shearing rotating speed described in step 1) is 1500 turns/min, and shear time is 40min;Defoamer is middle federal B458 oil The special defoamer of property;Dispersant is Polyethylene Glycol and the mono alkenyl succimide compositions according to mass ratio 1:2;Fire retardant is Tripolyphosphate ammonium;Powder is that calcium carbonate, aluminium hydroxide, aluminium oxide, potter's clay and cement are according to mass ratio 7:2:2:1:1;Diluent For methacrylic acid-beta-hydroxy ethyl ester;The mass ratio of defoamer, dispersant, fire retardant, powder and diluent is 2:1.5:1:390: 1000。
Step 2) described in epoxy resin be alicyclic based epoxy resin;Described modifying agent is 1,6-HD diacrylate Ester;The mass ratio of epoxy resin, modifying agent and product A is 75:5:20.
Firming agent described in step 3) is phthalic anhydride;The mass ratio of water, firming agent and product B is 4:50:46.
The present invention has a following Advantageous Effects:
1), good thermal stability of the present invention, owing to the epoxy radicals of cycloaliphatic epoxy resin is connected directly between on alicyclic ring, can be formed tight Close rigid molecular structure, after solidification, crosslink density increases, thus heat distortion temperature is higher, and Martin heat resistance can reach 190 More than DEG C, heat decomposition temperature is more than 360 DEG C.Cure shrinkage is little, and hot strength is high.The viscosity of cycloaliphatic epoxy resin all compares Little, when cast and compacting product, operation is more convenient, has superior mechanical performance and chemical proof and thermostability.
2), the present invention adds tripolyphosphate ammonium as fire retardant, environmental protection compared with traditional fire retardant PBDE Performance is higher.
3), the present invention matched by the multiple auxiliary agent such as dispersant and defoamer, powder can be made to be scattered in uniformly dilute Releasing in agent, product stability can be good.
4), the present invention by add modifying agent, the toughness of cycloaliphatic epoxy resin can be significantly improved, will not be because of warming plate Bending and cause coming off of fire proofing material.
5), the present invention use methacrylic acid-beta-hydroxy ethyl ester miscible with water as diluent, do not affect the addition of water, The aquation of cement will not be produced impact.
6), the present invention by cement and the cooperation of cycloaliphatic epoxy resin, form double shielding film, have the most waterproof Performance, is possible to prevent fire proofing material to come off because of rainwash.
7), the present invention can by spraying by the way of, coat and need on fireproof material, easy construction.
Detailed description of the invention
The present invention is further illustrated below in conjunction with instantiation.
Embodiment one
Make product A: defoamer, dispersant and fire retardant certain mass are set than joining the high shear filling diluent In Bei, being stirring evenly and then adding into the powder of certain mass, the mass ratio of defoamer, dispersant, fire retardant, powder and diluent is 2:1.5:1:390:1000, high speed shear certain time, it is fully dispersed in diluent to powder, obtains product A;Make and produce Product B: epoxy resin and modifying agent are joined in product A according to certain mass ratio, the matter of epoxy resin, modifying agent and product A Amount ratio is 75:5:20, and stirring is fully dispersed in diluent to epoxy resin and modifying agent, obtains product B;Make fire proofing wood Material: according to will add water and firming agent join in product B according to certain mass ratio, mix homogeneously, water, firming agent and product B Mass ratio is 4:50:46, i.e. obtains fire proofing material.
Embodiment two
Make product A: defoamer, dispersant and fire retardant certain mass are set than joining the high shear filling diluent In Bei, being stirring evenly and then adding into the powder of certain mass, the mass ratio of defoamer, dispersant, fire retardant, powder and diluent is 2:1.5:1:390:1000, high speed shear certain time, it is fully dispersed in diluent to powder, obtains product A;Make and produce Product B: epoxy resin and modifying agent are joined in product A according to certain mass ratio, the matter of epoxy resin, modifying agent and product A Amount ratio is 70:5:25, and stirring is fully dispersed in diluent to epoxy resin and modifying agent, obtains product B;Make fire proofing wood Material: according to will add water and firming agent join in product B according to certain mass ratio, the mass ratio of water, firming agent and product B is 4: 50:46, i.e. obtains fire proofing material.
Embodiment three
Make product A: defoamer, dispersant and fire retardant certain mass are set than joining the high shear filling diluent In Bei, being stirring evenly and then adding into the powder of certain mass, the mass ratio of defoamer, dispersant, fire retardant, powder and diluent is 2:1.5:1:390:1000, high speed shear certain time, it is fully dispersed in diluent to powder, obtains product A;Make and produce Product B: epoxy resin and modifying agent are joined in product A according to certain mass ratio, the matter of epoxy resin, modifying agent and product A Amount ratio is 80:5:15, and stirring is fully dispersed in diluent to epoxy resin and modifying agent, obtains product B;Make fire proofing wood Material: according to will add water and firming agent join in product B according to certain mass ratio, the mass ratio of water, firming agent and product B is 4: 50:46, i.e. obtains fire proofing material.
Embodiment four
Make product A: defoamer, dispersant and fire retardant certain mass are set than joining the high shear filling diluent In Bei, being stirring evenly and then adding into the powder of certain mass, the mass ratio of defoamer, dispersant, fire retardant, powder and diluent is 2:1.5:1:390:1000, high speed shear certain time, it is fully dispersed in diluent to powder, obtains product A;Make and produce Product B: epoxy resin and modifying agent are joined in product A according to certain mass ratio, the matter of epoxy resin, modifying agent and product A Amount ratio is 75:10:15, and stirring is fully dispersed in diluent to epoxy resin and modifying agent, obtains product B;Make fire proofing wood Material: according to will add water and firming agent join in product B according to certain mass ratio, the mass ratio of water, firming agent and product B is 4: 50:46, i.e. obtains fire proofing material.
In embodiment 1 to 4, described shearing rotating speed is 1500 turns/min, and shear time is 40min;Defoamer is middle federation The special defoamer of B458 oiliness;Dispersant is Polyethylene Glycol and the mono alkenyl succimide compositions according to mass ratio 1:2;Resistance Combustion agent is tripolyphosphate ammonium;Powder is that calcium carbonate, aluminium hydroxide, aluminium oxide, potter's clay and cement are according to mass ratio 7:2:2:1:1; Diluent is methacrylic acid-beta-hydroxy ethyl ester;Epoxy resin is alicyclic based epoxy resin;Described modifying agent is 1,6-HD Diacrylate.
Beneficial effects of the present invention is further illustrated below in conjunction with experimental data:
1, experiment material to be tested
1 materials and methods:
1.1 materials to be tested: the common fire proofing material of the present invention (in addition to not adding fire retardant and modifying agent, other technique and embodiment 1 one Cause), embodiment 1, embodiment 2, embodiment 3 and embodiment 4 do effectiveness comparison.
1.3 EXPERIMENTAL DESIGN: test set 5 process, by common fire proofing material (in addition to not adding fire retardant and modifying agent, other Technique is consistent with embodiment 1), embodiment 1, embodiment 2, embodiment 3 and embodiment 4 spray to polystyrene foam insulation respectively On plate, the same angle of alternating bending 40 times, observe insulation material with or without coming off;By common fire proofing material (except do not add fire retardant and Outside modifying agent, other technique is consistent with embodiment 1), embodiment 1, embodiment 2, embodiment 3 and embodiment 4 spray to polyphenyl second On alkene foam heat-insulating board, soak 45 days in water, observe insulation material with or without damage;Common fire proofing material is (fire-retardant except not adding Outside agent and modifying agent, other technique is consistent with embodiment 1), embodiment 1, embodiment 2, embodiment 3 and embodiment 4 spray to gather On styrenic foams warming plate, roasting under naked light.
This experiment other conditions in addition to the embodiment difference used are the most consistent.
2 results and analysis
Spray common fire proofing material (in addition to not adding fire retardant and modifying agent, other technique is consistent with embodiment 1), embodiment 1, reality Execute the polystyrene foam warming plate of example 2, embodiment 3 and embodiment 4, alternating bending 40 times, spray the poly-of common fire proofing material Styrenic foams warming plate (in addition to not adding fire retardant and modifying agent, other technique is consistent with embodiment 1) when bending 30 times, Fire proofing material surface occurs in that peeling fold, and the polystyrene foam warming plate spraying embodiment 1 to 4 does not all observe peeling Buckling phenomena, illustrates that insulation material of the present invention anti-crimping ability is strong, good toughness;Common fire proofing material will be sprayed (fire-retardant except not adding Outside agent and modifying agent, other technique is consistent with embodiment 1), embodiment 1, embodiment 2, embodiment 3 and the polyphenyl second of embodiment 4 Alkene foam heat-insulating board inserts in water, and partial denudation in atmosphere, soaks in water 45 days and observes, spray common fire proofing material and (remove Not adding outside fire retardant and modifying agent, other technique is consistent with embodiment 1) polystyrene foam warming plate at water and air interface Local whiting, and played bubble, and the polystyrene foam warming plate spraying embodiment 1 to 4 all do not observed foaming phenomena, says Bright water resistance of the present invention is good;To spray common fire proofing material (in addition to not adding fire retardant and modifying agent, other technique and embodiment 1 is consistent), embodiment 1, embodiment 2, embodiment 3 and embodiment 4 polystyrene foam warming plate roasting under naked light, spray general The polystyrene foam warming plate of logical fire proofing material (in addition to not adding fire retardant and modifying agent, other technique is consistent with embodiment 1) Began to give off a peculiar smell when 4 minutes, and had flare to occur after 12 minutes, the polystyrene foam insulation of spraying embodiment 1 Plate has abnormal flavour to send after toasting 5 minutes, is baked to 20 minutes have no flare;The polystyrene foam of spraying embodiment 2 to 4 is protected Temperature plate has abnormal flavour to send in baking after 5 minutes, and 15 to 20/there is the appearance of flare, embodiment 1 effect optimum be described.

Claims (5)

1. the preparation method of a fire proofing material, it is characterised in that follow the steps below:
1) product A is made: defoamer, dispersant and fire retardant certain mass ratio is joined the high shear filling diluent In equipment, it is stirring evenly and then adding into the powder of certain mass, the mass ratio of defoamer, dispersant, fire retardant, powder and diluent It is 0.5~3:0.5~3:0.5~3:200~500:1000, high speed shear 20min~60min, is fully dispersed in powder dilute Release in agent, obtain product A;
2), product B is made: join in product A by epoxy resin and modifying agent according to certain mass ratio, epoxy resin, modification The mass ratio of agent and product A is 60~89:1~10:10~30, and stirring to epoxy resin and modifying agent is fully dispersed in diluent In, obtain product B;
3), make fire proofing material: according to will add water and firming agent join in product B according to certain mass ratio, mix homogeneously, The mass ratio of water, firming agent and product B is 2~6:30~50:30~50, i.e. obtains fire proofing material;
Described dispersant is triethyl group hexyl phosphoric acid, methyl anyl alcohol, vinyl bis-stearamides, glycerol monostearate, poly-second A kind of or arbitrary proportion in glycol and mono alkenyl succimide two or more;
Described defoamer is to join in the Guangdong bought on tributyl phosphate, phenethanol oleate, polydimethylsiloxane and market A kind of or arbitrary proportion in the middle federal special defoamer of B458 oiliness that Fine Chemical Co., Ltd of nation produces two or more;
Described fire retardant is the two or more of a kind of or arbitrary proportion in tripolyphosphate ammonium, boric acid and Borax;
Described powder is the two or more of a kind of or arbitrary proportion in calcium carbonate, aluminium hydroxide, aluminium oxide, potter's clay and cement;
Described diluent is methacrylic acid-beta-hydroxy ethyl ester, expoxy propane lauryl ether, butyl glycidyl ether, 1,4-fourth A kind of or arbitrary proportion in Hexanediol diglycidyl ether, benzyl glycidyl ether and ethyl acetate two or more;
Described modifying agent is the one in 1,6 hexanediol diacrylate, end carboxyl propylene glycol polyethers and polybutadiene or any Ratio two or more;
Described epoxy resin is alicyclic based epoxy resin, propane type epoxy resin of di phenolic group and glycidyl ester epoxy resin In a kind of or arbitrary proportion two or more;
Described firming agent be the one in triethylene tetramine, ethylenediamine, maleic anhydride and phthalic anhydride or arbitrarily than Example two or more.
2. the preparation method of fire proofing material as claimed in claim 1, it is characterised in that: described powder fineness requirement is 1200 mesh ~3000 mesh.
3. the preparation method of fire proofing material as claimed in claim 1, it is characterised in that: shearing rotating speed described in step 1) is 1500 turns/min, shear time is 40min;Defoamer is the middle federal special defoamer of B458 oiliness;Dispersant is Polyethylene Glycol With mono alkenyl succimide according to the compositions of mass ratio 1:2;Fire retardant is tripolyphosphate ammonium;Powder is calcium carbonate, hydrogen-oxygen Change aluminum, aluminium oxide, potter's clay and cement according to mass ratio 7:2:2:1:1;Diluent is methacrylic acid-beta-hydroxy ethyl ester;Defoamer, The mass ratio of dispersant, fire retardant, powder and diluent is 2:1.5:1:390:1000.
4. the preparation method of fire proofing material as claimed in claim 1, it is characterised in that: step 2) described in epoxy resin be fat Ring same clan epoxy resin;Described modifying agent is 1,6 hexanediol diacrylate;The quality of epoxy resin, modifying agent and product A Ratio is 75:5:20.
5. the preparation method of fire proofing material as claimed in claim 1, it is characterised in that: firming agent described in step 3) is adjacent benzene Dicarboxylic acid anhydride;The mass ratio of water, firming agent and product B is 4:50:46.
CN201610631874.6A 2016-08-04 2016-08-04 A kind of preparation method of fire proofing material Active CN106243632B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107151111A (en) * 2017-06-16 2017-09-12 济南大学 A kind of regeneration aggregate pervious concrete

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101508825A (en) * 2009-03-30 2009-08-19 汕头市骏码凯撒有限公司 Epoxy resin embedding glue and method for producing the same
CN101921557A (en) * 2010-08-30 2010-12-22 新高电子材料(中山)有限公司 Halogen-free flame-retardant adhesive composition and flexible copper-clad plate using same
CN105111984A (en) * 2015-08-06 2015-12-02 南京艾布纳密封技术有限公司 Environmental-friendly flame-retardant epoxy automobile hemming adhesive and preparation method therefor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101508825A (en) * 2009-03-30 2009-08-19 汕头市骏码凯撒有限公司 Epoxy resin embedding glue and method for producing the same
CN101921557A (en) * 2010-08-30 2010-12-22 新高电子材料(中山)有限公司 Halogen-free flame-retardant adhesive composition and flexible copper-clad plate using same
CN105111984A (en) * 2015-08-06 2015-12-02 南京艾布纳密封技术有限公司 Environmental-friendly flame-retardant epoxy automobile hemming adhesive and preparation method therefor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107151111A (en) * 2017-06-16 2017-09-12 济南大学 A kind of regeneration aggregate pervious concrete

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