CN101676353A - Waterborne flame retardant adhesive and preparation method thereof - Google Patents

Waterborne flame retardant adhesive and preparation method thereof Download PDF

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Publication number
CN101676353A
CN101676353A CN200810200140A CN200810200140A CN101676353A CN 101676353 A CN101676353 A CN 101676353A CN 200810200140 A CN200810200140 A CN 200810200140A CN 200810200140 A CN200810200140 A CN 200810200140A CN 101676353 A CN101676353 A CN 101676353A
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CN
China
Prior art keywords
flame retardant
retardant adhesive
initiator
waterborne
waterborne flame
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN200810200140A
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Chinese (zh)
Inventor
刘国富
赵永旗
毛继明
戚向东
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SHANGHAI QXQC CHEMICAL TECHNOLOGY JOINT-STOCK Co Ltd
Original Assignee
SHANGHAI QXQC CHEMICAL TECHNOLOGY JOINT-STOCK Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by SHANGHAI QXQC CHEMICAL TECHNOLOGY JOINT-STOCK Co Ltd filed Critical SHANGHAI QXQC CHEMICAL TECHNOLOGY JOINT-STOCK Co Ltd
Priority to CN200810200140A priority Critical patent/CN101676353A/en
Publication of CN101676353A publication Critical patent/CN101676353A/en
Pending legal-status Critical Current

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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention provides a waterborne flame retardant adhesive used for external packages for installation, such as heat insulating materials, which is mainly prepared by reacting acrylic acid, methacrylic acid, butyl acrylate, ethyl acrylate, styrene, a functional monomer, an initiator, an emulsifier, a buffering agent, functional auxiliaries, a pH regulator, softened water and aluminium hydroxide.The invention also provides a preparation method of the waterborne flame retardant adhesive. The waterborne flame retardant adhesive is nontoxic, safe and environment-friendly. Stable blending emulsion is prepared by adding a given quantity of inorganic particles to a waterborne emulsion system to undergo full blending. The additive subjected to flame retardant treatment can be applied to the fields which are strict with the requirements of thermal properties. the cost of the waterborne flame retardant adhesive is greatly lowered and the raw materials of the waterborne flame retardant adhesive are obtained more easily and conveniently.

Description

Waterborne flame retardant adhesive and preparation method thereof
Technical field
The present invention relates to a kind of lagging material etc. of being used for waterborne flame retardant tackiness agent of outsourcing and preparation method thereof is installed, relate in particular to a kind of waterborne flame retardant adhesive and preparation method thereof.
Background technology
Flame-retarding adhesive glue is to compare specialty products in the tackiness agent series product, mainly be coated on the surface of wrapping material such as paper, polyester film, the centre sandwiches fire retardant materials such as asbestos, carry out the compound of thin-film material then, this composite prod is mainly used in installation outsourcings such as lagging material, is present popular lagging material form of construction work.
Fire-retardant in general superpolymer is compared with not fire-retardant same type of material, higher thermostability, lower rate of combustion is arranged, and be difficult to light.But at high temperature still produce so property gas, when condition is sufficient, still can burn.Some fire retardant materials are very difficult to light, and other fire retardant materials may can more easily be lighted under some test condition, and as the material of expandable flame retardant system, after lighting, burning is then put out certainly when the charcoal foam layer forms, thereby reached fire-retardant purpose a little while.
At present for being in great demand of flame-retarding adhesive, still seldom to the research in this field.Tackiness agent belongs to macromolecular compound, satisfies superpolymer incendiary general condition, if without fire-retardant finish, just can't use this fire-retardant field that requires.Now the fire retardant glue on the market mostly all is to adopt oily matter for producing main raw material, raw materials cost height not only, and contain many isolating harmful chemical substances that are difficult to, as the benzene class.Along with the mankind to the improving constantly of health requirements, the use range of such glue more and more is restricted, scope is more and more littler.Because there is obvious contradiction in the defective of the requirement in market and present fire retardant glue itself, the many producers in the heat-insulating and fire-proof industry can only adopt the tackiness agent of other types to replace to restricted product.Therefore, waterborne flame retardant adhesive has very big development space on the market.
Summary of the invention
Purpose of the present invention provides a kind of waterborne flame retardant adhesive exactly in order to address the above problem.
Another object of the present invention is to provide a kind of method for preparing waterborne flame retardant adhesive of the present invention.
The object of the present invention is achieved like this:
The invention discloses a kind of waterborne flame retardant adhesive, form by prepared in reaction: vinylformic acid, methacrylic acid, butyl acrylate, ethyl propenoate by following component, vinylbenzene, functional monomer, initiator, emulsifying agent, buffer reagent, functional aid, pH adjusts agent, softening water, aluminium hydroxide;
Described functional monomer is selected from least a in Phthalic acid, diallyl ester, Hydroxyethyl acrylate and the N hydroxymethyl acrylamide;
Described initiator is an ammonium persulphate;
Described emulsifying agent is selected from least a in sulfosuccinate and the phenolic ether sulphate;
Described buffer reagent is selected from least a in bicarbonate of ammonia and the sodium bicarbonate;
Described functional aid is selected from least a among OT75, mineral oil and the water soluble acrylic resin;
It is ammoniacal liquor that described pH adjusts agent;
The shared weight percent of above-mentioned each component is respectively: vinylformic acid 1~5%, methacrylic acid 1~5%, butyl acrylate 10~15%, ethyl propenoate 10~15%, vinylbenzene 10~20%; Functional monomer comprises Phthalic acid, diallyl ester 0~5%, Hydroxyethyl acrylate 0~5%, N hydroxymethyl acrylamide 0~5%; Initiator comprises ammonium persulphate 0~2%; Emulsifying agent comprises sulfosuccinate 0~2%, phenolic ether sulphate 0~5%; Buffer reagent comprises bicarbonate of ammonia 0~2%, sodium bicarbonate 0~1%; Functional aid comprises OT75 0~3%, mineral oil 0~1%, and the water soluble acrylic resin 0~2%; PH adjusts agent: ammoniacal liquor 0~5%; Softening water 25~40%; Aluminium hydroxide 5~10%.
Raw material of the present invention is that general raw material gets by market purchasing.
The present invention also provides a kind of preparation method of water soluble flocking glue of the present invention, realizes by following steps:
(a) quantitative emulsifying agent, buffer reagent, softening water are joined in the reactor, obtain mixing raw material after stirring and be warming up to 75~90 ℃;
(b) quantitative vinylformic acid, methacrylic acid, butyl acrylate, ethyl propenoate, vinylbenzene, functional monomer, emulsifying agent, buffer reagent are joined in the pre-emulsification still, stir and obtain mixing raw material after 30 minutes, emit wherein 1~15% as seed liquor;
(c) mixing raw material in the step a reactor is warming up to 80~90 ℃, drop into the seed liquor among the step b after, add initiator and softening water again, control temperature of reaction kettle to 80~90 ℃;
(d) with in the remaining mixing raw material in quantitative initiator, functional monomer and the pre-emulsification still of softening water adding step b, stir and obtain compound;
(e) compound that steps d is obtained splashes in the reactor, and temperature is controlled at 80~90 ℃, and the dropping time is 2~4 hours;
(f) dropwise after, maintain the temperature at 80~90 ℃, react after 1~3 hour, be cooled to 50~60 ℃;
(g) add functional aid and aluminium hydroxide, treat that temperature reduces to 40 ℃, adjust discharging after the viscosity.
Compared with prior art, the invention has the beneficial effects as follows: nontoxicity, safety and environmental protection.Add a certain amount of inorganic particulate by hydrotropisms's emulsion system, through mixing fully, thereby prepare stable blending emulsion, the tackiness agent of process fire-retardant finish can be applied to the field that thermal property requires the comparison strictness.And cost has the decline of big cost, and raw material sources are more prone to and make things convenient for.
Embodiment
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1 (unit: kilogram)
Prescription:
Reactor:
1. softening water 180 phenolic ether sulphates 2 bicarbonate of ammonia 0.2 sodium bicarbonate 0.3
2. softening water 17 ammonium persulphates 4
Pre-emulsification still:
3. softening water 115 phenolic ether sulphates 4 sulfosuccinates 1 bicarbonate of ammonia 0.2
4. butyl acrylate 140 ethyl propenoates 120 vinylbenzene 140 Phthalic acid, diallyl esters 5 Hydroxyethyl acrylates 5 vinylformic acid 8 methacrylic acids 7
5. softening water 8 N hydroxymethyl acrylamides 2
6. softening water 18 ammonium persulphates 4
7. mineral oil 1
8.OT75?3
9. the water soluble acrylic resin 10
10. aluminium hydroxide 10
11. ammoniacal liquor 8
Operation steps:
Reactor is joined rebasing liquid 1 in order, starts then to stir to be warming up to 78 ℃; Start pre-emulsification still and stir, join pre-emulsification kettle base solution 3; Be sequentially added into monomer 4 then, stir after 30 minutes, emit 30 kilograms of seed liquor; When the rebasing liquid 1 of reactor rises to 88 ℃, drop into seed liquor; And then add reactor towards still liquid 2; 85~86 ℃ of control temperature of reaction kettle; After raw material added 5,6 in the pre-emulsification still, beginning dripped in reactor, and temperature is controlled at 83~84 ℃, and the dropping time is 3~3.5 hours; After dripping end, be warming up to 88 ℃, be incubated 2 hours; Cool the temperature to 60 ℃ then, add 7, temperature is reduced to 50 ℃, adds 8,9 and 10, when temperature is reduced to 40 ℃, adds 11 and adjusts the viscosity discharging.
Embodiment 2 (unit: kilogram)
Prescription:
Reactor:
1. softening water 200 sulfosuccinates 3 bicarbonate of ammonia 0.2 sodium bicarbonate 0.3
2. softening water 17 ammonium persulphates 4
Pre-emulsification still:
3. softening water 95 phenolic ether sulphates 4 sulfosuccinates 1 bicarbonate of ammonia 0.2
4. butyl acrylate 160 ethyl propenoates 120 vinylbenzene 120 Phthalic acid, diallyl esters 3 Hydroxyethyl acrylates 3 vinylformic acid 3 methacrylic acids 7
5. softening water 8 N hydroxymethyl acrylamides 2
6. softening water 18 ammonium persulphates 4
7. mineral oil 1
8.OT75?3
9. the water soluble acrylic resin 10
10. aluminium hydroxide 10
Operation steps
Reactor is joined rebasing liquid 1 in order, starts then to stir to be warming up to 78 ℃; Start pre-emulsification still and stir, join pre-emulsification kettle base solution 3; Be sequentially added into monomer 4 then, stir after 30 minutes, emit 30 kilograms of seed liquor; When the rebasing liquid 1 of reactor rises to 88 ℃, drop into seed liquor; And then add reactor towards still liquid 2; 85~86 ℃ of control temperature of reaction kettle; After raw material added 5,6 in the pre-emulsification still, beginning dripped in reactor, and temperature is controlled at 83~84 ℃, and the dropping time is 3~3.5 hours; After dripping end, be warming up to 88 ℃, be incubated 2 hours; Cool the temperature to 60 ℃ then, add 7, temperature is reduced to 50 ℃, adds 8,9 and 10, when temperature is reduced to 40 ℃, adjusts discharging after the viscosity.

Claims (3)

1. a waterborne flame retardant adhesive is formed by prepared in reaction by following component: vinylformic acid, methacrylic acid, butyl acrylate, ethyl propenoate, vinylbenzene, functional monomer, initiator, emulsifying agent, buffer reagent, functional aid, pH adjusts agent, softening water, aluminium hydroxide;
Described functional monomer is selected from least a in Phthalic acid, diallyl ester, Hydroxyethyl acrylate and the N hydroxymethyl acrylamide;
Described initiator is a persulphate;
Described emulsifying agent is selected from least a in sulfosuccinate and the phenolic ether sulphate;
Described buffer reagent is selected from least a in bicarbonate of ammonia and the sodium bicarbonate;
Described functional aid is selected from least a among OT75, mineral oil and the water soluble acrylic resin;
It is ammoniacal liquor that described pH adjusts agent;
The shared weight percent of above-mentioned each component is respectively: vinylformic acid 1~5%, methacrylic acid 1~5%, butyl acrylate 10~15%, ethyl propenoate 10~15%, vinylbenzene 10~20%; Functional monomer comprises Phthalic acid, diallyl ester 0~5%, Hydroxyethyl acrylate 0~5%, N hydroxymethyl acrylamide 0~5%; Initiator comprises ammonium persulphate 0~2%; Emulsifying agent comprises sulfosuccinate 0~2%, phenolic ether sulphate 0~5%; Buffer reagent comprises bicarbonate of ammonia 0~2%, sodium bicarbonate 0~1%; Functional aid comprises OT750~3%, mineral oil 0~1%, and the water soluble acrylic resin 0~2%; PH adjusts agent: ammoniacal liquor 0~5%; Softening water 25~40%; Aluminium hydroxide 5~10%.
2. waterborne flame retardant adhesive as claimed in claim 1 is characterized in that, described initiator is an ammonium persulphate.
3. one kind prepares the method for waterborne flame retardant adhesive according to claim 1, may further comprise the steps:
(a) quantitative emulsifying agent, buffer reagent, softening water are joined in the reactor, obtain mixing raw material after stirring and be warming up to 75~90 ℃;
(b) quantitative vinylformic acid, methacrylic acid, butyl acrylate, ethyl propenoate, vinylbenzene, functional monomer, emulsifying agent, buffer reagent are joined in the pre-emulsification still, stir and obtain mixing raw material after 30 minutes, emit wherein 1~15% as seed liquor;
(c) mixing raw material in the step a reactor is warming up to 80~90 ℃, drop into the seed liquor among the step b after, add initiator and softening water again, control temperature of reaction kettle to 80~90 ℃;
(d) with in the remaining mixing raw material in quantitative initiator, functional monomer and the pre-emulsification still of softening water adding step b, stir and obtain compound;
(e) compound that steps d is obtained splashes in the reactor, and temperature is controlled at 80~90 ℃, and the dropping time is 2~4 hours;
(f) dropwise after, maintain the temperature at 80~90 ℃, react after 1~3 hour, be cooled to 50~60 ℃;
(g) add functional aid and aluminium hydroxide, treat that temperature reduces to 40 ℃, adjust discharging after the viscosity.
CN200810200140A 2008-09-19 2008-09-19 Waterborne flame retardant adhesive and preparation method thereof Pending CN101676353A (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
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CN101676353A true CN101676353A (en) 2010-03-24

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103304711A (en) * 2013-06-19 2013-09-18 中南大学 Preparation method of resin-wrapped aluminum hydroxide
CN103965813A (en) * 2013-01-31 2014-08-06 日东电工株式会社 Flame-retardant adhesive composition
CN105754522A (en) * 2014-12-16 2016-07-13 浙江新力化工有限公司 Flame retardant adhesive for glass fiber grid positioning and preparation method thereof
CN106752601A (en) * 2016-12-30 2017-05-31 上海奇想青晨新材料科技股份有限公司 A kind of carbon titanium water-base resin anti-flaming dope and preparation method thereof
CN107216836A (en) * 2017-07-19 2017-09-29 东莞市联洲知识产权运营管理有限公司 A kind of preparation method of two-component fire retarding wood adhesive A B glue
CN112126383A (en) * 2020-09-11 2020-12-25 陈会杰 Flame-retardant acrylic pressure-sensitive adhesive and preparation method thereof
CN112143421A (en) * 2020-09-01 2020-12-29 许贵真 Preparation method of flame-retardant high-solid-content acrylic pressure-sensitive adhesive

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103965813A (en) * 2013-01-31 2014-08-06 日东电工株式会社 Flame-retardant adhesive composition
CN103304711A (en) * 2013-06-19 2013-09-18 中南大学 Preparation method of resin-wrapped aluminum hydroxide
CN103304711B (en) * 2013-06-19 2015-04-22 中南大学 Preparation method of resin-wrapped aluminum hydroxide
CN105754522A (en) * 2014-12-16 2016-07-13 浙江新力化工有限公司 Flame retardant adhesive for glass fiber grid positioning and preparation method thereof
CN105754522B (en) * 2014-12-16 2018-08-21 浙江科力森化学有限公司 Fire retardant glue and preparation method thereof for fiberglass gridding positioning
CN106752601A (en) * 2016-12-30 2017-05-31 上海奇想青晨新材料科技股份有限公司 A kind of carbon titanium water-base resin anti-flaming dope and preparation method thereof
CN107216836A (en) * 2017-07-19 2017-09-29 东莞市联洲知识产权运营管理有限公司 A kind of preparation method of two-component fire retarding wood adhesive A B glue
CN112143421A (en) * 2020-09-01 2020-12-29 许贵真 Preparation method of flame-retardant high-solid-content acrylic pressure-sensitive adhesive
CN112126383A (en) * 2020-09-11 2020-12-25 陈会杰 Flame-retardant acrylic pressure-sensitive adhesive and preparation method thereof

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Open date: 20100324