CN104232006A - Novel flame-retardant polyurethane adhesive and preparation method thereof - Google Patents

Novel flame-retardant polyurethane adhesive and preparation method thereof Download PDF

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Publication number
CN104232006A
CN104232006A CN201410402110.0A CN201410402110A CN104232006A CN 104232006 A CN104232006 A CN 104232006A CN 201410402110 A CN201410402110 A CN 201410402110A CN 104232006 A CN104232006 A CN 104232006A
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China
Prior art keywords
polyurethane adhesive
component
preparation
retardant
novel flame
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CN201410402110.0A
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Chinese (zh)
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张敏
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TAICANG KANGSHENG CHEMICAL Co Ltd
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TAICANG KANGSHENG CHEMICAL Co Ltd
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Priority to CN201410402110.0A priority Critical patent/CN104232006A/en
Publication of CN104232006A publication Critical patent/CN104232006A/en
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Abstract

The invention provides a novel flame-retardant polyurethane adhesive and a preparation method thereof. The novel flame-retardant polyurethane adhesive is prepared from polytetrahydrofuran diol 1000, toluene diisocynate, a reaction type flame retardant, a chain extender and a cross-linking agent, wherein the reaction type flame retardant is dibromoneopentyl glycol; the chain extender is 1,4-butanediol; the cross-linking agent is trimethylolpropane. The preparation method comprises the following steps: (a) preparing a component A; (b) preparing a component B; and (c) preparing the polyurethane adhesive. The invention discloses the novel flame-retardant polyurethane adhesive and the preparation method thereof. The polyurethane adhesive is simple and feasible in production process, is not only excellent in flame retardant property, but also relatively long in service life, relatively good in thermal stability and relatively low in glass-transition temperature.

Description

A kind of novel flame-retardant polyurethane adhesive and preparation method thereof
Technical field
The present invention relates to a kind of tackiness agent, particularly relate to a kind of novel flame-retardant polyurethane adhesive and preparation method thereof, belong to field of adhesive technology.
Background technology
Tackiness agent is as the indispensable Chemicals of a kind of national economic development, be widely used in the every field in national economy, wherein, polyurethane adhesive is a kind of purposes adhesives widely, owing to containing carbamate groups and isocyanate group in its molecular chain, and these two kinds of groups have polarity and the strong feature of chemically reactive, and intermolecular energy forms hydrogen bond, therefore to a lot of material as leather, foam, glass, metal etc. have good chemical adhesive power.The raw material preparing polyurethane adhesive is generally polyvalent alcohol, chainextender and isocyanic ester etc., polyvalent alcohol is the main raw material preparing polyurethane adhesive, because its performance of difference of its molecular structure is also different, select the polyvalent alcohol of different relative molecular mass and different molecular structures can synthesize the polyurethane adhesive of different use properties.
At present, the application performance of the polyurethane adhesive that market is developed mostly concentrates on and improves its curing speed, tack, bonding strength and reduce the aspects such as bubble, these polyurethane adhesives are not mostly through fire-retardant finish, and urethane is combustiblematerials, meet fire can burn and produce a large amount of poisonous mist, therefore hinder polyurethane adhesive and be applied in wider scope.Although some polyurethane adhesive have passed through certain fire-retardant finish, flame retardant properties is general, and after fire-retardant finish, and working life of polyurethane adhesive, thermostability and second-order transition temperature are greatly affected, and over-all properties is general.
Summary of the invention
For the demand, the invention provides a kind of novel flame-retardant polyurethane adhesive and preparation method thereof, this polyurethane adhesive production technique is simple, and it not only has excellent flame retardant properties, and has longer working life, better thermostability and lower second-order transition temperature.
The present invention is a kind of novel flame-retardant polyurethane adhesive and preparation method thereof, described polyurethane adhesive is prepared from by polytetrahydrofuran diol 1000, tolylene diisocyanate, reactive flame retardant, chainextender and linking agent, described reactive flame retardant is dibromoneopentyl glycol, described chainextender is 1,4-butyleneglycol, described linking agent is TriMethylolPropane(TMP), and described preparation method comprises the steps: a) to prepare component A, b) prepare B component, c) produce polyurethane adhesive.
In a preferred embodiment of the present invention, each component that described component A comprises and mass percent are: 39.8% polytetrahydrofuran diol 1000,47.8% tolylene diisocyanate, 12.4% reactive flame retardant.
In a preferred embodiment of the present invention, each component that described B component comprises and mass percent are: 64.8% polytetrahydrofuran diol 1000,19.6% reactive flame retardant, 7.8% chainextender, 7.8% linking agent.
In a preferred embodiment of the present invention, the quality proportioning of described component A and B component is 8:5.
In a preferred embodiment of the present invention, in described step a), the processing condition of preparation component A are: temperature of reaction 80 DEG C, nitrogen protection lower reaction times 15min, vacuum outgas time 30min.
In a preferred embodiment of the present invention, in described step b), the processing condition of preparation B component are: whipping temp 80 DEG C, stirring velocity 400r/min, churning time 20min.
In a preferred embodiment of the present invention, in described step c), produce polyurethane adhesive and comprise the steps: 1) by component A and B component mixing, stir 10min and obtain batch mixing; 2) pour batch mixing into mould, be evacuated to bubble collapse in 80 DEG C; 3) mould is put into hydroponic box, in 50 DEG C of isothermal curing 10h.
Present invention is disclosed a kind of novel flame-retardant polyurethane adhesive and preparation method thereof, this polyurethane adhesive production technique is simple, it not only has excellent flame retardant properties, and has longer working life, better thermostability and lower second-order transition temperature.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation:
Fig. 1 is the process figure of embodiment of the present invention novel flame-retardant polyurethane adhesive preparation method.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
Fig. 1 is the process figure of embodiment of the present invention novel flame-retardant polyurethane adhesive preparation method; This polyurethane adhesive is prepared from by polytetrahydrofuran diol 1000, tolylene diisocyanate, reactive flame retardant, chainextender and linking agent, described reactive flame retardant is dibromoneopentyl glycol, described chainextender is 1,4-butyleneglycol, described linking agent is TriMethylolPropane(TMP), described preparation method comprises the steps: a) to prepare component A, b) prepares B component, c) produces polyurethane adhesive.
The novel flame-retardant polyurethane adhesive that the present invention mentions with polytetrahydrofuran diol 1000, tolylene diisocyanate for main raw material, introduce reactive flame retardant dibromoneopentyl glycol, chainextender 1,4-butyleneglycol, linking agent TriMethylolPropane(TMP), adopt semi-prepolymer method to be prepared.In this novel flame-retardant polyurethane adhesive preparation process, the component A of preparation and the quality proportioning of B component are 8:5; Wherein, each component of comprising of component A and mass percent are: 39.8% polytetrahydrofuran diol 1000,47.8% tolylene diisocyanate, 12.4% reactive flame retardant; Each component that B component comprises and mass percent are: 64.8% polytetrahydrofuran diol 1000,19.6% reactive flame retardant, 7.8% chainextender, 7.8% linking agent.Polytetrahydrofuran diol 1000 molecular chain that this novel flame-retardant polyurethane adhesive is selected is more submissive, can make reach 100min the working life of polyurethane adhesive, simultaneously, the molecular stuffing of polytetrahydrofuran diol 1000 is tight, molecular structure is not easily destroyed, after introducing reactive flame retardant dibromoneopentyl glycol, there is higher oxygen index, therefore polyurethane adhesive can be made to have better flame retardant effect.In addition, polytetrahydrofuran diol 1000 due to molecular chain more regular, more submissive as the molecule segment of soft section, therefore polyurethane binder can be made to have better thermostability, lower second-order transition temperature.
Embodiment
Concrete preparation method is as follows:
A) prepare component A, concrete preparation process is: by mass percentage, and first 39.8% polytetrahydrofuran diol 1000,47.8% tolylene diisocyanate, 12.4% reactive flame retardant are put into reactor, be heated to 80 DEG C, rapid stirring is even; Then 15min is reacted under nitrogen protection; Last vacuum outgas 30min, namely obtains component A polymeric polyisocyanate performed polymer, and sealing is preserved stand-by.
B) prepare B component, concrete preparation process is: by mass percentage, first 64.8% polytetrahydrofuran diol 1000,19.6% reactive flame retardant, 7.8% chainextender, 7.8% linking agent is put into reactor, is heated to 80 DEG C; Then stir 20min with 400r/min rotating speed, mix, namely obtain B component colourless transparent liquid, sealed type storage is for subsequent use.
C) produce polyurethane adhesive, concrete preparation process is: B component 8:5 mixing in mass ratio prepared by the component A first at room temperature step a) prepared and step b), and stirring velocity is 300r/min, obtains batch mixing after stirring 10min; Then pour batch mixing into mould, vacuumize until bubble collapse in 80 DEG C; Finally mould is put into hydroponic box, in 50 DEG C of isothermal curing 10h, namely obtain the novel flame-retardant polyurethane adhesive of excellent performance.
Present invention is disclosed a kind of novel flame-retardant polyurethane adhesive and preparation method thereof, this polyurethane adhesive production technique is simple, it not only has excellent flame retardant properties, and has longer working life, better thermostability and lower second-order transition temperature.
The above; be only the specific embodiment of the present invention; but protection scope of the present invention is not limited thereto; any those of ordinary skill in the art are in the technical scope disclosed by the present invention; the change can expected without creative work or replacement, all should be encompassed within protection scope of the present invention.Therefore, the protection domain that protection scope of the present invention should limit with claims is as the criterion.

Claims (7)

1. novel flame-retardant polyurethane adhesive and preparation method thereof, it is characterized in that, described polyurethane adhesive is prepared from by polytetrahydrofuran diol 1000, tolylene diisocyanate, reactive flame retardant, chainextender and linking agent, described reactive flame retardant is dibromoneopentyl glycol, described chainextender is 1,4-butyleneglycol, described linking agent is TriMethylolPropane(TMP), described preparation method comprises the steps: a) to prepare component A, b) prepare B component, c) produce polyurethane adhesive.
2. novel flame-retardant polyurethane adhesive according to claim 1 and preparation method thereof, it is characterized in that, each component that described component A comprises and mass percent are: 39.8% polytetrahydrofuran diol 1000,47.8% tolylene diisocyanate, 12.4% reactive flame retardant.
3. novel flame-retardant polyurethane adhesive according to claim 1 and preparation method thereof, it is characterized in that, each component that described B component comprises and mass percent are: 64.8% polytetrahydrofuran diol 1000,19.6% reactive flame retardant, 7.8% chainextender, 7.8% linking agent.
4. novel flame-retardant polyurethane adhesive according to claim 1 and preparation method thereof, is characterized in that, the quality proportioning of described component A and B component is 8:5.
5. novel flame-retardant polyurethane adhesive according to claim 1 and preparation method thereof; it is characterized in that; in described step a), the processing condition of preparation component A are: temperature of reaction 80 DEG C, nitrogen protection lower reaction times 15min, vacuum outgas time 30min.
6. novel flame-retardant polyurethane adhesive according to claim 1 and preparation method thereof, is characterized in that, in described step b), the processing condition of preparation B component are: whipping temp 80 DEG C, stirring velocity 400r/min, churning time 20min.
7. novel flame-retardant polyurethane adhesive according to claim 1 and preparation method thereof, is characterized in that, in described step c), produces polyurethane adhesive and comprises the steps: 1) by component A and B component mixing, stir 10min and obtain batch mixing; 2) pour batch mixing into mould, be evacuated to bubble collapse in 80 DEG C; 3) mould is put into hydroponic box, in 50 DEG C of isothermal curing 10h.
CN201410402110.0A 2014-08-15 2014-08-15 Novel flame-retardant polyurethane adhesive and preparation method thereof Pending CN104232006A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061723A (en) * 2015-08-11 2015-11-18 北京海月星科技有限公司 PU (polyurethane) daub and preparation method thereof
CN106221654A (en) * 2016-02-02 2016-12-14 北京理工大学 A kind of flame retardant bicomponent adhesive for polyurethane and preparation method thereof
CN106833352A (en) * 2017-03-21 2017-06-13 新疆科能防水防护技术股份有限公司 A kind of water conservancy project protective coating and preparation method thereof
CN107722908A (en) * 2017-11-14 2018-02-23 温州包鹿新材料有限公司 A kind of preparation method of polyurethane fireproof glue for building

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1978481A (en) * 2005-12-01 2007-06-13 天津科技大学 Self-extinguishing waterborn polyurethane material
WO2008149641A1 (en) * 2007-06-06 2008-12-11 Mitsui Chemicals Polyurethanes, Inc. Solventless laminating adhesive and process for production of composite film
CN101550327A (en) * 2008-04-03 2009-10-07 航天材料及工艺研究所 High hardness high-toughness polyurethane casting compound and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1978481A (en) * 2005-12-01 2007-06-13 天津科技大学 Self-extinguishing waterborn polyurethane material
WO2008149641A1 (en) * 2007-06-06 2008-12-11 Mitsui Chemicals Polyurethanes, Inc. Solventless laminating adhesive and process for production of composite film
CN101550327A (en) * 2008-04-03 2009-10-07 航天材料及工艺研究所 High hardness high-toughness polyurethane casting compound and application thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105061723A (en) * 2015-08-11 2015-11-18 北京海月星科技有限公司 PU (polyurethane) daub and preparation method thereof
CN105061723B (en) * 2015-08-11 2018-05-04 北京海月星科技有限公司 A kind of polyurethane clay and preparation method thereof
CN106221654A (en) * 2016-02-02 2016-12-14 北京理工大学 A kind of flame retardant bicomponent adhesive for polyurethane and preparation method thereof
CN106221654B (en) * 2016-02-02 2019-08-23 北京理工大学 A kind of flame retardant bicomponent adhesive for polyurethane and preparation method thereof
CN106833352A (en) * 2017-03-21 2017-06-13 新疆科能防水防护技术股份有限公司 A kind of water conservancy project protective coating and preparation method thereof
CN107722908A (en) * 2017-11-14 2018-02-23 温州包鹿新材料有限公司 A kind of preparation method of polyurethane fireproof glue for building
CN107722908B (en) * 2017-11-14 2019-09-27 骏能化工(龙南)有限公司 A kind of preparation method of polyurethane fireproof glue for building

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Application publication date: 20141224