CN109180898A - A kind of preparation method of waterborne polyurethane hot melt adhesive - Google Patents
A kind of preparation method of waterborne polyurethane hot melt adhesive Download PDFInfo
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- CN109180898A CN109180898A CN201810640074.XA CN201810640074A CN109180898A CN 109180898 A CN109180898 A CN 109180898A CN 201810640074 A CN201810640074 A CN 201810640074A CN 109180898 A CN109180898 A CN 109180898A
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- Prior art keywords
- hot melt
- melt adhesive
- waterborne polyurethane
- polyurethane hot
- preparation
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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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- 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
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- 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
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
-
- 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
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- 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
- C09J175/06—Polyurethanes from polyesters
-
- 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
- C09J175/08—Polyurethanes from polyethers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of preparation methods of waterborne polyurethane hot melt adhesive, take the pure and mild catalyst of a certain amount of polyether polyol, polyester polyols to be added in reaction kettle first, at a certain temperature vacuum distillation dehydration；Then under agitation, a certain amount of diisocyanate is being added into reaction kettle, after temperature reaction, is obtaining mix products；Backward resulting mix products in hydrophilic chain extender and small molecule chain extender is added, adjust temperature, the reaction was continued obtains reaction product；Neutralizer is distributed in distilled water, gained reaction product is added to above-mentioned neutralizer, high-speed stirred is to get arriving waterborne polyurethane hot melt adhesive.Preparation method of the invention has reaction condition mild, the advantages of low energy consumption, is liquid under gained hot melt adhesive room temperature, also has the characteristics that low melting glass, high solids content.
Description
Technical field
The present invention relates to hot melt adhesive technical field, in particular to a kind of polyurethane hot melt, specially a kind of aqueous poly- ammonia
The preparation method of ester hot melt adhesive.
Background technique
Polyurethane is a kind of multifunctional macromolecule synthetic material quickly grown, diversification and molecule due to raw material variety
The controllability of structure, can be made into the multiple products form such as foamed plastics, elastomer, coating, adhesive, purposes and its extensively.
Equally, by adjusting its raw material and formula, the multiple types of bonding between suitable a variety of materials, various different purposes be can be designed
Adhesive for polyurethane.Adhesive for polyurethane glue-line has excellent flexibility, impact resistance, chemical resistance, and has
Especially excellent resistance to low temperature and wearability is a kind of medium and high-grade adhesive.
Adhesive for polyurethane is developed in the fifties in last century, there is solvent type, emulsion-type and curable type three types, not only can be with
It is heating and curing, can also solidify at room temperature, it is easy to use, carbamate groups (- NHCOO-) or different chloric acid are contained on main chain
Ester group (- NCO).Its unique texture assigns its special performance, it can adapt to the bonding of various substrates, such as rubber, plastics, gold
Category, ceramics, timber, glass and fiber etc., oneself is formed a various in style, widely used industry so far, is eight big to close
At one of the important species in adhesive.
Most of polyurethane hot melt is all solid on the market at present, big in the prevalence of softening point height, melting viscosity
The disadvantages of cumbersome with construction technology.Hot melt adhesive can realize coating process, required equipment with aqueous polyurethane at normal temperature
It is also simple and convenient, therefore is more liked by industry, there is good market.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of waterborne polyurethane hot melt adhesive.Preparation method tool of the invention
There is the advantages of reaction condition is mild, and low energy consumption, is liquid under gained hot melt adhesive room temperature, also there is low melting glass, high solids content
The features such as.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of waterborne polyurethane hot melt adhesive, which comprises the following steps:
(1) the pure and mild 0.01-0.02 parts by weight catalysis of the polyester polyols of the polyether polyol, 5-10 parts by weight that take 30-40 parts by weight
Agent is added in reaction kettle, vacuum distillation dehydration 40-60 minutes at 110-120 DEG C, after cool to 70-80 DEG C；
(2) under agitation, 25-40 parts by weight diisocyanate is added into the reaction kettle of step (1), is warming up to 80-100
DEG C reaction 2-3 hours, obtain mix products；
(3) 3-5 part by weight of hydrophilic chain extender and 1-2 parts by weight small molecule chain extension are added into step (2) resulting mix products
Agent, adjustment temperature are 80-90 DEG C, and the reaction was continued 2-3 hours, obtains reaction product；
(4) neutralizer is distributed in distilled water, reaction product obtained by step (3) is added to above-mentioned neutralizer, high-speed stirred,
Obtain waterborne polyurethane hot melt adhesive.
Preferably, the polyether polyol is one of polytetrahydrofuran ether glycol, polyoxypropyleneglycol or a variety of.
Preferably, the polyester polyol is polyhexamethylene adipate glycol, in poly- decanedioic acid hexylene glycol esterdiol
It is one or more.
Preferably, the diisocyanate is methyl diphenylene diisocyanate.
Preferably, the catalyst is N,N-Dibenzylamine.
Preferably, the hydrophilic chain extender is second dihydroxy ethanesulfonic acid sodium, ethylenediamine base ethanesulfonic acid sodium or combinations thereof.
Preferably, the small molecule chain extender is one of butanediol, diethylene glycol (DEG) or trihydroxy methyl propionic acid or a variety of.
Preferably, the neutralizer is triethylamine.
Compared with prior art, the beneficial effects of the present invention are: method reaction condition of the invention is mild, low energy consumption, institute
Obtaining under hot melt adhesive room temperature is liquid, has the characteristics that low melting glass, high solids content.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of preparation method of waterborne polyurethane hot melt adhesive, which comprises the following steps:
(1) polytetrahydrofuran ether glycol of 30 parts by weight, the polyhexamethylene adipate glycol of 5 parts by weight and 0.01 parts by weight are taken
N,N-Dibenzylamine is added in reaction kettle, vacuum distillation dehydration 40 minutes at 110 DEG C, after cool to 70 DEG C；
(2) under agitation, 25 parts by weight methyl diphenylene diisocyanates are added into the reaction kettle of step (1), heat up
It is reacted 2 hours to 80 DEG C, obtains mix products；
(3) 3 parts by weight second dihydroxy ethanesulfonic acid sodium and 1 parts by weight butanediol are added into step (2) resulting mix products, adjusts
Whole temperature is 80 DEG C, and the reaction was continued 2 hours, obtains reaction product；
(4) neutralizer is distributed in suitable distilled water, reaction product obtained by step (3) is added to above-mentioned neutralizer, it is high
Speed stirs to arrive waterborne polyurethane hot melt adhesive.
Through detecting, gained waterborne polyurethane hot melt adhesive solid content be 50%, viscosity 200mPas, 130 DEG C of glue film fusing point.
Embodiment 2
A kind of preparation method of waterborne polyurethane hot melt adhesive, which comprises the following steps:
(1) polyoxypropyleneglycol of 35 parts by weight, the poly- decanedioic acid hexylene glycol esterdiol of 8 parts by weight and 0.015 parts by weight are taken
N,N-Dibenzylamine is added in reaction kettle, vacuum distillation dehydration 50 minutes at 115 DEG C, after cool to 75 DEG C；
(2) under agitation, 35 parts by weight methyl diphenylene diisocyanates are added into the reaction kettle of step (1), heat up
It is reacted 2.5 hours to 90 DEG C, obtains mix products；
(3) 4 parts by weight ethylenediamine base ethanesulfonic acid sodium and 1.5 parts by weight diethylene glycol (DEG)s are added into step (2) resulting mix products,
Adjusting temperature is 85 DEG C, and the reaction was continued 2.5 hours, obtains reaction product；
(4) neutralizer is distributed in distilled water, reaction product obtained by step (3) is added to above-mentioned neutralizer, high-speed stirred,
Obtain waterborne polyurethane hot melt adhesive.
Through detecting, gained waterborne polyurethane hot melt adhesive solid content be 52%, viscosity 250mPas, 120 DEG C of glue film fusing point.
Embodiment 3
A kind of preparation method of waterborne polyurethane hot melt adhesive, which comprises the following steps:
(1) polytetrahydrofuran ether glycol of 40 parts by weight, the poly- decanedioic acid hexylene glycol esterdiol of 10 parts by weight and 0.02 weight are taken
Part N,N-Dibenzylamine is added in reaction kettle, vacuum distillation dehydration 60 minutes at 120 DEG C, after cool to 80 DEG C；
(2) under agitation, 40 parts by weight methyl diphenylene diisocyanates are added into the reaction kettle of step (1), heat up
It is reacted 3 hours to 100 DEG C, obtains mix products；
(3) the second dihydroxy ethanesulfonic acid sodium and second that 5 parts by weight mass ratioes are 1:1 are added into step (2) resulting mix products
Two amido ethanesulfonic acid sodium and 2 parts by weight trihydroxy methyl propionic acid, adjustment temperature are 90 DEG C, and the reaction was continued 3 hours, obtain reaction and produce
Object；
(4) neutralizer is distributed in distilled water, reaction product obtained by step (3) is added to above-mentioned neutralizer, high-speed stirred,
Obtain waterborne polyurethane hot melt adhesive.
Through detecting, gained waterborne polyurethane hot melt adhesive solid content be 58%, viscosity 242mPas, 122 DEG C of glue film fusing point.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of preparation method of waterborne polyurethane hot melt adhesive, which comprises the following steps: (1) weigh 30-40 weight
The polyether polyol of part, the pure and mild 0.01-0.02 part by weight of catalyst of polyester polyols of 5-10 parts by weight are added in reaction kettle,
Vacuum distillation dehydration 40-60 minutes at 110-120 DEG C, after cool to 70-80 DEG C；(2) under agitation, to step (1)
25-40 parts by weight diisocyanate is added in reaction kettle, is warming up to 80-100 DEG C of reaction 2-3 hours, obtains mix products；(3)
3-5 part by weight of hydrophilic chain extender and 1-2 parts by weight small molecule chain extender, adjustment are added into step (2) resulting mix products
Temperature is 80-90 DEG C, and the reaction was continued 2-3 hours, obtains reaction product；(4) neutralizer is distributed in distilled water, by step
(3) gained reaction product is added to above-mentioned neutralizer, and high-speed stirred is to get arriving waterborne polyurethane hot melt adhesive.
2. the preparation method of waterborne polyurethane hot melt adhesive as described in claim 1, it is characterised in that: the polyether polyol is
One of polytetrahydrofuran ether glycol, polyoxypropyleneglycol are a variety of.
3. the preparation method of waterborne polyurethane hot melt adhesive as described in claim 1, it is characterised in that: the polyester polyol is
One of polyhexamethylene adipate glycol, poly- decanedioic acid hexylene glycol esterdiol are a variety of.
4. the preparation method of waterborne polyurethane hot melt adhesive as described in claim 1, it is characterised in that: the diisocyanate is
Methyl diphenylene diisocyanate.
5. the preparation method of waterborne polyurethane hot melt adhesive as described in claim 1, it is characterised in that: the catalyst is two
Quinoline Anaesthetie Ether.
6. the preparation method of waterborne polyurethane hot melt adhesive as described in claim 1, it is characterised in that: the hydrophilic chain extender is
Second dihydroxy ethanesulfonic acid sodium, ethylenediamine base ethanesulfonic acid sodium or combinations thereof.
7. the preparation method of waterborne polyurethane hot melt adhesive as described in claim 1, it is characterised in that: the small molecule chain extender
For one of butanediol, diethylene glycol (DEG) or trihydroxy methyl propionic acid or a variety of.
8. the preparation method of waterborne polyurethane hot melt adhesive as described in claim 1, it is characterised in that: the neutralizer is three second
Amine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810640074.XA CN109180898A (en) | 2018-06-21 | 2018-06-21 | A kind of preparation method of waterborne polyurethane hot melt adhesive |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810640074.XA CN109180898A (en) | 2018-06-21 | 2018-06-21 | A kind of preparation method of waterborne polyurethane hot melt adhesive |
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| Publication Number | Publication Date |
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| CN109180898A true CN109180898A (en) | 2019-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810640074.XA Pending CN109180898A (en) | 2018-06-21 | 2018-06-21 | A kind of preparation method of waterborne polyurethane hot melt adhesive |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336911A (en) * | 2021-05-24 | 2021-09-03 | 合肥科天水性科技有限责任公司 | Bio-based waterborne polyurethane hot melt adhesive and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06199974A (en) * | 1992-12-29 | 1994-07-19 | Nikka Chem Co Ltd | Polyurethane dispersion |
| CN103102861A (en) * | 2013-02-22 | 2013-05-15 | 中国工程物理研究院化工材料研究所 | Low-softening point thermoplastic polyurethane hot melt adhesive and preparation method thereof |
| CN103554415A (en) * | 2013-10-18 | 2014-02-05 | 广东银洋树脂有限公司 | Method for preparing waterborne polyurethane hot melt adhesive |
| CN104927747A (en) * | 2015-06-05 | 2015-09-23 | 华南理工大学 | Waterborne polyurethane hot melt adhesive as well as preparation method and application thereof |
-
2018
- 2018-06-21 CN CN201810640074.XA patent/CN109180898A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06199974A (en) * | 1992-12-29 | 1994-07-19 | Nikka Chem Co Ltd | Polyurethane dispersion |
| CN103102861A (en) * | 2013-02-22 | 2013-05-15 | 中国工程物理研究院化工材料研究所 | Low-softening point thermoplastic polyurethane hot melt adhesive and preparation method thereof |
| CN103554415A (en) * | 2013-10-18 | 2014-02-05 | 广东银洋树脂有限公司 | Method for preparing waterborne polyurethane hot melt adhesive |
| CN104927747A (en) * | 2015-06-05 | 2015-09-23 | 华南理工大学 | Waterborne polyurethane hot melt adhesive as well as preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336911A (en) * | 2021-05-24 | 2021-09-03 | 合肥科天水性科技有限责任公司 | Bio-based waterborne polyurethane hot melt adhesive and preparation method and application thereof |
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Application publication date: 20190111 |
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