CN108977157A - A kind of Aqueous Polyurethane Adhesives and preparation method thereof - Google Patents
A kind of Aqueous Polyurethane Adhesives and preparation method thereof Download PDFInfo
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- CN108977157A CN108977157A CN201810936189.3A CN201810936189A CN108977157A CN 108977157 A CN108977157 A CN 108977157A CN 201810936189 A CN201810936189 A CN 201810936189A CN 108977157 A CN108977157 A CN 108977157A
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- Prior art keywords
- aqueous polyurethane
- parts
- polyurethane adhesives
- glycol
- diisocyanate
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Classifications
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- 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
-
- 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)
- Adhesives Or Adhesive Processes (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of Aqueous Polyurethane Adhesives and preparation method thereof, the raw material comprising following parts by weight: 44~46 parts of base polyurethane prepolymer for use as, 53.5~55.5 parts of deionized water, 2~3 parts of neutralizer and 0.01~0.5 part of amine chain extender.The Aqueous Polyurethane Adhesives are the aqueous polyurethanes that solid content is 45%, good using tack, and formation emulsion intercalation method is good, and viscosity is lower.It can be used for the fields such as surface covering, the adhesive of flexible parent metal.
Description
Technical field
The present invention relates to adhesive preparation fields more particularly to a kind of Aqueous Polyurethane Adhesives and preparation method thereof.
Background technique
Aqueous polyurethane is that a kind of design is strong, the novel aqueous high molecular material of environment-friendly and green, can be applied to fabric painting
The various fields such as layer, coating, adhesive, fibre trimmer.The enhancing of people's environmental consciousness and government are for VOC in recent years
The formulation of relevant policies, aqueous polyurethane replace conventional organic solvents as decentralized medium using water, application process is nontoxic, it is safe,
Low VOC shows the trend that aqueous polyurethane gradually substitutes solvent borne polyurethane.How to provide a kind of can substitute the poly- ammonia of solvent borne
The aqueous polyurethane of ester is problem to be solved.
Summary of the invention
Based on the problems of prior art, the object of the present invention is to provide a kind of Aqueous Polyurethane Adhesives and its systems
Preparation Method, can substitute solvent borne polyurethane, nontoxic, safety and VOC is low.
The purpose of the present invention is what is be achieved through the following technical solutions:
Embodiment of the present invention provides a kind of Aqueous Polyurethane Adhesives, the raw material comprising following parts by weight:
44~46 parts of base polyurethane prepolymer for use as, 53.5~55.5 parts of deionized water, 2~3 parts of neutralizer and amine chain extender
0.01~0.5 part.
Embodiment of the present invention also provides a kind of preparation method of Aqueous Polyurethane Adhesives, is used to prepare of the present invention
Aqueous Polyurethane Adhesives, comprising the following steps:
The each component of the Aqueous Polyurethane Adhesives is taken by formula of the present invention；
(1) it prepares the base polyurethane prepolymer for use as containing hydrophilic monomer: pressing base polyurethane prepolymer for use as formula for polyalcohol, diisocyanate
Ester, hydrophilic monomer react 2h at a temperature of 80~90 DEG C, and polyol chain extender is then added and reacts 2~4h, until-NCO's contains
Amount reaches theoretical value, and performed polymer obtained is the base polyurethane prepolymer for use as containing hydrophilic monomer；
(2) neutralization reaction: being cooled to 25~45 DEG C for performed polymer made from the step (1), and neutralizer reaction 15 is added
~20min；
(3) under the shear action of high speed disperser, amine emulsion dispersion: is added into the reaction solution of the step (2)
The solution of chain extender and deionized water mixing, 20~30min of emulsion dispersion, aqueous polyurethane emulsion obtained is aqueous poly- ammonia
Ester adhesive.
As seen from the above technical solution provided by the invention, Aqueous Polyurethane Adhesives provided in an embodiment of the present invention
And preparation method thereof, it has the advantage that:
This method simple process, the Aqueous Polyurethane Adhesives solid content of preparation 45% or so, viscosity 60~
900mpas, stability are good, tack is excellent, aluminize transfer adhesive, alloy corrosion-resistant field applied to cigarette packet, have nontoxic, safety
And the advantage that VOC is low, alternative solvent borne polyurethane.
Specific embodiment
Below with reference to particular content of the invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts,
Belong to protection scope of the present invention.The content being not described in detail in the embodiment of the present invention belongs to professional and technical personnel in the field
The well known prior art.
The embodiment of the present invention provides a kind of Aqueous Polyurethane Adhesives, the raw material comprising following parts by weight:
44~46 parts of base polyurethane prepolymer for use as, 53.5~55.5 parts of deionized water, 2~3 parts of neutralizer and amine chain extender
0.01~0.5 part.
In above-mentioned adhesive, base polyurethane prepolymer for use as is prepared by following raw material in parts by weight, comprising:
67~68 parts of polyalcohol, 23~24 parts of diisocyanate, 4~5 parts of hydrophilic monomer and polyol chain extender 0.1~1
Part.
In above-mentioned base polyurethane prepolymer for use as, polyalcohol is the combination of any one or more of following substance: polyadipate fourth
Glycol esterdiol, polydiethylene glycol adipate glycol, polypropylene glycol adipate glycol, polyadipate ethylene glycol butanediol ester
Glycol, polytetrahydrofuran ether glycol, polypropylene oxide glycol.
Preferably, the number-average molecular weight of above-mentioned polyalcohol is 1000~2000.
In above-mentioned base polyurethane prepolymer for use as, diisocyanate is any one or more of following substance combination: isophorone
Diisocyanate, methyl diphenylene diisocyanate, toluene di-isocyanate(TDI), 4,4'- dicyclohexyl methyl hydride diisocyanate, 1,
Hexamethylene-diisocyanate.
In above-mentioned base polyurethane prepolymer for use as, hydrophilic monomer is the one or more combination of following substance: dimethylolpropionic acid, two
Hydroxymethyl propionic acid, ethylenediamine base ethanesulfonic acid sodium；
The polyol chain extender is any one or several combinations of following substance: trimethylolpropane, diethylene glycol (DEG), 1,4-
Butanediol, 1,6-HD, 1,3 butylene glycol.
In above-mentioned adhesive, neutralizer is the combination of any one or more of following substance: triethylamine, sodium hydroxide.
In above-mentioned adhesive, amine chain extender is the combination of one or more of following substance: ethylenediamine, divinyl three
Amine, triethylene tetramine.
Above-mentioned adhesive further include: 0.000001~0.0002 part of organic solvent.
The embodiment of the present invention provides a kind of preparation method of Aqueous Polyurethane Adhesives, is used to prepare above-mentioned aqueous poly- ammonia
Ester adhesive, comprising the following steps:
The each component of the Aqueous Polyurethane Adhesives is taken by above-mentioned formula；
(1) preparation of the base polyurethane prepolymer for use as containing hydrophilic monomer: by polyalcohol, diisocyanate, hydrophilic monomer 80
2h is reacted at a temperature of~90 DEG C, polyol chain extender is then added and reacts 2~4h, until the content of-NCO reaches theoretical value, is made
The performed polymer obtained is the base polyurethane prepolymer for use as containing hydrophilic monomer；
(2) neutralization reaction: being cooled to 25~45 DEG C for performed polymer made from the step (1), and neutralizer reaction 15 is added
~20min；
(3) under the shear action of high speed disperser, amine emulsion dispersion: is added into the reaction solution of the step (2)
The solution of chain extender and deionized water mixing, 20~30min of emulsion dispersion, aqueous polyurethane emulsion obtained is aqueous poly- ammonia
Ester adhesive.
In above-mentioned preparation method,
In the step (1), addition accounts for the acetone of performed polymer total weight 10%, the step (3) emulsion dispersion it
Afterwards, acetone is removed using vacuum decompression method；Alternatively, addition accounts for the third of performed polymer total weight 30% before the step (2)
Ketone removes acetone using vacuum decompression method after the step (3) emulsion dispersion.
The present invention is compared to be had the advantage that with the prior art
(1) preparation method of the invention does not contain organic tin or amines catalyst.
(2) preparation method of the invention avoids pre-polymerization production procedure because organic solvent is more, causes condensation process
Larger thermal loss.
(3) preparation method of the invention, emulsion dispersion process performed polymer viscosity is smaller, easy to operate efficient, reproducible.
The embodiment of the present invention is specifically described in further detail below.
Embodiment 1
The present embodiment provides a kind of Aqueous Polyurethane Adhesives, preparation method is following (each component is by weight):
22 parts of polyneopentyl glycol adipate glycol, polyadipate Isopropanediol esterdiol are added first in there-necked flask
260 parts, dehydration 2h is vacuumized at a temperature of 120 DEG C, is cooled to 80~85 DEG C, 15 parts of DMPA is added, 39 parts of acetone are added, stir
20min is mixed, 100 parts of IPDI is then added, temperature is kept for 80-85 DEG C, reacts 2h；Then 1.2 parts of 1,4-butanediol is added,
2h is reacted, is cooled to 40~45 DEG C, 120 parts of acetone, which are added, reduces performed polymer viscosity.
Neutralization reaction: carrying out 10~15min of neutralization reaction using 11 parts of triethylamines, and 8 parts of A95 are added in rear chain extension process,
5~10min is reacted, the solution of 142 parts of deionized waters and the mixing of 7 parts of ethylenediamine is added, is added at one time, stirring and emulsifying dispersion
20~30min.
De- ketone processing:, taking off 1~3h of ketone, content of acetone < 200ppm by 55 DEG C of set temperature, pressure 0.098Pa, admittedly contained
The aqueous polyurethane emulsion that amount is 45%, as Aqueous Polyurethane Adhesives.
The product is the lotion of pale blue, and solid content is 45 ± 1%, and partial size is in 60~90nm, and viscosity is in 60~900mpa
s。
Embodiment 2
The present embodiment provides a kind of Aqueous Polyurethane Adhesives, preparation method is following (each component is by weight):
282 parts of polybutylene glyool adipate are added in there-necked flask and vacuumizes dehydration 2h at a temperature of 120 DEG C, is cooled to
80~85 DEG C, 15 parts of DMPA is added, 39 parts of acetone are added, stirs 20min, 100 parts of MDI is then added, temperature keeps 80
~85 DEG C, react 2h；Then 1.2 parts of 1,4-butanediol is added, reacts 2h, is cooled to 40~45 DEG C, 120 parts of acetone drops are added
Low performed polymer viscosity.
Neutralization reaction: neutralization reaction 10-15min is carried out using 11 parts of triethylamines, 8 parts of A95 are added in rear chain extension process, instead
5-10min is answered, the solution of 142 parts of deionized waters and the mixing of 7 parts of ethylenediamine is added, is added at one time, stirring and emulsifying disperses 20-
30min。
De- ketone processing:, taking off 1~3h of ketone by 55 DEG C of set temperature, pressure 0.098Pa, obtain solid content be 45% it is aqueous poly-
Urethane lotion, as Aqueous Polyurethane Adhesives.
The product is nattier blue lotion, and solid content is 45 ± 1%, partial size in 60~90nm, viscosity 60~
900mpa·s。
The Aqueous Polyurethane Adhesives are good using tack, and formation emulsion intercalation method is good, and viscosity is lower.The hydrophilic list
Body is DMPA and A95 (ethylenediamine base ethanesulfonic acid sodium)；The stability, which refers to store 7 days at 50 DEG C, not to be precipitated, and 3000 turns
Centrifuge 15min is not precipitated；The viscosity is lower to refer to viscosity between 60~900mpas.It is prepared by the present invention aqueous
Polyurethane viscosity is lower, can be used for the surface covering of flexible parent metal, the fields such as adhesive.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (10)
1. a kind of Aqueous Polyurethane Adhesives, which is characterized in that the raw material comprising following parts by weight:
44~46 parts of base polyurethane prepolymer for use as, 53.5~55.5 parts of deionized water, 2~3 parts of neutralizer and amine chain extender 0.01~
0.5 part.
2. Aqueous Polyurethane Adhesives according to claim 1, which is characterized in that the base polyurethane prepolymer for use as is by following heavy
The raw material of amount number is prepared, comprising:
67~68 parts of polyalcohol, 23~24 parts of diisocyanate, 4~5 parts of hydrophilic monomer and 0.1~1 part of polyol chain extender.
3. Aqueous Polyurethane Adhesives according to claim 2, which is characterized in that the polyalcohol is in following substance
Any one or several combination: polybutylene glyool adipate, polydiethylene glycol adipate glycol, polyadipate propylene glycol
Esterdiol, polyadipate ethylene glycol butyl glycol ester diol, polytetrahydrofuran ether glycol, polypropylene oxide glycol.
4. Aqueous Polyurethane Adhesives according to claim 2 or 3, which is characterized in that the equal molecule of the number of the polyalcohol
Amount is 1000~2000.
5. Aqueous Polyurethane Adhesives according to claim 2 or 3, which is characterized in that the diisocyanate is following
Any one or more of substance combination: isophorone diisocyanate, methyl diphenylene diisocyanate, toluene diisocynate
Ester, 4,4'- dicyclohexyl methyl hydride diisocyanate, hexamethylene diisocyanate.
6. Aqueous Polyurethane Adhesives according to claim 2 or 3, which is characterized in that the hydrophilic monomer is following object
The one or more combination of matter: dimethylolpropionic acid, dihydromethyl propionic acid, ethylenediamine base ethanesulfonic acid sodium；
The polyol chain extender is any one or several combinations of following substance: trimethylolpropane, diethylene glycol (DEG), 1,4- fourth two
Alcohol, 1,6-HD, 1,3 butylene glycol.
7. Aqueous Polyurethane Adhesives according to claim 1, which is characterized in that the neutralizer is in following substance
Any one or several combination: triethylamine, sodium hydroxide；
The amine chain extender is the combination of one or more of following substance: ethylenediamine, diethylenetriamine, triethylene four
Amine.
8. Aqueous Polyurethane Adhesives according to claim 1, which is characterized in that further include: organic solvent 0.000001
~0.0002 part.
9. a kind of preparation method of Aqueous Polyurethane Adhesives, which is characterized in that be used to prepare any one of claim 1 to 8 institute
The Aqueous Polyurethane Adhesives stated, comprising the following steps:
It is according to claim 1 to be formulated each component for taking the Aqueous Polyurethane Adhesives；
(1) prepare the base polyurethane prepolymer for use as containing hydrophilic monomer: by base polyurethane prepolymer for use as formula by polyalcohol, diisocyanate,
Hydrophilic monomer reacts 2h at a temperature of 80~90 DEG C, and polyol chain extender is then added and reacts 2~4h, until the content of-NCO reaches
To theoretical value, performed polymer obtained is the base polyurethane prepolymer for use as containing hydrophilic monomer；
(2) neutralization reaction: being cooled to 25~45 DEG C for base polyurethane prepolymer for use as made from the step (1), and neutralizer reaction is added
15~20min；
(3) under the shear action of high speed disperser, amine chain extension emulsion dispersion: is added into the reaction solution of the step (2)
The solution of agent and deionized water mixing, 20~30min of emulsion dispersion, aqueous polyurethane emulsion obtained is water-borne polyurethane bond
Glutinous agent.
10. the preparation method of Aqueous Polyurethane Adhesives according to claim 9, which is characterized in that in the method,
In the step (1), the acetone that addition accounts for performed polymer total weight 10% is adopted after the step (3) emulsion dispersion
Acetone is removed with vacuum decompression method；Alternatively, the acetone for accounting for performed polymer total weight 30% is added before the step (2),
After step (3) emulsion dispersion, acetone is removed using vacuum decompression method.
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Cited By (4)
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| CN110551270A (en) * | 2019-09-17 | 2019-12-10 | 北京高盟新材料股份有限公司 | Aqueous polyurethane dispersion and preparation method and application thereof |
| CN111072906A (en) * | 2019-12-31 | 2020-04-28 | 北京华腾新材料股份有限公司 | Activation temperature controllable waterborne polyurethane emulsion and preparation method and application thereof |
| CN111072899A (en) * | 2019-12-13 | 2020-04-28 | 北京高盟新材料股份有限公司 | Waterborne polyurethane automotive interior coating adhesive and preparation method thereof |
| CN115785830A (en) * | 2022-12-15 | 2023-03-14 | 江阴通利光电科技有限公司 | Preparation method of substrate-free double-sided adhesive tape and double-sided adhesive tape |
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