CN109867743A - A kind of room-temperature self-crosslinking water-based acrylic dispersion and preparation method thereof - Google Patents
A kind of room-temperature self-crosslinking water-based acrylic dispersion and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of room-temperature self-crosslinking water-based acrylic dispersions and preparation method thereof, belong to synthesis of polymer material field.The room-temperature self-crosslinking water-based acrylic dispersion is composed of the following raw materials by weight: vinyl-based soft monomer 30-57 parts, hard monomer 15-35 parts vinyl-based, 15-43 parts of function monomer, 0.5-15 parts of cross-linking monomer, 0.5-9 parts of crosslinking agent, 0.5-4 parts of initiator, 4-15 parts of neutralizer, 70-200 parts of deionized water, 1-3 parts of pH buffer, 0.05-0.2 parts of chain-transferring agent.Room-temperature self-crosslinking water-based acrylic dispersion of the present invention is made using the method for semicontinuous-seed free radical polymerization.The present invention has the advantages that dried coating film speed is fast, water-tolerant, hardness are high, can crosslinked at low temperature film forming, safety and environmental protection meets industry development trend, has wide application field.
Description
Technical field
The present invention relates to synthesis of polymer material technical fields, and in particular to a kind of room-temperature self-crosslinking water-based acrylic resin
Dispersion and preparation method thereof.
Background technique
The environmental-friendly theme for having become 21 century development, with the enhancing and relevant law policy of people's environmental consciousness
The discharge of limitation volatile organic compounds (VOC) is put into effect, the solvent based coating of high VOC content is by unprecedented challenge.
Compared with traditional solvent based coating, water paint only contains minimal amount of VOC using water as primary solvent, is a kind of novel
Environmental protection coating material, have many advantages, such as it is nontoxic, using it is safe, convenient for storage and transportation.
Water-borne acrylic coatings are because it is short with drying time, flexibility is good, color is shallow, guarantor's light at low cost and excellent is protected
Color and outdoor weathe resistance etc. are widely used in the fields such as machine-building, communications and transportation, light industry, chemical industry, building.However, at present
Most of water-based acrylic resin belongs to thermoplastic on domestic market, intermolecular to only exist hydrogen bond, Van der Waals force, cannot be formed
The disadvantages of stable chemical bond, generally existing poor water resistance, low temperature becomes fragile, high temperature after tack, it is seriously limited in new and high technology
The application in field.
Summary of the invention
The invention proposes a kind of room-temperature self-crosslinking water-based acrylic dispersions and preparation method thereof, overcome above-mentioned
The shortcomings that prior art and deficiency introduce ketone hydrazine ambient cross-linking system using the method for copolymerization to third in water-based acrylic resin
Olefin(e) acid resin is modified, and this method not only pollutes small, and processed preparation process is simple, at low cost, and in the curing process
Tridimensional network is formed, so that the mechanical performance of film, water resistance, solvent resistance, low temperature is become fragile, the comprehensive performances such as high temperature after tack
Improved simultaneously.
It realizes the technical scheme is that a kind of room-temperature self-crosslinking water-based acrylic dispersion, including following heavy
Measure the raw material of part: vinyl-based soft monomer 31-57 parts, hard monomer 16-35 parts vinyl-based, 15-43 parts of function monomer, crosslinking list
0.5-15 parts of body, 0.5-9 parts of crosslinking agent, 0.5-4 parts of initiator, 4-15 parts of neutralizer, 40-80 parts of solvent, deionized water 70-
200 parts, 1-3 parts of pH buffer, 0.02-0.2 parts of chain-transferring agent.
The vinyl-based soft monomer is selected from butyl methacrylate, butyl acrylate, acrylic acid-2-ethyl caproite, third
The secondary butyl ester of olefin(e) acid, n-octyl, lauryl acrylate, Isooctyl acrylate monomer, vinylacetate, methacrylic acid are different pungent
One of ester, n octyl methacrylate or any several combinations；The vinyl-based hard monomer is selected from methyl methacrylate
One of ester, methyl acrylate, ethyl methacrylate, ethyl acrylate, styrene, divinylbenzene, acrylonitrile are appointed
It anticipates several combinations.
The function monomer be acid and carboxylic monomer mixing, it is described acid selected from acrylic acid, methacrylic acid, butenoic acid,
At least one of maleic anhydride and clothing saccharic acid, the carboxylic monomer be selected from hydroxy-ethyl acrylate, hydroxyethyl methacrylate,
At least one of hydroxypropyl acrylate and hydroxy propyl methacrylate.
The cross-linking monomer is Diacetone Acrylamide, and the crosslinking agent is adipic dihydrazide, succinic acid hydrazide ii, carbon
At least one of acid dihydrazide.
The initiator is benzoyl peroxide, azo-bis-isobutyl cyanide, a tert-butyl hydroperoxide, di-tert-butyl peroxide
At least one of object, two t-amyl peroxy compounds；The solvent is one of n-butanol, isopropanol, isobutanol, n-butyl ether
Or any several combinations.
The neutralizer is ammonium hydroxide, triethylamine, 2-amino-2-methyl-1-propanol, N, N- dimethylethanolamine, hydroxide
At least one of tetramethyl-ammonium；The pH buffer is the combination of one or both of sodium bicarbonate, ammonium hydrogencarbonate；Chain tra nsfer
Agent is n-dodecyl mercaptan.
The preparation method of the room-temperature self-crosslinking water-based acrylic dispersion, steps are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) residual solvent, monomer mixed solution are added in the reaction kettle equipped with condenser pipe, stirring rod and thermometer, 80
DEG C -88 DEG C of constant temperature are added in 1/3 step (1) dissolved initiator for reaction 25-40 minutes；Add dissolution in 1/3 step (1)
Initiator afterwards is then at the uniform velocity added remaining mix monomer, constant temperature 1 hour, dissolved initiation in remaining step (1) is added
Agent, and it is warming up to 90-95 DEG C of constant temperature 2-3 hours, obtain water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, neutralizer is added, adjusts pH between 7.0-9.0, addition deionized water high speed dispersion is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
The mass fraction of monomer mixed solution is 10%-25% in the step (1).
The adding manner of remaining mix monomer is to be added dropwise in the step (2), and controlling total time for adding is 2-3h.
The solid content of room-temperature self-crosslinking water-based acrylic dispersion is 30-50% in the step (3).
The beneficial effects of the present invention are: the present invention by introduced when prepared by resin can the ketone hydrazine of room temperature crosslinking curing be crosslinked
System achievees the purpose that crosslinking curing by the pH of control system in resin film forming.Ketone hydrazine cross-linking system, in alkaline condition
Under do not react, in solutions of weak acidity, can reacting at room temperature, it is cross-linking modified to achieve the purpose that, the method for modifying is not only energy saving
Environmentally friendly, low in cost and production preparation is easy, and water resistance, the salt fog resistance that can improve water soluble acrylic acid film simultaneously are poor, low
The defects such as temperature becomes fragile, high temperature after tack and hardness of film are low, can also greatly improve the mechanical performance of film, have wide application
Prospect.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of room-temperature self-crosslinking water-based acrylic dispersion, including following component according to parts by weight:
Vinyl soft monomer: butyl acrylate, 31 parts；
Vinyl hard monomer: methyl methacrylate, styrene account for 10,6 parts respectively；
Function monomer: acrylic acid, hydroxypropyl acrylate, 11,4 parts；
Cross-linking monomer: Diacetone Acrylamide, 2 parts；
Crosslinking agent: succinic acid hydrazide ii, 1.5 parts；
Initiator: azo-bis-isobutyl cyanide, 0.5 part；
Buffer: sodium bicarbonate, 1 part；
Solvent: n-butanol, 44 parts；
Dispersing agent: deionized water, 112 parts；
Chain-transferring agent: n-dodecyl mercaptan, 0.02 part；
Neutralizer: triethylamine, in right amount.
The room-temperature self-crosslinking water-based acrylic dispersion preparation process are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) monomer mixed solution of residual solvent, mass fraction 15% is added to equipped with condenser pipe, stirring rod and thermometer
In reaction kettle, in 85 DEG C of constant temperature, it is added 1/3 initiator for reaction 30 minutes；1/3 initiator is added, is then at the uniform velocity added remaining mixed
Monomer is closed, constant temperature 1 hour, remaining initiator is added, and be warming up to 93 DEG C of constant temperature 2 hours, obtains water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, appropriate neutralizer is added, adjusts pH to 8.0, deionized water progress high speed dispersion is added and is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
Embodiment 2
A kind of room-temperature self-crosslinking water-based acrylic dispersion, including following component according to parts by weight:
Vinyl soft monomer: butyl acrylate, acrylic acid-2-ethyl caproite account for 26,11 parts respectively；
Vinyl hard monomer: methyl methacrylate, styrene account for 10.6,13.9 parts respectively；
Function monomer: acrylic acid, hydroxypropyl acrylate account for 12,11 parts respectively；
Cross-linking monomer: Diacetone Acrylamide, 6 parts；
Crosslinking agent: adipic dihydrazide, succinic acid hydrazide ii account for 2.5,1 parts respectively；
Initiator: azo-bis-isobutyl cyanide, a tert-butyl hydroperoxide, 0.3,0.75 part；
Buffer: sodium bicarbonate, 2.5 parts；
Solvent: n-butanol, n-butyl ether account for 52,6 parts respectively；
Dispersing agent: deionized water, 125 parts；
Chain-transferring agent: n-dodecyl mercaptan, 0.02 part；
Neutralizer: triethylamine, in right amount.
The room-temperature self-crosslinking water-based acrylic dispersion preparation process are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) monomer mixed solution of residual solvent, mass fraction 15% is added to equipped with condenser pipe, stirring rod and thermometer
In reaction kettle, in 85 DEG C of constant temperature, it is added 1/3 initiator for reaction 30 minutes；1/3 initiator is added, is then at the uniform velocity added remaining mixed
Monomer is closed, constant temperature 1 hour, remaining initiator is added, and be warming up to 93 DEG C of constant temperature 2 hours, obtains water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, appropriate neutralizer is added, adjusts pH to 7.5, deionized water progress high speed dispersion is added and is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
Embodiment 3
A kind of room-temperature self-crosslinking water-based acrylic dispersion, including following component according to parts by weight:
Vinyl soft monomer: butyl acrylate, acrylic acid-2-ethyl caproite, isooctyl methacrylate, account for 31.5 respectively,
9.5,16 parts；
Vinyl hard monomer: methyl methacrylate, styrene, acrylonitrile account for 11.5,16.5,7 parts respectively；
Function monomer: acrylic acid, hydroxypropyl acrylate account for 12,31 parts respectively；
Cross-linking monomer: Diacetone Acrylamide, 15 parts；
Crosslinking agent: adipic dihydrazide, succinic acid hydrazide ii account for 6,3 parts respectively；
Initiator: azo-bis-isobutyl cyanide, a tert-butyl hydroperoxide, 1.5,2.5 parts；
Buffer: sodium bicarbonate, 3 parts；
Solvent: n-butanol, n-butyl ether account for 65,6 parts respectively；
Dispersing agent: deionized water, 180 parts；
Chain-transferring agent: n-dodecyl mercaptan, 0.15 part；
Neutralizer: triethylamine, N, N- dimethylethanolamine, in right amount.
The room-temperature self-crosslinking water-based acrylic dispersion preparation process are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) monomer mixed solution of residual solvent, mass fraction 20% is added to equipped with condenser pipe, stirring rod and thermometer
In reaction kettle, in 85 DEG C of constant temperature, it is added 1/3 initiator for reaction 40 minutes；1/3 initiator is added, is then at the uniform velocity added remaining mixed
Monomer is closed, constant temperature 1 hour, remaining initiator is added, and be warming up to 95 DEG C of constant temperature 2 hours, obtains water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, appropriate neutralizer is added, adjusts pH to 8.0, deionized water progress high speed dispersion is added and is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
Embodiment 4
A kind of room-temperature self-crosslinking water-based acrylic dispersion, including following component according to parts by weight:
Vinyl soft monomer: butyl acrylate, isooctyl methacrylate account for 28,14 parts respectively；
Vinyl hard monomer: methyl methacrylate, styrene, acrylonitrile account for 9,12,5 parts respectively；
Function monomer: methacrylic acid, butenoic acid, maleic anhydride, hydroxypropyl acrylate, hydroxyethyl methacrylate, point
8,4,5,15,6 parts are not accounted for；
Cross-linking monomer: Diacetone Acrylamide, 7 parts；
Crosslinking agent: carbon acid dihydrazide, succinic acid hydrazide ii account for 2,3 parts respectively；
Initiator: benzoyl peroxide, a tert-butyl hydroperoxide, 0.6,0.4 part；
Buffer: sodium bicarbonate, 1.5 parts；
Solvent: isopropanol, n-butyl ether account for 48,6 parts respectively；
Dispersing agent: deionized water, 140 parts；
Chain-transferring agent: n-dodecyl mercaptan, 0.1 part；
Neutralizer: triethylamine, N, N- dimethylethanolamine, in right amount.
The room-temperature self-crosslinking water-based acrylic dispersion preparation process are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) monomer mixed solution of residual solvent, mass fraction 10% is added to equipped with condenser pipe, stirring rod and thermometer
In reaction kettle, in 85 DEG C of constant temperature, it is added 1/3 initiator for reaction 25 minutes；1/3 initiator is added, is then at the uniform velocity added remaining mixed
Monomer is closed, constant temperature 1 hour, remaining initiator is added, and be warming up to 90 DEG C of constant temperature 2 hours, obtains water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, appropriate neutralizer is added, adjusts pH to 7.5, deionized water progress high speed dispersion is added and is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
Embodiment 5
A kind of room-temperature self-crosslinking water-based acrylic dispersion, including following component according to parts by weight:
Vinyl soft monomer: butyl acrylate, butyl methacrylate account for 21,9 parts respectively；
Vinyl hard monomer: methyl methacrylate, styrene account for 17,13 parts respectively；
Function monomer: methacrylic acid, maleic anhydride, hydroxyethyl methacrylate account for 14,2,21 parts respectively；
Cross-linking monomer: Diacetone Acrylamide, 5 parts；
Crosslinking agent: adipic dihydrazide, succinic acid hydrazide ii account for 3,1 parts respectively；
Initiator: benzoyl peroxide, di-tert-butyl peroxide, 0.3,0.5 part；
Buffer: sodium bicarbonate, 1 part；
Solvent: isopropanol, n-butyl ether account for 60,11 parts respectively；
Dispersing agent: deionized water, 146 parts；
Chain-transferring agent: n-dodecyl mercaptan, 0.05 part；
Neutralizer: triethylamine, tetramethyl ammonium hydroxide, in right amount.
The room-temperature self-crosslinking water-based acrylic dispersion preparation process are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) monomer mixed solution of residual solvent, mass fraction 15% is added to equipped with condenser pipe, stirring rod and thermometer
In reaction kettle, in 88 DEG C of constant temperature, it is added 1/3 initiator for reaction 30 minutes；1/3 initiator is added, is then at the uniform velocity added remaining mixed
Monomer is closed, constant temperature 1 hour, remaining initiator is added, and be warming up to 90 DEG C of constant temperature 2 hours, obtains water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, appropriate neutralizer is added, adjusts pH to 9, deionized water is added and carries out high speed dispersion formation water
Property acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
Embodiment 6
A kind of room-temperature self-crosslinking water-based acrylic dispersion, including following component according to parts by weight:
Vinyl soft monomer: butyl acrylate, 31 parts；
Vinyl hard monomer: methyl methacrylate, 35 parts；
Function monomer: acrylic acid, hydroxypropyl acrylate, 12,21 parts；
Cross-linking monomer: Diacetone Acrylamide, 0.5 part；
Crosslinking agent: succinic acid hydrazide ii, 0.5 part；
Initiator: azo-bis-isobutyl cyanide, 0.5 part；
Buffer: sodium bicarbonate, 1 part；
Solvent: isopropanol, 65 parts；
Dispersing agent: deionized water, 100 parts；
Chain-transferring agent: n-dodecyl mercaptan, 0.02 part；
Neutralizer: triethylamine, in right amount.
The room-temperature self-crosslinking water-based acrylic dispersion preparation process are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) monomer mixed solution of residual solvent, mass fraction 17% is added to equipped with condenser pipe, stirring rod and thermometer
In reaction kettle, in 88 DEG C of constant temperature, it is added 1/3 initiator for reaction 30 minutes；1/3 initiator is added, is then at the uniform velocity added remaining mixed
Monomer is closed, constant temperature 1 hour, remaining initiator is added, and be warming up to 95 DEG C of constant temperature 2 hours, obtains water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, appropriate neutralizer is added, adjusts pH to 8.0, deionized water progress high speed dispersion is added and is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
Embodiment 7
A kind of room-temperature self-crosslinking water-based acrylic dispersion, including following component according to parts by weight:
Vinyl soft monomer: butyl acrylate, acrylic acid-2-ethyl caproite account for 41,16 parts respectively；
Vinyl hard monomer: methyl methacrylate, acrylonitrile account for 30,5 parts respectively；
Function monomer: acrylic acid, hydroxypropyl acrylate, 14.5,28.5 parts；
Cross-linking monomer: Diacetone Acrylamide, 15 parts；
Crosslinking agent: succinic acid hydrazide ii, 9 parts；
Initiator: azo-bis-isobutyl cyanide, 4 parts；
Buffer: sodium bicarbonate, 3 parts；
Solvent: isopropanol, n-butyl ether, 65,24 parts；
Dispersing agent: deionized water, 160 parts；
Chain-transferring agent: n-dodecyl mercaptan, 0.2 part；
Neutralizer: triethylamine, N, N- dimethylethanolamine, in right amount.
The room-temperature self-crosslinking water-based acrylic dispersion preparation process are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) monomer mixed solution of residual solvent, mass fraction 25% is added to equipped with condenser pipe, stirring rod and thermometer
In reaction kettle, in 85 DEG C of constant temperature, it is added 1/3 initiator for reaction 40 minutes；1/3 initiator is added, is then at the uniform velocity added remaining mixed
Monomer is closed, constant temperature 1 hour, remaining initiator is added, and be warming up to 95 DEG C of constant temperature 2 hours, obtains water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, appropriate neutralizer is added, adjusts pH to 7.5, deionized water progress high speed dispersion is added and is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
To further illustrate room-temperature self-crosslinking water-based acrylic dispersion disclosed in this invention, the present invention is also to reality
The room-temperature self-crosslinking water-based acrylic acid dispersion and film performance for applying example 1~7 have carried out corresponding test, and test method is as follows:
(1) storage and transportation stability test: acrylic dispersion sample being installed and is put into 50 DEG C of baking ovens, and constant temperature is placed 2 weeks, is taken
Be placed under room temperature environment and observe out, such as without gel or be divided into phenomenon occur, then pass through test.
(2) film water absorption rate test: the test of gained acrylic dispersion film water absorption rate uses GB/T1733-93
Method.Certain mass (W is weighed first0) film be soaked in water, take out at regular intervals, quickly erase table with filter paper
Weigh (W immediately after the water of face1), follow-on test for a period of time, until sample tends to swelling equilibrium, water absorption rate (P) calculation formula are as follows:
(3) hardness of film is tested: gained acrylic dispersion hardness of film is measured according to the method for GB/T6739-1996.
(4) adhesive force measures: according to the attachment of the method measurement dispersions obtained film of embodiment of GB/T9286-1998
Power.
(5) surface drying time is tested: room-temperature self-crosslinking water-based acrylic dispersion prepared by embodiment is uniformly applied
It is put on polyfluortetraethylene plate, 25 DEG C of freeze-day with constant temperature, the surface drying time of film is measured according to the method for GB1728-79.
(6) the film degree of cross linking is tested: will be placed on drying 7 days in 25 DEG C of isoperibol after emulsion film, is weighed certain matter
Measure M0Film be put into the Soxhlet extractor equipped with ethyl acetate and extract 24 hours, then take out and 25 DEG C freeze-day with constant temperature 2 days,
Claim its mass M1, film degree of cross linking F is calculated according to the following formula:
(1) mechanics performance determining: according to the method for GB13022-91, film is measured using UTM4204 type universal material puller system
Mechanical property, test result is as follows shown in table:
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of room-temperature self-crosslinking water-based acrylic dispersion, it is characterised in that the raw material including following parts by weight: ethylene
31-57 parts of base class soft monomer, hard monomer 16-35 parts vinyl-based, 15-43 parts of function monomer, 0.5-15 parts of cross-linking monomer, crosslinking
0.5-9 parts of agent, 0.5-4 parts of initiator, 4-15 parts of neutralizer, 40-80 parts of solvent, 70-200 parts of deionized water, pH buffer 1-3
Part, 0.02-0.2 parts of chain-transferring agent.
2. room-temperature self-crosslinking water-based acrylic dispersion according to claim 1, it is characterised in that: the vinyl
Class soft monomer is being selected from butyl methacrylate, butyl acrylate, acrylic acid-2-ethyl caproite, sec-butyl acrylate, acrylic acid just
Monooctyl ester, lauryl acrylate, Isooctyl acrylate monomer, vinylacetate, isooctyl methacrylate, in n octyl methacrylate
One or any of several combination；The vinyl-based hard monomer is selected from methyl methacrylate, methyl acrylate, metering system
One of acetoacetic ester, ethyl acrylate, styrene, divinylbenzene, acrylonitrile or any several combinations.
3. room-temperature self-crosslinking water-based acrylic dispersion according to claim 1, it is characterised in that: the function list
Body is the mixing of acid and carboxylic monomer, and the acid is selected from acrylic acid, methacrylic acid, butenoic acid, maleic anhydride and clothing sugar
At least one of acid, the carboxylic monomer are selected from hydroxy-ethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate and first
At least one of base hydroxypropyl acrylate.
4. room-temperature self-crosslinking water-based acrylic dispersion according to claim 1, it is characterised in that: the crosslinking is single
Body is Diacetone Acrylamide, and the crosslinking agent is adipic dihydrazide, succinic acid hydrazide ii, at least one in carbon acid dihydrazide
Kind.
5. room-temperature self-crosslinking water-based acrylic dispersion according to claim 1, it is characterised in that: the initiator
For benzoyl peroxide, azo-bis-isobutyl cyanide, a tert-butyl hydroperoxide, di-tert-butyl peroxide, two t-amyl peroxies
At least one of object；The solvent is one of n-butanol, isopropanol, isobutanol, n-butyl ether or any several combinations.
6. room-temperature self-crosslinking water-based acrylic dispersion according to claim 1, it is characterised in that: the neutralizer
For ammonium hydroxide, triethylamine, 2-amino-2-methyl-1-propanol, N, at least one in N- dimethylethanolamine, tetramethyl ammonium hydroxide
Kind；The pH buffer is the combination of one or both of sodium bicarbonate, ammonium hydrogencarbonate；Chain-transferring agent is dodecyl sulphur
Alcohol.
7. the preparation method of room-temperature self-crosslinking water-based acrylic dispersion described in any one of claims 1-6, feature
It is that steps are as follows:
(1) by formula weigh vinyl-based soft monomer, vinyl-based hard monomer, function monomer, cross-linking monomer, chain-transferring agent and
PH buffer simultaneously carries out being mixed to form monomer mixed solution；It weighs the initiator of formula ratio and is dissolved in spare in suitable solvent；
(2) residual solvent, monomer mixed solution are added in the reaction kettle equipped with condenser pipe, stirring rod and thermometer, 80
Dissolved initiator for reaction 25-40min in 1/3 step (1) is added in DEG C -88 DEG C of constant temperature；It adds in 1/3 step (1) after dissolution
Initiator, remaining mix monomer is then at the uniform velocity added, constant temperature 1 hour, dissolved initiator in remaining step (1) is added,
And it is warming up to 90-95 DEG C of constant temperature 2-3 hours, obtain water-based acrylic resin；
(3) 50 DEG C are adjusted the temperature to, neutralizer is added, adjusts pH between 7.0-9.0, addition deionized water high speed dispersion is formed
Water soluble acrylic acid dispersion, is eventually adding crosslinking agent and filtering and discharging obtains room-temperature self-crosslinking water-based acrylic dispersion.
8. the preparation method of room-temperature self-crosslinking water-based acrylic dispersion according to claim 7, it is characterised in that:
The mass fraction of monomer mixed solution is 10%-25% in the step (1).
9. the preparation method of room-temperature self-crosslinking water-based acrylic dispersion according to claim 7, it is characterised in that:
The adding manner of remaining mix monomer is to be added dropwise in the step (2), and controlling total time for adding is 2-3h.
10. the preparation method of room-temperature self-crosslinking water-based acrylic dispersion according to claim 7, feature exist
In: the solid content of room-temperature self-crosslinking water-based acrylic dispersion is 30-50% in the step (3).
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| CN110373135A (en) * | 2019-08-15 | 2019-10-25 | 平湖铂淳胶粘技术有限公司 | A kind of acrylic acid series hot melt adhesive and preparation method thereof |
| CN111349200A (en) * | 2020-04-20 | 2020-06-30 | 广东花果山环保科技有限公司 | Aqueous high-hardness low-film-forming-temperature single-component acrylic resin and preparation method thereof |
| CN111808245A (en) * | 2020-07-24 | 2020-10-23 | 郑州中科新兴产业技术研究院 | Epoxidized soybean oil modified aqueous acrylic resin dispersion and preparation method thereof |
| CN111848878A (en) * | 2020-07-27 | 2020-10-30 | 中国科学院化学研究所 | Aqueous acrylic acid dispersion and preparation method and application thereof |
| CN112608406A (en) * | 2020-11-27 | 2021-04-06 | 浙江可思克高新材料股份有限公司 | Heavy calcium carbonate grinding dispersant and preparation method thereof |
| CN113105571A (en) * | 2021-03-29 | 2021-07-13 | 华南理工大学 | Low-temperature self-crosslinking waterborne epoxy modified acrylic resin and preparation method and application thereof |
| CN115010846A (en) * | 2022-06-23 | 2022-09-06 | 安徽尚德轨道设备制造有限公司 | Synthesis of special resin for cold spray zinc and preparation method of cold spray zinc |
| CN116162387A (en) * | 2022-12-09 | 2023-05-26 | 安徽拓力工程材料科技有限公司 | Durable reflective coating and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110373135A (en) * | 2019-08-15 | 2019-10-25 | 平湖铂淳胶粘技术有限公司 | A kind of acrylic acid series hot melt adhesive and preparation method thereof |
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| CN111349200A (en) * | 2020-04-20 | 2020-06-30 | 广东花果山环保科技有限公司 | Aqueous high-hardness low-film-forming-temperature single-component acrylic resin and preparation method thereof |
| CN111808245A (en) * | 2020-07-24 | 2020-10-23 | 郑州中科新兴产业技术研究院 | Epoxidized soybean oil modified aqueous acrylic resin dispersion and preparation method thereof |
| CN111808245B (en) * | 2020-07-24 | 2023-03-21 | 郑州中科新兴产业技术研究院 | Epoxidized soybean oil modified aqueous acrylic resin dispersion and preparation method thereof |
| CN111848878A (en) * | 2020-07-27 | 2020-10-30 | 中国科学院化学研究所 | Aqueous acrylic acid dispersion and preparation method and application thereof |
| CN112608406A (en) * | 2020-11-27 | 2021-04-06 | 浙江可思克高新材料股份有限公司 | Heavy calcium carbonate grinding dispersant and preparation method thereof |
| CN113105571A (en) * | 2021-03-29 | 2021-07-13 | 华南理工大学 | Low-temperature self-crosslinking waterborne epoxy modified acrylic resin and preparation method and application thereof |
| CN115010846A (en) * | 2022-06-23 | 2022-09-06 | 安徽尚德轨道设备制造有限公司 | Synthesis of special resin for cold spray zinc and preparation method of cold spray zinc |
| CN116162387A (en) * | 2022-12-09 | 2023-05-26 | 安徽拓力工程材料科技有限公司 | Durable reflective coating and preparation method and application thereof |
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