CN106244058A - A kind of speed is viscous from dry emulsion type adhesive and preparation method and application - Google Patents
A kind of speed is viscous from dry emulsion type adhesive and preparation method and application Download PDFInfo
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- CN106244058A CN106244058A CN201610614278.7A CN201610614278A CN106244058A CN 106244058 A CN106244058 A CN 106244058A CN 201610614278 A CN201610614278 A CN 201610614278A CN 106244058 A CN106244058 A CN 106244058A
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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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J111/00—Adhesives based on homopolymers or copolymers of chloroprene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention belongs to the technical field of adhesive, disclose a kind of speed viscous from dry emulsion type adhesive and preparation method and application.Described adhesive includes following component: acrylic acid ester emulsion, watersoluble neoprene emulsion；Deionized water, hydrophilic gas phase nano silicon dioxide, pH adjusting agent, aqueous wetting dispersing agent, zinc oxide fluid dispersion, defoamer, sterilization antiseptic, antioxidant；Described acrylic acid ester emulsion and watersoluble neoprene emulsion are matrix resin emulsion；Described pH adjusting agent is pH adjusting agent and the pH adjusting agent of watersoluble neoprene emulsion of acrylic acid ester emulsion.The speed of the present invention is viscous good, the most viscous fast from dry emulsion type adhesive good stability, instantaneous bond effect, and the open hour are long, and heat resistance water resistance is excellent.Described adhesive is for the bonding and household articles bonding of material.
Description
Technical field
The invention belongs to the technical field of adhesive, relate to a kind of emulsion-type adhesive, be specifically related to a kind of speed viscous from dry
Emulsion-type adhesive and preparation method and application.
Background technology
The soft furnitures such as the sofa that uses in the market, mattress, medicated pillow mainly have with low viscosity aqueous adhesive: aqueous
Neoprene adhesive and Aqueous Polyurethane Adhesives etc.；Wherein aqueous polyurethane soft furniture adhesive needs heat-activated ability
Using, this does not meets with the sector adhesive cold bonding condition, separately have double-component system polyurethane adhesive in-convenience in use, to setting
Have particular/special requirement etc. to limit it and be widely used.Watersoluble neoprene system adhesive has environmental protection, nontoxic, tasteless, and adhesive property is good
It is widely used etc. advantage；But current adhesive there is also some shortcoming and defect.
One-component watersoluble neoprene gluing agent: due to polychloroprene latex, viscous slow at the beginning of this type adhesive, drying time
Slowly, thermo-labile, poor water resistance；This type water-based neoprene stick is applicable to low side occasion, inapplicable in most of techniques.Third
The compound adhesive of olefin(e) acid neoprene: after adding acrylic emulsion, although for the most viscous, heat-resisting have part to improve, but due to
The ionic system difference of both systems, product stability is poor, easy breakdown of emulsion.Double-component aqueous neoprene adhesive: use aqueous
Neoprene adds demulsifier and mixes in use, at contact surface breakdown of emulsion thus form the mode of cohesive force, advantage is maximum
Improve initial bonding strength, can accomplish that moment is combined, shortcoming is the problem of thermostability and the resistance to water not changing neoprene system, with
Time for product use bring inconvenience.Modified model acrylic acid neoprene composite adhesive: add stabilizer in system, adjusts
Acrylic acid vitrification point, thus while being greatly improved initial bonding strength, improve the stability of product, and heat-resisting resistance to
Aqueous can also obtain a certain degree of raising.
Acrylic emulsion adhesive has abundant raw material source, and synthesis technique is flexible, and performance is various, wide adaptability,
The advantage such as with low cost, safe and convenient to use, is adhesive field development speed Environment-friendlyadhesive adhesive faster.Patent application
(CN101333424) disclose utilize acrylic acid ester emulsion, tackifier resin emulsion, watersoluble neoprene emulsion prepare for sofa, screen
The furniture spray paint such as wind, swivel chair is bonding and the Aqueous Adhesives that is used in that automotive trim is bonding, foam is bonding etc., although this application profit
Improve initial cohesiveness with acrylic acid ester emulsion and tackifier resin emulsion, but the poor stability of this adhesive and speed glue effect
Difference.Patent (CN101560367) disclose a kind of prepare watersoluble neoprene environmental protection glue spraying technical recipe, described adhesive use
The resin emulsions such as modified rosin emulsion, water-borne acrylic resin emulsion, ethylene-vinyl acetate copolymer emulsion are equipped with other and help
Agent and filler prepare, although this adhesive has preferable initial bonding strength, adhesion strength is excellent, holding power is excellent, heat-resisting ageing-resisting is excellent
Feature, but its stability needs to be investigated.Patent application (CN102191686A) have employed blending and modifying principle, and preparation is for skin
The environment-protective adhesive that the materials such as leather, sponge, non-woven fabrics, timber are bonding；But poor stability, the most viscous slow, thermostability occur sometimes
The problems such as resistance to water is more weak；Such adhesive cannot meet the requirement on speed viscosity energy and adhesive effect on adhesive property,
Range of application has certain limitation.
Summary of the invention
Bad for prior art aqueous adhesive stability, to application material the viscous poor effect of some speed, is dried speed
The problems such as degree is slow, initial bonding strength difference, or easily occur that owing to formula is unreasonable adhesive property reduces, blocks spray gun, preparation technology
Condition illustrates the problems such as not clear；The primary and foremost purpose of the present invention is to provide a kind of speed viscous from dry emulsion type adhesive.Described speed is glued
From dry emulsion type adhesive good stability, just glue, speed is viscous fast, natural drying, open hour length, heat resistance water resistance are excellent
Different.
Another object of the present invention is to provide above-mentioned speed the viscous preparation method from dry emulsion type adhesive.The present invention utilizes
Modification of acrylate emulsions watersoluble neoprene emulsion, uses suitable preparation technology, adds modifying agent, stabilizer, and regulator etc. helps
Agent preparation just glues, speed viscous fast, natural drying, good stability, easy to use, excellent the sticking from dry speed slimy milk sol of adhesive property
Agent.
It is still another object of the present invention to provide the viscous application from dry emulsion type adhesive of above-mentioned speed.
The purpose of the present invention is achieved through the following technical solutions:
A kind of speed is viscous from dry emulsion type adhesive, including following component: acrylic acid ester emulsion, watersoluble neoprene emulsion；Go from
Sub-water, hydrophilic gas phase nano silicon dioxide, pH adjusting agent, aqueous wetting dispersing agent, zinc oxide fluid dispersion, defoamer, sterilization are prevented
Rotten agent, antioxidant；Described acrylic acid ester emulsion and watersoluble neoprene emulsion are matrix resin emulsion.Described pH adjusting agent is propylene
The pH adjusting agent of acid esters emulsion and the pH adjusting agent of watersoluble neoprene emulsion.
In described matrix resin emulsion, acrylic acid ester emulsion is (0.5～2) with the mass ratio of watersoluble neoprene emulsion: 1；
The quality of described deionized water is the 5～8% of described matrix resin quality of the emulsion；
Quality is described matrix resin quality of the emulsion the 0.5～1.5% of described hydrophilic gas phase nano silicon dioxide；
The quality of described pH adjusting agent is that the pH value of described matrix resin emulsion is adjusted to pH is the matter needed for 9～12
Amount；
The quality of described aqueous wetting dispersing agent is the 0.1～0.3% of described matrix resin quality of the emulsion；
The quality of described zinc oxide fluid dispersion is the 0.5～1.5% of described matrix resin quality of the emulsion
The quality of described defoamer is the 0.1～0.2% of described matrix resin quality of the emulsion；
The quality of described sterilization antiseptic is the 0.1～0.2% of described matrix resin quality of the emulsion；
The quality of described antioxidant is the 0.1～0.2% of described matrix resin quality of the emulsion.
The vitrification point of described acrylic acid ester emulsion below-50 DEG C, described acrylic acid ester emulsion viscosity be 100～
200mPa.s；The particle diameter of described acrylic acid ester emulsion is below 250 nanometers, below preferably 200 nanometers；More preferably 150 receive
Below meter.
The preparation method of described acrylic acid ester emulsion, specifically comprises the following steps that
(1) take in the monomer component of acrylic ester synthesizing emulsion: acrylate soft monomer 40～70 parts, hard monomer 0～8
Part, function monomer 1～3 parts, emulsifying agent 0.8～2 parts, initiator 0.3～0.65 part, buffer agent 0.1～0.15 part, deionized water
35～65 parts；
(2) deionized water 20～40 weight portion, emulsifying agent 0.8～2 weight portion, initiator 0.1～0.45 weight portion are added
Enter in reactor, dispersed with stirring 5～10 minutes under 400～600r/min speed conditions；Again at 600～1000r/min rotating speeds
Lower addition acrylate soft monomer 40～70 weight portion, hard monomer 0～8 weight portion, function monomer 1～3 weight portion, pre-emulsification 10
～20 minutes, obtain pre-emulsion；
(3) under agitation, in reactor add 15～25 parts by weight of deionized water, 0.1～0.2 weight portion cause
Agent and 0.1～0.15 weight portion buffer agent are uniformly mixed so as to obtain bottom solution, in the reactor equipped with bottom solution add 10～
The pre-emulsion of 20 mass parts, is warming up to 80～82 DEG C of reactions 30～60min, drips the pre-breast of residual mass part in reactor
Liquid, continuously dropping 2.5～3h, heat up after dropping 84～86 DEG C of insulation reaction 2～2.5h, and cooling is filtered, discharging, obtained
Described acrylic acid ester emulsion.
Described acrylate soft monomer is at least one in lauryl methacrylate and butyl acrylate and acrylic acid
The mixture of different monooctyl ester, wherein Isooctyl acrylate monomer accounts for the 70～90% of acrylate soft monomer gross mass.Described hard monomer is
Acrylic acid methyl ester. or methyl methacrylate；Described function monomer be in acrylamide, acrylic acid and methacrylic acid at least
A kind of mixture with 2-(Acryloyloxy)ethanol；Described emulsifying agent be anionic emulsifier and nonionic emulsifier mixing answer
Co-emulsifier, in described compound emulsifying agent, anionic emulsifier is (10～15) with the mass ratio of nonionic emulsifier: (5
～10), described anionic emulsifier is sodium lauryl sulphate, and described nonionic emulsifier is OP-10；Described initiator
For persulfate, preferably persulfuric acid ammonium salt；Described buffer agent is sodium bicarbonate or sodium carbonate；It is preferably sodium bicarbonate.
Described watersoluble neoprene emulsion (i.e. watersoluble neoprene latex) is the watersoluble neoprene emulsion of highly crystalline speed, is preferably height knot
More than one in brilliant speed watersoluble neoprene emulsion I or highly crystalline speed watersoluble neoprene emulsion II；Described highly crystalline speed aqueous
Neoprene emulsion I is more than one in Bayer Bitterfeld GmbH C84 or Japanese east Cao SL-390, described highly crystalline speed watersoluble neoprene emulsion
II is Bayer Bitterfeld GmbH CXP2694, in Bayer Bitterfeld GmbH CXP2717 or Japanese electric apparatus chemistry ALX-800 more than one.
The particle diameter of described hydrophilic gas phase nano silicon dioxide is less than 100 nanometers, below preferably 70 nanometers, described hydrophilic gas
Phase nano silicon specific surface area is more than 200cm2/g。
The pH adjusting agent of described acrylic acid ester emulsion is ammonia or organic amine, and organic amine is low fat amine or alcamines, excellent
Elect moral modest MA-95 amine nertralizer as；The pH adjusting agent of described watersoluble neoprene emulsion is faintly acid aminoacid or boric acid, preferably boron
Acid；
Described aqueous wetting dispersing agent is water solublity wetting dispersing agent, preferably ammonium polyacrylate salt aqueous wetting and dispersing
This moral of agent, preferably hamming modest Disponer W-519 anionic wetting dispersing agent or BYK-152 aqueous polyacrylamide acid ammonium salt
Wetting dispersing agent；
Described zinc oxide fluid dispersion is water nano zinc oxide fluid dispersion；It is purchased from Shenzhen nano development in science and technology company limited；
Described defoamer is silicone modification defoamer, and preferably Polyether Modified Polysiloxanes Defoaming Agent is purchased from middle federation
Defoamer, model B-0518/0519/0520；
Described antioxidant is vitamin E oil, 2,6 ditertiary butyl p cresol or 4-methyl-6-tert base phenol, is preferably
Vitamin E oil.
Described preservative is emulsion preservative JB11, BX90 or BX80, preferably BX90 or BX80.
The viscous preparation method from dry emulsion type adhesive of described speed, comprises the following steps:
(1) stirring under conditions of, use acrylic acid ester emulsion pH adjusting agent regulation acrylic acid ester emulsion pH to 9～
12, obtain alkalescence acrylic acid ester emulsion；Described in step (1), speed of agitator is 300～500 revs/min；
(2) hydrophilic gas phase nano silicon dioxide is dissolved in deionized water, adds aqueous wetting dispersing agent and be uniformly dispersed；Again
Add zinc oxide fluid dispersion to be uniformly dispersed, obtain mixed solution；
(3) mixed solution step (2) prepared adds in the alkaline acrylic acid ester emulsion of step (1), dispersed with stirring 10
～30 minutes, obtain containing crylic acid ester mixture solution；Described in step (3), speed of agitator is 300～500 revs/min；
(4) use the pH to 9～12 of the pH adjusting agent regulation watersoluble neoprene emulsion of watersoluble neoprene emulsion, obtain alkaline aqueous
Neoprene emulsion；
(5) under agitation, the alkaline aqueous neoprene emulsion of step (4) is slowly added into step (3) containing acrylate
In mixed solution, disperse 90～150 minutes, obtain just adhesive；Described in step (5), speed of agitator is 300～500 revs/min
Clock；
(6) adding sterilization antiseptic, antioxidant and defoamer in first adhesive, dispersed with stirring is uniform, filters discharging,
Obtain described speed viscous from dry emulsion type adhesive.
Filter described in step (6) and refer to filter with 150 mesh or less than the filter cloth of 150 mesh.
The viscous emulsion-type adhesive of the viscous speed of a kind of speed, is prepared by above-mentioned preparation method.Described speed is viscous from dry emulsion type gluing
Agent good stability, instantaneous bond effect are good, the most viscous fast, and the open hour are long, and heat resistance water resistance is excellent.
Described speed is viscous is used for the bonding, at sofa, bed of the materials such as leather, sponge, non-woven fabrics, timber from dry emulsion adhesive
Pad, the household articles such as medicated pillow is widely used；Can with roller coat, brush, the various ways such as spraying uses, the most special to sizing equipment
Requirement, more stable more prominent than multiple adhesive product performance currently on the market, cost is lower, easy to use.
Compared with prior art, present invention have the advantage that and beneficial effect:
(1) present invention screening by raw material, self-control vitrification point low, particle diameter is little, just glues, heat resistance good third
Olefin(e) acid ester emulsion, watersoluble neoprene emulsion selects the watersoluble neoprene emulsion of one or both highly crystalline speed, by two kinds of main bodys
The pH value regulation of resin emulsion and the addition of stabilizer improve stability and the concertedness effect of emulsion mixture；
(2) present invention makes emulsion by adding the raw materials such as hydrophilic gas phase nano silicon dioxide, nano zinc oxide fluid dispersion
The heat resistance of adhesive, adhesive property etc. improve further；And the addition of hydrophilic gas phase nano silicon dioxide can improve
The heat resistance of water-soluble spraying glue and dry tolerance energy, stop the emulsion adhesive infiltration to gross porosity footpath base material, so that it is being sprayed
Thing surface forms uniform film；Nano zinc oxide fluid dispersion can further enhance the adhesive strength of above-mentioned adhesive；
(3) present invention improves the combination property of above-mentioned emulsion type adhesive by adding water-soluble multifunctional auxiliary agent,
Add aqueous wetting dispersing agent and improve the dispersion effect of the filler such as hydrophilic gas phase nano silicon dioxide and nano zinc oxide fluid dispersion；
Add defoamer and reduce the preparation of above-mentioned emulsion type adhesive and the blister formation of the process of use, thus promote adhesive practicality
Energy；Add sterilization antiseptic and can suppress antibacterial, prevent emulsion adhesive from storing and adhesives process is putrid and deteriorated；Add anti-
Oxidant can reduce adhesive deterioration by oxidation speed, extends the adhesive bonding life-span.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Acrylic acid ester emulsion in embodiment is prepared by the following method and obtains:
(1) take in the monomer component of acrylic ester synthesizing emulsion: acrylate soft monomer 40～70 parts, hard monomer 0～8
Part, function monomer 1～3 parts, emulsifying agent 0.8～2 parts, initiator 0.3～0.65 part, buffer agent 0.1～0.15 part, deionized water
35～65 parts；
(2) deionized water 20～40 weight portion, emulsifying agent 0.8～2 weight portion, initiator 0.1～0.45 weight portion are added
Enter in reactor, dispersed with stirring 5～10 minutes under 400～600r/min speed conditions；Again at 600～1000r/min rotating speeds
Lower addition acrylate soft monomer 40～70 weight portion, hard monomer 0～8 weight portion, function monomer 1～3 weight portion, pre-emulsification 10
～20 minutes, obtain pre-emulsion；
(3) under agitation, in reactor add 15～25 parts by weight of deionized water, 0.1～0.2 weight portion cause
Agent and 0.1～0.15 weight portion buffer agent are uniformly mixed so as to obtain bottom solution, in the reactor equipped with bottom solution add 10～
The pre-emulsion of 20 mass parts, is warming up to 80～82 DEG C of reactions 30～60min, drips the pre-breast of residual mass part in reactor
Liquid, continuously dropping 2.5～3h, heat up after dropping 84～86 DEG C of insulation reaction 2～2.5h, and cooling is filtered, discharging, obtained
Described acrylic acid ester emulsion.
Described acrylate soft monomer is at least one in lauryl methacrylate and butyl acrylate and acrylic acid
The mixture of different monooctyl ester, wherein Isooctyl acrylate monomer accounts for the 70～90% of acrylate soft monomer gross mass.Described hard monomer is
Acrylic acid methyl ester. or methyl methacrylate；Described function monomer be in acrylamide, acrylic acid and methacrylic acid at least
A kind of mixture with 2-(Acryloyloxy)ethanol；Described emulsifying agent be anionic emulsifier and nonionic emulsifier mixing answer
Co-emulsifier, in described compound emulsifying agent, anionic emulsifier is (10～15) with the mass ratio of nonionic emulsifier: (5
～10), described anionic emulsifier is sodium lauryl sulphate, and described nonionic emulsifier is OP-10；Described initiator
For persulfate, preferably persulfuric acid ammonium salt；Described buffer agent is sodium bicarbonate or sodium carbonate；It is preferably sodium bicarbonate.
Embodiment 1
The viscous preparation method from dry emulsion type adhesive of a kind of speed, comprises the steps:
(1) 50g acrylic acid ester emulsion (particle diameter is that 250～200 nanometers, vitrification point are for-65 DEG C) is taken, at 300 revs/min
Under clock stirring condition, with moral modest MA-95 amine nertralizer, ph value of emulsion is adjusted to 9, obtains alkalescence acrylic acid ester emulsion；
(2) 0.75g hydrophilic gas phase nano silicon dioxide (particle diameter is below 100 nanometers) is taken, water-soluble with the deionization of 7.5g
Solve；The moral modest Disponer W-519 anionic wetting dispersing agent adding 0.15g is uniformly dispersed, and adds 0.75g nano oxygen
Change zinc dispersion liquid to be uniformly dispersed, obtain mixed solution；
(3) mixed solution step (2) prepared adds in the alkaline acrylic acid ester emulsion of step (1), at 500 revs/min
Disperse 10 minutes under clock stirring condition, obtain containing crylic acid ester mixture solution；
(4) weigh 80g highly crystalline speed watersoluble neoprene emulsion II (Japanese electric apparatus chemistry watersoluble neoprene latex A LX-800) and
20g highly crystalline speed watersoluble neoprene emulsion I (east Cao's watersoluble neoprene emulsion SL-390), is adjusted to 9 with boric acid by pH value, obtains alkalescence
Watersoluble neoprene emulsion；
(5) under agitation (rotating speed 500 revs/min), the alkaline aqueous neoprene emulsion of step (4) is slowly added into step
Suddenly (3) are containing in crylic acid ester mixture solution, disperse 90 minutes, obtain just adhesive；
(6) add in first adhesive sterilization antiseptic JB11,0.15g of 0.15g DBPC 2,6 ditertiary butyl p cresol and
The Polyether Modified Polysiloxanes Defoaming Agent B-0518 of 0.15g, keeps 500 revs/min of conditions of rotating speed to be uniformly dispersed, with the filter of 150 mesh
Cloth filters discharging, obtains described speed viscous from dry emulsion type adhesive.
Embodiment 2
The viscous preparation method from dry emulsion type adhesive of a kind of speed comprises the steps:
(1) 60g acrylic acid ester emulsion (particle diameter is that 150～200 nanometers, vitrification point are for-60 DEG C) is taken, at 400 revs/min
Under clock stirring condition, with ethylenediamine, ph value of emulsion is adjusted to 10, obtains alkalescence acrylic acid ester emulsion；
(2) the hydrophilic gas phase nano silicon dioxide that 1.2g particle diameter is below 70 nanometers is weighed, water-soluble with the deionization of 9.6g
Solve；The moral modest Disponer W-519 anionic wetting dispersing agent adding 0.24g is uniformly dispersed, and adds 1.2g nano zine oxide
Dispersion liquid is uniformly dispersed, and obtains mixed solution；
(3) mixed solution step (2) prepared adds in the alkaline acrylic acid ester emulsion of step (1), at 400 revs/min
Disperse 15 minutes under clock stirring condition, obtain containing crylic acid ester mixture solution；
(4) 60g highly crystalline speed watersoluble neoprene emulsion II (Bayer watersoluble neoprene emulsion CXP2694) and 40g height knot are weighed
Brilliant speed watersoluble neoprene emulsion I (east Cao's watersoluble neoprene emulsion SL-390), is adjusted to 10 with boric acid by pH value, obtains alkaline aqueous chlorine
Fourth emulsion；
(5) under agitation (rotating speed 400 revs/min), the alkaline aqueous neoprene emulsion of step (4) is slowly added into step
Suddenly (3) are containing in crylic acid ester mixture solution, disperse within 100 minutes, to obtain just adhesive；
(6) in first adhesive, add the DBPC 2,6 ditertiary butyl p cresol of sterilization antiseptic BX90,0.224g of 0.224g
With the Polyether Modified Polysiloxanes Defoaming Agent B-0519 of 0.224g, keep 400 revs/min of conditions of rotating speed to be uniformly dispersed, use 100 purposes
Filter-cloth filtering discharging, obtains described speed viscous from dry emulsion type adhesive.
Embodiment 3
The viscous preparation method from dry emulsion type adhesive of a kind of speed comprises the steps:
(1) 80g acrylic acid ester emulsion (particle diameter is that below 150 nanometers, vitrification point are for-65 DEG C) is taken, at 400 revs/min
Under clock stirring condition, with ethylenediamine, ph value of emulsion is adjusted to 10, obtains alkalescence acrylic acid ester emulsion；
(2) 2.16g hydrophilic gas phase nano silicon dioxide (particle diameter is for less than 70 nanometers) is weighed, with the deionized water of 12.6g
Dissolve；The BYK-152 aqueous polyacrylamide acid ammonium salt wetting dispersing agent adding 0.45g is uniformly dispersed, and adds 2.25g nano zine oxide
Dispersion liquid is uniformly dispersed, and obtains mixed solution；
(3) mixed solution step (2) prepared adds in the alkaline acrylic acid ester emulsion of step (1), at 400 revs/min
Disperse 15 minutes under clock stirring condition, obtain containing crylic acid ester mixture solution；
(4) 40g highly crystalline speed watersoluble neoprene emulsion II (Bayer watersoluble neoprene emulsion CXP2717) is weighed；Tie with 60g height
Brilliant speed watersoluble neoprene emulsion I (Bayer watersoluble neoprene emulsion C84), is adjusted to 10 with boric acid by pH value, obtains alkaline aqueous neoprene
Emulsion；
(5) under agitation (rotating speed 400 revs/min), the alkaline aqueous neoprene emulsion of step (4) is slowly added into step
Suddenly (3) are containing in crylic acid ester mixture solution, disperse 120 minutes, obtain just adhesive；
(6) in first adhesive, add the vitamin E oil of sterilization antiseptic BX80,0.324g of 0.324g and 0.324g
Polyether Modified Polysiloxanes Defoaming Agent B-0520, keeps 400 revs/min of conditions of rotating speed to be uniformly dispersed, goes out with the filter-cloth filtering of 150 mesh
Material, obtains described speed viscous from dry emulsion type adhesive.
Embodiment 4
The viscous preparation method from dry emulsion type adhesive of a kind of speed comprises the steps:
(1) take 100g acrylic acid ester emulsion (particle diameter is that 150～200 nanometers, vitrification point are for-55 DEG C), 400 turns/
Under minute stirring condition, with ethylenediamine, ph value of emulsion is adjusted to 11, obtains alkalescence acrylic acid ester emulsion；
(2) 3g hydrophilic gas phase nano silicon dioxide (particle diameter is for less than 100 nanometers) is weighed, with the deionized water dissolving of 16g；
The BYK-152 aqueous polyacrylamide acid ammonium salt wetting dispersing agent adding 0.6g is uniformly dispersed, and adds 3g nano zinc oxide fluid dispersion and divides
Dissipate uniformly, obtain mixed solution；
(3) mixed solution step (2) prepared adds in the alkaline acrylic acid ester emulsion of step (1), at 300 revs/min
Disperse 20 minutes under clock stirring condition, obtain containing crylic acid ester mixture solution；
(4) 20g highly crystalline speed watersoluble neoprene emulsion II (Bayer watersoluble neoprene emulsion CXP2694) and 80g height knot are weighed
Brilliant speed watersoluble neoprene emulsion I (Bayer watersoluble neoprene emulsion C84), is adjusted to 11 with boric acid by pH value, obtains alkaline aqueous neoprene
Emulsion；
(5) under agitation (rotating speed is 300 revs/min), the alkaline aqueous neoprene emulsion of step (4) is slowly added into
Step (3), containing in crylic acid ester mixture solution, is disperseed 150 minutes, obtains just adhesive；
(6) add in first adhesive 0.4g the vitamin E oil of sterilization antiseptic BX80,0.4g and the polyethers of 0.4g
Modified organic silicon defoamer B-0518, keeps 300 revs/min of conditions of rotating speed to be uniformly dispersed, with the filter-cloth filtering discharging of 150 mesh,
Obtain described speed viscous from dry emulsion type adhesive.
Embodiment 5
The viscous preparation method from dry emulsion type adhesive of a kind of speed comprises the steps:
(1) 120g acrylic acid ester emulsion (particle diameter is that below 150 nanometers, vitrification point are for-50 DEG C) is taken, at 400 revs/min
Under clock stirring condition, with triethylamine, ph value of emulsion is adjusted to 12, obtains alkalescence acrylic acid ester emulsion；
(2) 3.3g hydrophilic gas phase nano silicon dioxide (particle diameter is for less than 70 nanometers) is weighed, water-soluble with the deionization of 17.6g
Solve；The Disponer W-519 anionic wetting dispersing agent adding 0.66g is uniformly dispersed, and adds the dispersion of 3.3g nano zine oxide
Liquid is uniformly dispersed, and obtains mixed solution；
(3) mixed solution step (2) prepared adds in the alkaline acrylic acid ester emulsion of step (1), at 300 revs/min
Disperse 30 minutes under clock stirring condition, obtain containing crylic acid ester mixture solution；
(4) weigh 100g highly crystalline speed watersoluble neoprene emulsion I (Bayer watersoluble neoprene emulsion C84), use faintly acid amino
PH value is adjusted to 12 by acid, obtains alkaline aqueous neoprene emulsion；
(5) under agitation (rotating speed 400 revs/min), the alkaline aqueous neoprene emulsion of step (4) is slowly added into step
Suddenly (3) are containing in crylic acid ester mixture solution, disperse 130 minutes, obtain just adhesive；
(6) in first adhesive add 0.44g sterilization antiseptic BX90,0.44g 4-methyl-6-tert base phenol and
The Polyether Modified Polysiloxanes Defoaming Agent B-0519 of 0.44g, keeps 300 revs/min of conditions of rotating speed to be uniformly dispersed, with the filter of 150 mesh
Cloth filters discharging, obtains described speed viscous from dry emulsion type adhesive.
Embodiment 6
The viscous preparation method from dry emulsion type adhesive of a kind of speed, comprises the steps:
(1) 200g acrylic acid ester emulsion (particle diameter is that below 150 nanometers, vitrification point are for-50 DEG C) is taken, at 400 revs/min
Under clock stirring condition, with ammonia, acrylic acid ester emulsion pH value is adjusted to 11, obtains alkalescence acrylic acid ester emulsion；
(2) 1.5g hydrophilic gas phase nano silicon dioxide (particle diameter is for less than 70 nanometers) is weighed, water-soluble with the deionization of 15g
Solve；The BYK-152 aqueous polyacrylamide acid ammonium salt wetting dispersing agent adding 0.3g is uniformly dispersed, and adds the dispersion of 1.5g nano zine oxide
Liquid is uniformly dispersed, and obtains mixed solution；
(3) mixed solution of step (2) is added in the alkaline acrylic acid ester emulsion of step (1), stir at 400 revs/min
Disperse 20 minutes under the conditions of mixing, obtain containing acrylic acid ester emulsion；
(4) weigh 100g highly crystalline speed watersoluble neoprene emulsion II (Japanese electric apparatus chemistry ALX-800), use faintly acid amino
PH value is adjusted to 11 by acid, obtains alkaline aqueous neoprene emulsion；
(5) under agitation (rotating speed 300 revs/min), the alkaline aqueous neoprene emulsion of step (4) is slowly added into step
Suddenly (3) are containing in crylic acid ester mixture solution, disperse 140 minutes, obtain just adhesive；
(6) in first adhesive add 0.3g sterilization antiseptic JB11,0.3g 4-methyl-6-tert base phenol and
The Polyether Modified Polysiloxanes Defoaming Agent B-0520 of 0.3g, keeps 300 revs/min of conditions of rotating speed to be uniformly dispersed, with the filter cloth of 100 mesh
Filter discharging, obtain described speed viscous from dry emulsion type adhesive.
It is as follows that the speed of embodiment 1～6 preparation glues air-dry water-based emulsion-type adhesive performance test methods, test result such as table
Shown in 1 and 2:
1. the most viscous time test condition: cut the high-density sponge foam of 12*10*1cm specification, glue is evenly coated in sea
Continuous side, width about 2cm, immediately after by sponge doubling, sponge can mutually bond, and does not apply external force two surface and does not separates
Separate；
The most instantaneous cohesive force performance test conditions: cut the height of 12*10*2cm, 12*10*1.5cm and 12*10*1cm specification
Density foam foam, is evenly coated in sponge side glue, width about 2cm, and immediately after by sponge doubling, sponge can phase
Bonding, does not apply external force and does not flicks, be then followed successively by excellent, good, general mutually；
The most repeatedly paste number of times test condition: cut the high-density sponge foam of 12*10*1cm specification, glue is uniformly coated with
In sponge side, width about 2cm, by bonding for sponge doubling, sponge can paste number of times repeatedly；
4 open hour test conditions: cut the high-density sponge foam of 12*10*1cm specification, glue is evenly coated in sea
Continuous side, width about 2cm, at 25 DEG C, under 50% damp condition, placement certain time, by bonding for sponge doubling, records permissible
Bonding standing time；
5. high-temperature stability test condition: be placed in by the testing sample of preparation in 50 DEG C of baking ovens, takes out after standing 72h, sees
Examine and whether produce flocculation breakdown of emulsion, if having instantaneous adhesive property, there is no breakdown of emulsion and have instantaneous adhesive property then to pass through；
The most heat-resisting test condition: after the sponge after bonding is placed 24h, be placed in 85 DEG C together, in the baking oven of 75% humidity,
Observation flicks the time；
The most resistance to aqueous alkali test condition: after the sponge after bonding is placed 24h, be placed in 40 DEG C of thermokalite water, pass through washing machine
It is a circulating water wash with 30min, records the washing times that do not comes unglued.
Table 1 speed glues the physical property from dry emulsion type adhesive and performance parameter
The fast physical property glued from dry emulsion type adhesive of table 2 and performance parameter:
Above example is some embodiments of the present invention, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
It is the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. a speed is viscous from dry emulsion type adhesive, it is characterised in that: include following component: acrylic acid ester emulsion, watersoluble neoprene
Emulsion；Deionized water, hydrophilic gas phase nano silicon dioxide, pH adjusting agent, aqueous wetting dispersing agent, zinc oxide fluid dispersion, froth breaking
Agent, sterilization antiseptic, antioxidant；Described acrylic acid ester emulsion and watersoluble neoprene emulsion are matrix resin emulsion；Described pH adjusts
Joint agent is pH adjusting agent and the pH adjusting agent of watersoluble neoprene emulsion of acrylic acid ester emulsion.
The most according to claim 1, speed is viscous from dry emulsion type adhesive, it is characterised in that: the glass of described acrylic acid ester emulsion
Changing temperature≤-50 DEG C, described acrylic acid ester emulsion viscosity is 100～200mPa.s；Particle diameter≤250 of described acrylic acid ester emulsion
Nanometer；
Described watersoluble neoprene emulsion is the watersoluble neoprene emulsion of highly crystalline speed.
The most according to claim 2, speed is viscous from dry emulsion type adhesive, it is characterised in that: described watersoluble neoprene emulsion is high knot
More than one in brilliant speed watersoluble neoprene emulsion I or highly crystalline speed watersoluble neoprene emulsion II；Described highly crystalline speed aqueous
Neoprene emulsion I is more than one in Bayer Bitterfeld GmbH C84 or Japanese east Cao SL-390, described highly crystalline speed watersoluble neoprene emulsion
II is Bayer Bitterfeld GmbH CXP2694, in Bayer Bitterfeld GmbH CXP2717 or Japanese electric apparatus chemistry ALX-800 more than one.
The most according to claim 1, speed is viscous from dry emulsion type adhesive, it is characterised in that: described hydrophilic gas phase nano titanium dioxide
Particle diameter≤100 nanometer of silicon, specific surface area >=200cm2/g；
The pH adjusting agent of described acrylic acid ester emulsion is ammonia or organic amine；The pH adjusting agent of described watersoluble neoprene emulsion is weak acid
Acidic amino acid or boric acid；
Described aqueous wetting dispersing agent is ammonium polyacrylate salt aqueous wetting dispersing agent；
Described zinc oxide fluid dispersion is water nano zinc oxide fluid dispersion；
Described defoamer is silicone modification defoamer；Described antioxidant is vitamin E oil, DBPC 2,6 ditertiary butyl p cresol
Or 4-methyl-6-tert base phenol；
Described preservative is emulsion preservative JB11, BX90 or BX80.
The most according to claim 4, speed is viscous from dry emulsion type adhesive, it is characterised in that: described defoamer is polyether-modified to have
Machine silicon defoaming agent；
Described antioxidant is vitamin E oil；Described preservative is BX90 or BX80.
The most according to claim 1, speed is viscous from dry emulsion type adhesive, it is characterised in that: the pH of described acrylic acid ester emulsion adjusts
Joint agent regulation acrylic acid ester emulsion pH is 9～12；Watersoluble neoprene emulsion pH adjusting agent regulation watersoluble neoprene emulsion pH be 9～
12。
The most according to claim 1, speed is viscous from dry emulsion type adhesive, it is characterised in that: propylene in described matrix resin emulsion
Acid esters emulsion is (0.5～2) with the mass ratio of watersoluble neoprene emulsion: 1；
The quality of described deionized water is the 5～8% of described matrix resin quality of the emulsion；
Quality is described matrix resin quality of the emulsion the 0.5～1.5% of described hydrophilic gas phase nano silicon dioxide；
The quality of described aqueous wetting dispersing agent is the 0.1～0.3% of described matrix resin quality of the emulsion；
The quality of described zinc oxide fluid dispersion is the 0.5～1.5% of described matrix resin quality of the emulsion；
The quality of described defoamer is the 0.1～0.2% of described matrix resin quality of the emulsion；
The quality of described sterilization antiseptic is the 0.1～0.2% of described matrix resin quality of the emulsion；
The quality of described antioxidant is the 0.1～0.2% of described matrix resin quality of the emulsion.
8. according to the viscous preparation method from dry emulsion type adhesive of speed described in any one of claim 1～7, it is characterised in that: bag
Include following steps:
(1) under conditions of stirring, the pH to 9～12 of the pH adjusting agent regulation acrylic acid ester emulsion of acrylic acid ester emulsion is used,
Obtain alkalescence acrylic acid ester emulsion；
(2) hydrophilic gas phase nano silicon dioxide is dissolved in deionized water, adds aqueous wetting dispersing agent and be uniformly dispersed；Add
Zinc oxide fluid dispersion is uniformly dispersed, and obtains mixed solution；
(3) mixed solution step (2) prepared adds in the alkaline acrylic acid ester emulsion of step (1), dispersed with stirring 10～30
Minute, obtain containing crylic acid ester mixture solution；
(4) use the pH to 9～12 of the pH adjusting agent regulation watersoluble neoprene emulsion of watersoluble neoprene emulsion, obtain alkaline aqueous neoprene
Emulsion；
(5) under agitation, the alkaline aqueous neoprene emulsion of step (4) is slowly added into step (3) containing crylic acid ester mixture
In solution, disperse 90～150 minutes, obtain just adhesive；
(6) adding sterilization antiseptic, antioxidant and defoamer in first adhesive, dispersed with stirring is uniform, filters discharging, obtains
Described speed is viscous from dry emulsion type adhesive.
The viscous preparation method from dry emulsion type adhesive of speed the most according to claim 8, it is characterised in that: institute in step (1)
Stating speed of agitator is 300～500 revs/min；Described in step (3), speed of agitator is 300～500 revs/min；In step (5)
Described speed of agitator is 300～500 revs/min；
Filter described in step (6) and refer to filter with 150 mesh or less than the filter cloth of 150 mesh.
10. according to the viscous application from dry emulsion type adhesive of speed described in any one of claim 1～7, it is characterised in that: described speed
The viscous bonding and household articles bonding being used for material from dry emulsion adhesive；Described material bonding includes leather, sponge, nonwoven
Cloth, timber.
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