CN106590475A - Novel acrylic ester glue and preparation method thereof - Google Patents
Novel acrylic ester glue and preparation method thereof Download PDFInfo
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- CN106590475A CN106590475A CN201610912415.5A CN201610912415A CN106590475A CN 106590475 A CN106590475 A CN 106590475A CN 201610912415 A CN201610912415 A CN 201610912415A CN 106590475 A CN106590475 A CN 106590475A
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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
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention relates to a novel acrylic ester glue, which comprises the following components: isooctyl acrylate, isobutyl acrylate, isomethyl acrylate, hydroxyethyl ester, glyceride, acrylic acid, ethyl acetate, toluene, methanol, benzoyl peroxide, and peroxide Al13N. The peroxide Al13N added in the components can protect acrylic ester glue from being oxidized by oxygen in the air during use, improves the glue stability, thermal conductivity, abrasion resistance, high temperature resistance, anticorrosion performance and other comprehensive performance, and ensures the high quality of the glue. In the preparation process, ethyl acetate is added in three times successively at different amounts, 50wt% of the raw materials are put into a reaction kettle as the kettle bottom material, and the rest 50% are added dropwise after intense reaction, the dripping time is controlled within 1h, the whole reaction lasts 3h, the reaction time is greatly shortened, the production efficiency is improved, and the preparation process is simple, therefore the method is suitable for large-scale industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method technical field of glue, and in particular to a kind of novel acrylic ester glue and its
Preparation method.
Background technology
Traditional acrylate glue carries out polymerisation in solution by acrylic ester monomer or emulsion polymerization is made, its preparation
Method is：By cooling down storage tank in reaction storage tank, reaction heat is taken away, can be used to prepare pressure sensitive adhesive, it is also possible to for direct
Bonding miscellaneous part, but there are following defects in traditional acrylate glue and preparation method thereof：
(1) formula is unreasonable, causes the performance of glue not good；Such as：Higher anti-Static Shear Strength, higher stripping
Power, high temperature resistant, preferably resisting ageing for long time, conformable to gluing of surfaces, low organic gas volatilization, low-surface-energy material bonding；
(2) response time is oversize, and a usual batch complete response time was more than 10 hours；
(3) preparation method step is more complicated.
Accordingly, it would be desirable to develop a kind of new glue and its existing glue preparation method is improved.
The content of the invention
It is an object of the present invention to provide a kind of novel acrylic ester pressure-sensitive glue and preparation method thereof.
To solve above-mentioned technical problem, above-mentioned purpose is realized, technical scheme is as follows：
A kind of novel acrylic ester glue, including the component of following parts by weight：Acrylate monomer 150-200 parts, hydroxyl
Ethyl ester 10-15 parts, glyceride 0.2-0.8 parts, acrylic acid 1-2 parts, organic solvent 220-285 parts, initiator 0.2-0.4 parts, mistake
Oxidation Al13N 0.1-0.4 parts；
Preferably, described acrylate monomer includes following components：Isooctyl acrylate monomer, Isobutyl 2-propenoate, propylene
The different methyl ester of acid；Described organic solvent includes following components：Ethyl acetate, toluene, methanol；Described initiator is benzoyl peroxide
Formyl；
Preferably, described a kind of novel acrylic ester glue, the parts by weight of each component are Isooctyl acrylate monomer 120-
150 parts, Isobutyl 2-propenoate 20-30 parts, the different methyl ester 10-20 parts of acrylic acid, hydroxyl ethyl ester 10-15 part, glyceride 0.2-0.8 parts,
Acrylic acid 1-2 parts, ethyl acetate 170-200 parts, toluene 35-55 parts, methanol 15-30 parts, benzoyl peroxide 0.2-0.4 parts,
Peroxidating Al13N 0.1-0.4 parts；
Preferably, described a kind of novel acrylic ester glue, the parts by weight of each component are Isooctyl acrylate monomer 135
Part, 25 parts of Isobutyl 2-propenoate, 15 parts of the different methyl ester of acrylic acid, 13 parts of hydroxyl ethyl ester, 0.5 part of glyceride, 1.5 parts of acrylic acid, acetic acid
185 parts of ethyl ester, 45 parts of toluene, 22.5 parts of methanol, 0.3 part of benzoyl peroxide, peroxidating Al130.25 part of N；
A kind of preparation method of novel acrylic ester pressure-sensitive glue of the present invention is comprised the following steps that：
(1) by acrylate monomer, hydroxyl ethyl ester, glyceride, acrylic acid, organic solvent, initiator and peroxidating Al13N is dilute
Release and be sufficiently mixed after several times, in being added to glue reactor, addition is 50%, carry out at the uniform velocity stirring reaction, reactor turns
Speed is 10 revs/min；
(2) heating mode is opened, repeatedly lasting slow heating heats up, and temperature rises to 94 ± 2 DEG C in reactor, until instead
Answer and occur in kettle boiling phenomenon just to stop heating up, be incubated 15-30min；
(3) after intense reaction, then it is added drop-wise to remaining 50% as dropping liquid in reactor, time for adding is set in
45min-60min, simultaneous reactions kettle rotating speed is set to 60 revs/min to carry out being sufficiently stirred for reaction, the temperature during Deca in reactor
Degree control is at 94 ± 2 DEG C；
(4) reactor carries out insulation 90min-120min after completion of dropwise addition, persistently stirs, until reaction kettle for reaction is stopped
Only, till glue surface is steady；
(5) after reaction terminates, reactor stops stirring, and question response kettle is down to room temperature, and filtering and discharging gets product.
Preferably, extension rate is 1-5 times in the step (1)；
Preferably, the acrylate monomer in described step (1) is Isooctyl acrylate monomer, Isobutyl 2-propenoate, propylene
The different methyl ester of acid；Described organic solvent is ethyl acetate, three kinds of organic solvents of toluene and methanol；Described initiator is peroxidating
Benzoyl；
Preferably, the mixing in described step (1) is comprised the following steps：First by acrylate monomer, hydroxyl ethyl ester, glycerol
Ester, acrylic acid are added in reactor, are subsequently added into the ethyl acetate of a part；Again with toluene, formaldehyde is by benzoyl peroxide
It is added to after dissolving in reactor, is subsequently added into the ethyl acetate of a part；Add peroxidating Al13N, is eventually adding remaining
Reaction is sufficiently stirred for after ethyl acetate；
Preferably, the ratio of weight and number of described ethyl acetate successively three additions is 95:10:80；
Preferably, the reactor is sending out for the Application No. 201610439476.4 that applicant applies in 2016.06.20
Efficient glue reactor described in bright patent.
Isooctyl acrylate monomer can be used to manufacture coating, binding agent, fiber and fabric-modifying, processing aid, and leather processing is helped
Agent etc.；As polymerized monomer, for soft polymer, internal plasticization is played in the copolymer；Also serve as solvent.It is mainly used as system
Make the soft monomer of acrylate solvent-borne type and emulsion-type pressure-sensitive；Also serve as the main list of production note pad microspheric pressure sensitive adhesive
Body；For synthetic fabrics processing, and make adhesive (anti-wound pressure sensitive adhesive).
Isobutyl 2-propenoate is the monomer of organic synthesiss, for synthetic resin, plastics, coating, printing-ink, adhesive,
Lube oil additive, dental materialss, fibre finish, paper finishing agent etc..
The different methyl ester of acrylic acid is a kind of important organic synthesiss monomer and raw material, high with not being polymerized when less than 10 DEG C
The characteristics of polymerization being susceptible to when 10 DEG C；Light, heat, peroxide etc. can all accelerate its polymerization；It is organic synthesiss
The monomer of intermediate and high molecular polymer, is widely used as adhesive, coating, leather and sheet processing auxiliary agent etc..
Acrylic acid is important organic synthesiss raw material and synthetic resin monomer, is the very fast vinyl list of polymerization speed
Body；Great majority are to manufacture the esters of acrylic acids such as acrylic acid methyl ester., ethyl ester, butyl ester, hydroxyl ethyl ester；Acrylic acid and acrylate can be with
Homopolymerization and copolymerization, its polymer is used for the industrial departments such as synthetic resin, synthetic fibers, super absorbent resin, building materials, coating.
Ethyl acetate, is a kind of broad-spectrum fine chemical product, is also one with excellent dissolubility, quick-drying
Plant very important Organic Chemicals and fabulous industrial solvent.
Toluene, is the important source material of organic chemical industry, stable chemical nature, 103 DEG C of boiling point, in a large number as acrylate monomer
The dielectric solvent of polymerization synthesis.
Methanol, is a kind of solvent more more preferable than ethanol, can dissolve many inorganic salts.
Benzoyl peroxide, is a kind of strong oxidizer, with strong oxidizing property, is easily reduced to benzoic acid, is adhesives industries
Most widely used initiator.
Peroxidating Al13N, is a kind of nanocluster, with good heat conductivility, while with excellent abrasion performance
Can, the mixing uniformity and stability of formula each component can be improved, while the resistance to elevated temperatures and anti-corrosion of glue can also be improved
Performance.
The invention has the beneficial effects as follows：A kind of novel acrylic ester glue of the present invention, adds peroxidating in component
Al13N, with protection acrylate glue by the dioxygen oxidation in air, will not improve in use glue stability,
The combination properties such as heat conductivity, abrasion resistance, resistance to elevated temperatures and antiseptic property, it is ensured that the high-quality of glue；In preparation technology
In three times not commensurability sequencing is added ethyl acetate, and by reacting the raw material of 50% weight as bottom material input
Kettle, afterwards 50% after intense reaction Deca, in time for adding control 1h, whole response time 3h reaction terminates, and the response time is big
It is big to shorten, production efficiency is improve, preparation process is simple is adapted to large-scale industrial production.
Specific embodiment
Below by specific embodiment, the present invention is described further, but embodiment is not intended to limit the protection of the present invention
Scope.
Embodiment 1
A kind of novel acrylic ester glue, including the component of following weight：Acrylate monomer 3750g, hydroxyl ethyl ester 250g,
Glyceride 5g, acrylic acid 25g, organic solvent 5500g, initiator 5g, peroxidating Al13N 2.5g；
Preferably, described acrylate monomer includes following components：Isooctyl acrylate monomer, Isobutyl 2-propenoate, propylene
The different methyl ester of acid；Described organic solvent includes following components：Ethyl acetate, toluene, methanol；Described initiator is benzoyl peroxide
Formyl；
Preferably, described a kind of novel acrylic ester glue, the weight of each component be Isooctyl acrylate monomer 3000g, third
The different methyl ester 250g of olefin(e) acid isobutyl ester 500g, acrylic acid, hydroxyl ethyl ester 250g, glyceride 5g, acrylic acid 25g, ethyl acetate 4250g,
Toluene 875g, methanol 375g, benzoyl peroxide 5g, peroxidating Al13N 2.5g；
A kind of preparation method of novel acrylic ester pressure-sensitive glue of the present invention is comprised the following steps that：
(1) by Isooctyl acrylate monomer 1500g, Isobutyl 2-propenoate 250g, the different methyl ester 125g of acrylic acid, hydroxyl ethyl ester 125g,
Glyceride 2.5g, acrylic acid 12.5g, toluene 437.5g, methanol 187.5g, peroxidating toluoyl 2.5g and peroxidating Al13N
1.25g is sufficiently mixed after being diluted 1 times, in being added to glue reactor, carries out at the uniform velocity stirring reaction, and reactor rotating speed is 10
Rev/min；
(2) heating mode is opened, repeatedly lasting slow heating heats up, and temperature rises to 94 ± 2 DEG C in reactor, until instead
Answer and occur in kettle boiling phenomenon just to stop heating up, be incubated 15min；
(3) it is after intense reaction then remaining Isooctyl acrylate monomer 1500g, Isobutyl 2-propenoate 250g, acrylic acid is different
Methyl ester 125g, hydroxyl ethyl ester 125g, glyceride 2.5g, acrylic acid 12.5g, toluene 437.5g, methanol 187.5g, peroxidating toluoyl
2.5g and peroxidating Al13N 1.25g are added drop-wise in reactor as dropping liquid, and time for adding is set in 45min, simultaneous reactions kettle
Rotating speed is set to 60 revs/min to carry out being sufficiently stirred for reaction, and the temperature control during Deca in reactor is at 94 ± 2 DEG C；
(4) reactor carries out insulation 120min after completion of dropwise addition, persistently stirs, until reaction kettle for reaction stops, glue surface
Till steady；
(5) after reaction terminates, reactor stops stirring, and question response kettle is down to room temperature, and filtering and discharging gets product.
Preferably, the mixing in described step (1) is comprised the following steps：First by Isooctyl acrylate monomer 1500g, acrylic acid
The different methyl ester 125g of isobutyl ester 250g, acrylic acid, hydroxyl ethyl ester 125g, glyceride 2.5g, acrylic acid 12.5g are added in reactor,
It is subsequently added into 2182.5g ethyl acetates；Again with toluene 437.5g, methanol 187.5g will be added after benzoyl peroxide 2.5g dissolvings
To in reactor, 229.7g ethyl acetates are subsequently added into；Add peroxidating Al13N 1.25g, are eventually adding 1837.8g acetic acid
Reaction is sufficiently stirred for after ethyl ester；
Preferably, the reactor is sending out for the Application No. 201610439476.4 that applicant applies in 2016.06.20
Efficient glue reactor described in bright patent.
Embodiment 2
A kind of novel acrylic ester glue, including the component of following parts by weight：Acrylate monomer 5000g, hydroxyl ethyl ester
375g, glyceride 20g, acrylic acid 50g, organic solvent 7125g, initiator 10g, peroxidating Al13N 10g；
Preferably, described acrylate monomer includes following components：Isooctyl acrylate monomer, Isobutyl 2-propenoate, propylene
The different methyl ester of acid；Described organic solvent includes following components：Ethyl acetate, toluene, methanol；Described initiator is benzoyl peroxide
Formyl；
Preferably, described a kind of novel acrylic ester glue, the parts by weight of each component are Isooctyl acrylate monomer
The different methyl ester 500g of 3750g, Isobutyl 2-propenoate 750g, acrylic acid, hydroxyl ethyl ester 375g, glyceride 20g, acrylic acid 50g, acetic acid second
Ester 5000g, toluene 1375g, methanol 750g, benzoyl peroxide 10g, peroxidating Al13N 10g；
A kind of preparation method of novel acrylic ester pressure-sensitive glue of the present invention is comprised the following steps that：
(1) by Isooctyl acrylate monomer 1875g, Isobutyl 2-propenoate 375g, the different methyl ester 250g of acrylic acid, hydroxyl ethyl ester
187.5g, glyceride 10g, acrylic acid 25g, ethyl acetate 2500g, toluene 687.5g, methanol 375g, benzoyl peroxide 5g,
Peroxidating Al13N 5g are sufficiently mixed after being diluted 5 times, in being added to glue reactor, carry out at the uniform velocity stirring reaction, reactor
Rotating speed is 10 revs/min；
(2) heating mode is opened, repeatedly lasting slow heating heats up, and temperature rises to 94 ± 2 DEG C in reactor, until instead
Answer and occur in kettle boiling phenomenon just to stop heating up, be incubated 30min；
(3) it is after intense reaction then remaining Isooctyl acrylate monomer 1875g, Isobutyl 2-propenoate 375g, acrylic acid is different
Methyl ester 250g, hydroxyl ethyl ester 187.5g, glyceride 10g, acrylic acid 25g, ethyl acetate 2500g, toluene 687.5g, methanol 375g,
Benzoyl peroxide 5g, peroxidating Al13N 5g are added drop-wise in reactor as dropping liquid, and time for adding is set in 60min, while
Reactor rotating speed is set to 60 revs/min to carry out being sufficiently stirred for reaction, and the temperature control during Deca in reactor is at 94 ± 2 DEG C；
(4) reactor carries out insulation 90min after completion of dropwise addition, persistently stirs, until reaction kettle for reaction stops, glue surface is put down
Till steady；
(5) after reaction terminates, reactor stops stirring, and question response kettle is down to room temperature, and filtering and discharging gets product.
Preferably, the acrylate monomer in described step (1) is Isooctyl acrylate monomer, Isobutyl 2-propenoate, propylene
The different methyl ester of acid；Described organic solvent is ethyl acetate, three kinds of organic solvents of toluene and methanol；Described initiator is peroxidating
Benzoyl；
Preferably, the mixing in described step (1) is comprised the following steps：First by Isooctyl acrylate monomer 1875g, acrylic acid
The different methyl ester 250g of isobutyl ester 375g, acrylic acid, hydroxyl ethyl ester 187.5g, glyceride 10g, acrylic acid 25g are added in reactor, are connect
Addition 2567.5g ethyl acetates；Again with toluene 687.5g, methanol 375g will be added to reaction after benzoyl peroxide 5g dissolvings
In kettle, 270.3g ethyl acetates are subsequently added into；Add peroxidating Al13N5g, is eventually adding after 2162.2g ethyl acetates fully
Stirring reaction；
Preferably, the reactor is sending out for the Application No. 201610439476.4 that applicant applies in 2016.06.20
Efficient glue reactor described in bright patent.
Embodiment 3
A kind of novel acrylic ester glue, including the component of following weight：Acrylate monomer 4375g parts, hydroxyl ethyl ester
325g, glyceride 12.5g, acrylic acid 37.5g, organic solvent 6312.5g, initiator 7.5g, peroxidating Al13N 6.25g；
Preferably, described acrylate monomer includes following components：Isooctyl acrylate monomer, Isobutyl 2-propenoate, propylene
The different methyl ester of acid；Described organic solvent includes following components：Ethyl acetate, toluene, methanol；Described initiator is benzoyl peroxide
Formyl；
Preferably, described a kind of novel acrylic ester glue, the weight of each component be Isooctyl acrylate monomer 3375g, third
The different methyl ester 375g of olefin(e) acid isobutyl ester 625g, acrylic acid, hydroxyl ethyl ester 325g, glyceride 12.5g, acrylic acid 37.5g, ethyl acetate
4625g, toluene 1125g, methanol 562.5g, benzoyl peroxide 7.5g, peroxidating Al13N 6.25g；
A kind of preparation method of novel acrylic ester pressure-sensitive glue of the present invention is comprised the following steps that：
(1) by Isooctyl acrylate monomer 1687.5g, Isobutyl 2-propenoate 312.5g, the different methyl ester 187.5g of acrylic acid, hydroxyl ethyl ester
162.5g, glyceride 6.25g, acrylic acid 18.75g, ethyl acetate 2312.5g, toluene 562.5g, methanol 281.25g, peroxidating
Benzoyl 3.75g, peroxidating Al13N 3.125g are sufficiently mixed after diluting 3 times, in being added to glue reactor, are at the uniform velocity stirred
Reaction is mixed, reactor rotating speed is 10 revs/min；
(2) heating mode is opened, repeatedly lasting slow heating heats up, and temperature rises to 94 ± 2 DEG C in reactor, until instead
Answer and occur in kettle boiling phenomenon just to stop heating up, be incubated 30min；
(3) after intense reaction, then by remaining Isooctyl acrylate monomer 1687.5g, Isobutyl 2-propenoate 312.5g, propylene
The different methyl ester 187.5g of acid, hydroxyl ethyl ester 162.5g, glyceride 6.25g, acrylic acid 18.75g, ethyl acetate 2312.5g, toluene
562.5g, methanol 281.25g, benzoyl peroxide 3.75g, peroxidating Al13N 3.125g are added drop-wise to reactor as dropping liquid
In, time for adding is set in 60min, and simultaneous reactions kettle rotating speed is set to 60 revs/min to carry out being sufficiently stirred for reaction, anti-during Deca
The temperature control in kettle is answered at 94 ± 2 DEG C；
(4) reactor carries out insulation 90min after completion of dropwise addition, persistently stirs, until reaction kettle for reaction stops, glue surface is put down
Till steady；
(5) after reaction terminates, reactor stops stirring, and question response kettle is down to room temperature, and filtering and discharging gets product.
Preferably, the acrylate monomer in described step (1) is Isooctyl acrylate monomer, Isobutyl 2-propenoate, propylene
The different methyl ester of acid；Described organic solvent is ethyl acetate, three kinds of organic solvents of toluene and methanol；Described initiator is peroxidating
Benzoyl；
Preferably, the mixing in described step (1) is comprised the following steps：First by Isooctyl acrylate monomer 1687.5g, propylene
The different methyl ester 187.5g of sour isobutyl ester 312.5g, acrylic acid, hydroxyl ethyl ester 162.5g, glyceride 6.25g, acrylic acid 18.75g are added to
In reactor, the ethyl acetate of 2375g is subsequently added into；Again with toluene 562.5g, methanol 281.25g, by benzoyl peroxide
It is added in reactor after 3.75g dissolvings, is subsequently added into 250g ethyl acetates；Add peroxidating Al13N 3.125g, finally add
Enter and reaction is sufficiently stirred for after 2000g ethyl acetates；
Preferably, the reactor is sending out for the Application No. 201610439476.4 that applicant applies in 2016.06.20
Efficient glue reactor described in bright patent.
The novel acrylic ester glue items of formula and embodiment 1-3 of using method production are detected, number is detected
According to such as table 1 below, xanthochromia performance test conditions are：Temperature 70 C, humidity 95%R.H., uninterrupted 72 hours of constant temperature and humidity or 720
Hour：
The invention has the beneficial effects as follows：A kind of novel acrylic ester glue of the present invention, adds peroxidating in component
Al13N, with protection acrylate glue by the dioxygen oxidation in air, will not improve in use glue stability,
The combination properties such as heat conductivity, abrasion resistance, resistance to elevated temperatures and antiseptic property, it is ensured that the high-quality of glue；In preparation technology
In three times not commensurability different order is added ethyl acetate, and by reacting the raw material of 50% weight as bottom material input
Kettle, afterwards 50% after intense reaction Deca, in time for adding control 1h, whole response time 3h reaction terminates, and the response time is big
It is big to shorten, production efficiency is improve, preparation process is simple is adapted to large-scale industrial production.
It should be noted that above example is only to illustrate technical scheme and unrestricted.Although with reference to compared with
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the technology of invention
Scheme is modified or equivalent, and without deviating from the scope of technical solution of the present invention, it all should cover the power in the present invention
In sharp claimed range.
Claims (10)
1. a kind of novel acrylic ester glue, it is characterised in that its composition of raw materials includes the component of following weight portion：Acrylate
Monomer 150-200 parts, hydroxyl ethyl ester 10-15 part, glyceride 0.2-0.8 parts, acrylic acid 1-2 parts, organic solvent 220-285 parts, draw
Send out agent 0.2-0.4 parts, peroxidating Al13N 0.1-0.4 parts.
2. a kind of novel acrylic ester glue as claimed in claim 1, it is characterised in that described acrylate monomer includes
Following components：The different methyl ester of Isooctyl acrylate monomer, Isobutyl 2-propenoate, acrylic acid；Described organic solvent includes following components：Vinegar
Acetoacetic ester, toluene, methanol；Described initiator is benzoyl peroxide.
3. a kind of novel acrylic ester glue as claimed in claim 2, it is characterised in that the parts by weight of each component are third
It is the different monooctyl ester 120-150 parts of olefin(e) acid, Isobutyl 2-propenoate 20-30 parts, the different methyl ester 10-20 parts of acrylic acid, hydroxyl ethyl ester 10-15 part, sweet
Grease 0.2-0.8 parts, acrylic acid 1-2 parts, ethyl acetate 170-200 parts, toluene 35-55 parts, methanol 15-30 parts, benzoyl peroxide
Formyl 0.2-0.4 parts, peroxidating Al13N 0.1-0.4 parts.
4. a kind of novel acrylic ester glue as claimed in claim 3, it is characterised in that the parts by weight of each component are third
135 parts of the different monooctyl ester of olefin(e) acid, 25 parts of Isobutyl 2-propenoate, 15 parts of the different methyl ester of acrylic acid, 13 parts of hydroxyl ethyl ester, 0.5 part of glyceride, propylene
1.5 parts of acid, 185 parts of ethyl acetate, 45 parts of toluene, 22.5 parts of methanol, 0.3 part of benzoyl peroxide, peroxidating Al13N 0.25
Part.
5. a kind of preparation method of novel acrylic ester glue as claimed in claim 1, it is characterised in that including following technique
Step：
（1）By acrylate monomer, hydroxyl ethyl ester, glyceride, acrylic acid, organic solvent, initiator and peroxidating Al13N is fully mixed
After closing dilution several times, in being added to glue reactor, addition is 50%, carries out at the uniform velocity stirring reaction, and reactor rotating speed is 10
Rev/min；
（2）Heating mode is opened, repeatedly lasting slow heating heats up, and temperature rises to 94 ± 2 DEG C in reactor, until reactor
In occur boiling phenomenon just stop heat up, be incubated 15-30min；
（3）After intense reaction, then it is added drop-wise to remaining 50% as dropping liquid in reactor, time for adding is set in
45min-60min, simultaneous reactions kettle rotating speed is set to 60 revs/min to carry out being sufficiently stirred for reaction, the temperature during Deca in reactor
Degree control is at 94 ± 2 DEG C；
（4）After completion of dropwise addition reactor carry out be incubated 90min-120min reactors persistently stir, until reaction kettle for reaction is stopped
Only, glue surface is steady；
（5）After reaction terminates, reactor stops stirring, and question response kettle is down to room temperature, and filtering and discharging gets product.
6. a kind of preparation method of novel acrylic ester glue as claimed in claim 5, it is characterised in that the step（1）
Middle extension rate is 1-5 times.
7. a kind of preparation method of novel acrylic ester glue as claimed in claim 5, it is characterised in that described step
（1）In acrylate monomer be Isooctyl acrylate monomer, Isobutyl 2-propenoate, the different methyl ester of acrylic acid；Described organic solvent is
Ethyl acetate, three kinds of organic solvents of toluene and methanol；Described initiator is benzoyl peroxide.
8. a kind of preparation method of novel acrylic ester glue as claimed in claim 7, it is characterised in that described step
（1）In mixing comprise the following steps：First acrylate monomer, hydroxyl ethyl ester, glyceride, acrylic acid are added in reactor,
It is subsequently added into the ethyl acetate of a part；Again with toluene, formaldehyde is added in reactor after benzoyl peroxide is dissolved, then
Add the ethyl acetate of a part；Add peroxidating Al13N, is eventually adding after remaining ethyl acetate and is sufficiently stirred for reaction.
9. a kind of preparation method of novel acrylic ester glue as claimed in claim 8, it is characterised in that described acetic acid second
The ratio of weight and number of ester successively three additions is 95:10:80.
10. the preparation method of a kind of novel acrylic ester glue as described in claim 5-9 any one, it is characterised in that
The reactor is efficient glue reactor.
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| CN201610912415.5A CN106590475A (en) | 2016-10-20 | 2016-10-20 | Novel acrylic ester glue and preparation method thereof |
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| CN201610912415.5A CN106590475A (en) | 2016-10-20 | 2016-10-20 | Novel acrylic ester glue and preparation method thereof |
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| CN112680143A (en) * | 2020-12-21 | 2021-04-20 | 四川开物华包装材料有限公司 | Glue for Japanese paper adhesive tape and production process thereof |
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