CN107523242A - A kind of heat-conducting type polyacrylate pressure-sensitive and preparation method thereof - Google Patents
A kind of heat-conducting type polyacrylate pressure-sensitive and preparation method thereof Download PDFInfo
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- CN107523242A CN107523242A CN201710769910.XA CN201710769910A CN107523242A CN 107523242 A CN107523242 A CN 107523242A CN 201710769910 A CN201710769910 A CN 201710769910A CN 107523242 A CN107523242 A CN 107523242A
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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
- C09J143/00—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 containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Adhesives based on derivatives of such polymers
- C09J143/04—Homopolymers or copolymers of monomers containing silicon
-
- 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
-
- 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
-
- 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
- C09J11/08—Macromolecular additives
-
- 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
- C08F220/1812—C12-(meth)acrylate, e.g. lauryl (meth)acrylate
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
Abstract
The invention discloses a kind of heat-conducting type polyacrylate pressure-sensitive and preparation method thereof, the composition of wherein polyacrylate dispersion is：In terms of parts by weight：40 58 parts of lauryl acrylate, 50 70 parts of EMA, 24 36 parts of (3 methacryloxypropyl) trimethyl silane, 10 15 parts of N t-octyls acrylamide, 69 parts of N acryloyl morpholines, 68 parts of myristyl acid methyl esters α sodium sulfonates, 9 14 parts of Brij 35 carboxylic acid sodium, 30 50 parts of itaconic acid, 32 45 parts of acrylic acid.The pressure sensitive adhesive of the application has good heat conductivility, can rapidly by heat transfer, and the pressure sensitive adhesive initial cohesiveness of the application is good, hold viscosity energy it is strong and can be permanent retention property it is stable, asepsis environment-protecting, the scope of application is wider.
Description
Technical field
The present invention relates to textile auxiliary field, more particularly to a kind of heat-conducting type polyacrylate pressure-sensitive and its preparation side
Method.
Background technology
Pressure sensitive adhesive refers to that, to pressure-sensitive adhesive, only slight finger pressure need to be applied during use, without the aid of molten
The means such as agent, heating or illumination can be with firmly being binded by glutinous object, and stripping is not easily damaged, will not dry up in the long period
The characteristics of.Pressure sensitive adhesive majority is made into the pressure sensitive adhesive product application such as adhesive tape, glued membrane.Pressure sensitive adhesive product be widely used in automobile,
The fields such as packaging, construction material, electronic apparatus, daily necessities and health care, can play tie up, seal, insulating, protecting and
Various connection functions, its demand and the application such as fixed constantly expand.Polyacrylate pressure sensitive adhesive is pressure-sensitive
The most wide kind of yield maximum application in glue, polyacrylate have good weatherability, oil resistivity, water resistance and light resistance
The advantage such as excellent, and acrylic monomer also has a good chemism, the homopolymerization of acrylic monomer, copolymerization and and its
The copolyreaction of his monomer is all easier to carry out, and easily controllable reaction process.
Powerful function is integrated into less component by electronic equipment at present, is easily generated heat in the course of work, electricity
Sub- device temperature, which raises, can cause the equipment speed of service to slow down, and the easily first failure in device work midway, dimensional space limits and it
Performance issue in terms of him.Therefore, temperature control has become vital challenge in electronic device design engineering, be
In the case that operating space is less and less, how efficiently more heats to be distributed.In order that heat generating components to dissipate
The highly efficient transmission heat of thermal part, heat generating components and thermal component are fixed with Cheng Caiyong pressure sensitive adhesives.
It is pressure-sensitive that Chinese patent CN201110445746.x discloses a kind of high-temperature-resistant microwave oven door patch solvent-type acrylic
Adhesive, its formula include：Sticky monomer, interior polycondensation monomer, modified monomer, initiator and solvent, described sticky monomer are third
Olefin(e) acid butyl ester, described interior polycondensation monomer are methyl acrylate, described modified monomer is acrylic acid, described initiator is peroxide
Change benzoyl, described solvent are ethyl acetate, and the weight percent proportioning of each component is：Butyl acrylate 20~35%, propylene
Sour methyl esters 5~15%, acrylic acid 1~5%, benzoyl peroxide 0.15~0.35%, ethyl acetate 45~65%, its feature exist
In：Also include crosslinking agent in component, described crosslinking agent is melamine resin, and described melamine resin exists
Percentage by weight in component is 2.5~3.5%.The invention is reached by changing the formula of Acryloid-type pressure-sensitive adhesive
The requirement of 210 DEG C of heatproof is needed to micro-wave oven door patch.Although the pressure sensitive adhesive can keep stable under the high temperature conditions, it dissipates
Heat energy power still has to be strengthened.
The content of the invention
It is an object of the invention to provide a kind of heat-conducting type polyacrylate pressure-sensitive and preparation method thereof, the application's is pressure-sensitive
Glue has good heat conductivility, can be rapidly by heat transfer, and the pressure sensitive adhesive initial cohesiveness of the application is good, hold viscosity energy
Strong and can be permanent retention property is stable, asepsis environment-protecting, and the scope of application is wider.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, comprises the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, uncle N-
Octyl acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium according to
Secondary to be added to the water, after stirring 30-40min, by itaconic acid, acrylic acid is added thereto, and continues to stir 20-30min, it is single that mixing is made
Precursor emulsion；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition,
Hydroxyethyl cellulose is added, mercaptan, is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6-6.5, is heated to 90-95 DEG C,
The ammonium persulfate of half amount is added, reaction 40-50min is carried out under counterflow condition, it is single that remaining mixing is added dropwise thereto again afterwards
Precursor emulsion and remaining ammonium persulfate, after being added dropwise to complete, continue stirring reaction 90-120min, after reaction terminates, regulation pH is 7-
7.5, room temperature is down to, polyacrylate dispersion is made；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control temperature
For 40-50 DEG C, after ultrasonic disperse after 1-2h, Brij 35 carboxylic acid sodium is added dropwise, is entered using high-shear mixer
Row is dispersed with stirring 15-20min, and heat conduction particle dispersion liquid is made；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added obtained poly-
In acrylic acid ester emulsion, 50-60 DEG C is heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
Preferably, the usage amount of each component is in the step (1), in terms of parts by weight：Lauryl acrylate 40-58
Part, EMA 50-70 parts, (3- methacryloxypropyls) trimethyl silane 24-36 parts, N- t-octyl acryloyls
Amine 10-15 parts, N- acryloyl morpholine 6-9 parts, myristyl acid methyl esters α-sodium sulfonate 6-8 parts, Brij 35
Carboxylic acid sodium 9-14 parts, itaconic acid 30-50 parts, acrylic acid 32-45 parts.
Preferably, obtained mix monomer emulsion solid content is 38% in the step (1).
Preferably, the mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in the step (2):100.
Preferably, the mass ratio of the usage amount of hydroxyethyl cellulose and emulsion is 0.6 in the step (2):100, mercaptan
Usage amount and emulsion mass ratio be 0.4:100.
Preferably, the time for adding of remaining mix monomer emulsion and remaining ammonium persulfate is added dropwise in the step (2)
For 2-3h.
Preferably, the mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in the step (3), is received
The mass fraction of rice aluminum oxide is 15%.
Preferably, mixing speed when being stirred scattered using high-shear mixer in the step (3) is 10000-
15000r/min。
Preferably, the usage amount of each component is in the step (4), in terms of parts by weight：Polyacrylate dispersion 100
Part, heat conduction particle dispersion liquid 22-28 parts, polycarbodiimide 1-2 parts, antifreezing agent 2-3 parts, preservative 3-6 parts.
A kind of heat-conducting type polyacrylate pressure-sensitive, is prepared by above method.
The invention has the advantages that using (3- methacryloxypropyls) trimethyl silane to polyacrylate
It is modified, further improves the water resistance of obtained pressure sensitive adhesive, weatherability, improve making for prepared pressure sensitive adhesive
Use stability.It is copolymerized by adding N- t-octyls acrylamide and itaconic acid, improves obtained polyacrylate
Cross-linking properties so that prepared pressure sensitive adhesive has good initial cohesiveness.Utilize micron expanded graphite powder and nano aluminium oxide
It is used in conjunction with, the particle of two kinds of particle sizes can cooperate, and nano aluminium oxide can be very good to fill micron expanded graphite
Hole between particle contact, while the usage amount of nano-scale particle is reduced, preparation cost is reduced, and can ensure that pressure sensitive adhesive has
There is good heat-conducting effect.
Embodiment
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be formed to the present invention.
Embodiment 1
A kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, comprises the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, uncle N-
Octyl acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium according to
Secondary to be added to the water, after stirring 30-40min, by itaconic acid, acrylic acid is added thereto, and continues to stir 20-30min, it is single that mixing is made
Precursor emulsion, solid content 38%；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition,
Hydroxyethyl cellulose is added, mercaptan, is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6, is heated to 90 DEG C, adds half
The ammonium persulfate of amount, reaction 40min is carried out under counterflow condition, remaining mix monomer emulsion and residue is added dropwise thereto again afterwards
Ammonium persulfate, after being added dropwise to complete, continue stirring reaction 90min, after reaction terminates, regulation pH is 7, is down to room temperature, is made poly-
Acrylic acid ester emulsion；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control temperature
For 40 DEG C, after ultrasonic disperse after 1h, Brij 35 carboxylic acid sodium is added dropwise, is stirred using high-shear mixer
Scattered 15min, is made heat conduction particle dispersion liquid；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added obtained poly-
In acrylic acid ester emulsion, 50 DEG C are heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
The usage amount of each component is in the step (1), in terms of parts by weight：40 parts of lauryl acrylate, metering system
50 parts of acetoacetic ester, 24 parts of (3- methacryloxypropyls) trimethyl silane, 10 parts of N- t-octyls acrylamide, N- acryloyls
6 parts of quinoline, myristyl acid methyl esters α -6 parts of sodium sulfonate, 9 parts of Brij 35 carboxylic acid sodium, 30 parts of itaconic acid, propylene
32 parts of acid.
The mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in the step (2):100；Hydroxyethyl cellulose
The mass ratio of usage amount and emulsion is 0.6:100, the usage amount of mercaptan and the mass ratio of emulsion are 0.4:100；It is added dropwise remaining
The time for adding of mix monomer emulsion and remaining ammonium persulfate is 2h.
The mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in the step (3), nano oxidized
The mass fraction of aluminium is 15%；Mixing speed when being stirred scattered using high-shear mixer is 10000r/min.
The usage amount of each component is in the step (4), in terms of parts by weight：100 parts of polyacrylate dispersion, heat conduction
22 parts of dispersion liquid of grain, 1 part of polycarbodiimide, 2 parts of antifreezing agent, 3 parts of preservative.
Embodiment 2
A kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, comprises the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, uncle N-
Octyl acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium according to
Secondary to be added to the water, after stirring 40min, by itaconic acid, acrylic acid is added thereto, and continues to stir 30min, and mix monomer breast is made
Liquid, solid content 38%；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition,
Hydroxyethyl cellulose is added, mercaptan, is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6.5, is heated to 95 DEG C, adds one
The ammonium persulfate of half amount, reaction 50min is carried out under counterflow condition, remaining mix monomer emulsion and surplus is added dropwise thereto again afterwards
Remaining ammonium persulfate, after being added dropwise to complete, continue stirring reaction 120min, after reaction terminates, regulation pH is 7.5, is down to room temperature, is made
Obtain polyacrylate dispersion；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control temperature
For 50 DEG C, after ultrasonic disperse after 2h, Brij 35 carboxylic acid sodium is added dropwise, is stirred using high-shear mixer
Scattered 20min, is made heat conduction particle dispersion liquid；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added obtained poly-
In acrylic acid ester emulsion, 60 DEG C are heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
The usage amount of each component is in the step (1), in terms of parts by weight：58 parts of lauryl acrylate, metering system
70 parts of acetoacetic ester, 36 parts of (3- methacryloxypropyls) trimethyl silane, 15 parts of N- t-octyls acrylamide, N- acryloyls
9 parts of quinoline, myristyl acid methyl esters α -8 parts of sodium sulfonate, 14 parts of Brij 35 carboxylic acid sodium, 50 parts of itaconic acid, third
45 parts of olefin(e) acid.
The mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in the step (2):100；Hydroxyethyl cellulose
The mass ratio of usage amount and emulsion is 0.6:100, the usage amount of mercaptan and the mass ratio of emulsion are 0.4:100；It is added dropwise remaining
The time for adding of mix monomer emulsion and remaining ammonium persulfate is 2-3h.
The mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in the step (3), nano oxidized
The mass fraction of aluminium is 15%；Mixing speed when being stirred scattered using high-shear mixer is 15000r/min.It is described
The usage amount of each component is in step (4), in terms of parts by weight：100 parts of polyacrylate dispersion, heat conduction particle dispersion liquid 28
Part, 2 parts of polycarbodiimide, 3 parts of antifreezing agent, 6 parts of preservative.
Embodiment 3
A kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, comprises the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, uncle N-
Octyl acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium according to
Secondary to be added to the water, after stirring 30min, by itaconic acid, acrylic acid is added thereto, and continues to stir 30min, and mix monomer breast is made
Liquid, solid content 38%；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition,
Hydroxyethyl cellulose is added, mercaptan, is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6, is heated to 95 DEG C, adds half
The ammonium persulfate of amount, reaction 40min is carried out under counterflow condition, remaining mix monomer emulsion and residue is added dropwise thereto again afterwards
Ammonium persulfate, after being added dropwise to complete, continue stirring reaction 120min, after reaction terminates, regulation pH is 7, is down to room temperature, is made poly-
Acrylic acid ester emulsion；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control temperature
For 50 DEG C, after ultrasonic disperse after 1h, Brij 35 carboxylic acid sodium is added dropwise, is stirred using high-shear mixer
Scattered 20min, is made heat conduction particle dispersion liquid；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added obtained poly-
In acrylic acid ester emulsion, 50 DEG C are heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
The usage amount of each component is in the step (1), in terms of parts by weight：58 parts of lauryl acrylate, metering system
50 parts of acetoacetic ester, 36 parts of (3- methacryloxypropyls) trimethyl silane, 10 parts of N- t-octyls acrylamide, N- acryloyls
9 parts of quinoline, myristyl acid methyl esters α -6 parts of sodium sulfonate, 14 parts of Brij 35 carboxylic acid sodium, 30 parts of itaconic acid, third
45 parts of olefin(e) acid.
The mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in the step (2):100；Hydroxyethyl cellulose
The mass ratio of usage amount and emulsion is 0.6:100, the usage amount of mercaptan and the mass ratio of emulsion are 0.4:100；It is added dropwise remaining
The time for adding of mix monomer emulsion and remaining ammonium persulfate is 2h.
The mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in the step (3), nano oxidized
The mass fraction of aluminium is 15%；Mixing speed when being stirred scattered using high-shear mixer is 15000r/min.
The usage amount of each component is in the step (4), in terms of parts by weight：100 parts of polyacrylate dispersion, heat conduction
22 parts of dispersion liquid of grain, 2 parts of polycarbodiimide, 2 parts of antifreezing agent, 6 parts of preservative.
Embodiment 4
A kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, comprises the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, uncle N-
Octyl acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium according to
Secondary to be added to the water, after stirring 40min, by itaconic acid, acrylic acid is added thereto, and continues to stir 20min, and mix monomer breast is made
Liquid, solid content 38%；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition,
Hydroxyethyl cellulose is added, mercaptan, is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6.5, is heated to 90 DEG C, adds one
The ammonium persulfate of half amount, reaction 50min is carried out under counterflow condition, remaining mix monomer emulsion and surplus is added dropwise thereto again afterwards
Remaining ammonium persulfate, after being added dropwise to complete, continue stirring reaction 90min, after reaction terminates, regulation pH is 7.5, is down to room temperature, is made
Obtain polyacrylate dispersion；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control temperature
For 4 DEG C, after ultrasonic disperse after 2h, Brij 35 carboxylic acid sodium is added dropwise, is stirred using high-shear mixer
Scattered 15min, is made heat conduction particle dispersion liquid；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added obtained poly-
In acrylic acid ester emulsion, 60 DEG C are heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
The usage amount of each component is in the step (1), in terms of parts by weight：40 parts of lauryl acrylate, metering system
70 parts of acetoacetic ester, 24 parts of (3- methacryloxypropyls) trimethyl silane, 15 parts of N- t-octyls acrylamide, N- acryloyls
6 parts of quinoline, myristyl acid methyl esters α -8 parts of sodium sulfonate, 9 parts of Brij 35 carboxylic acid sodium, 50 parts of itaconic acid, propylene
32 parts of acid.
The mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in the step (2):100；Hydroxyethyl cellulose
The mass ratio of usage amount and emulsion is 0.6:100, the usage amount of mercaptan and the mass ratio of emulsion are 0.4:100；It is added dropwise remaining
The time for adding of mix monomer emulsion and remaining ammonium persulfate is 3h.
The mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in the step (3), nano oxidized
The mass fraction of aluminium is 15%；Mixing speed when being stirred scattered using high-shear mixer is 10000r/min.
The usage amount of each component is in the step (4), in terms of parts by weight：100 parts of polyacrylate dispersion, heat conduction
28 parts of dispersion liquid of grain, 1 part of polycarbodiimide, 3 parts of antifreezing agent, 3 parts of preservative.
Embodiment 5
A kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, comprises the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, uncle N-
Octyl acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium according to
Secondary to be added to the water, after stirring 35min, by itaconic acid, acrylic acid is added thereto, and continues to stir 25min, and mix monomer breast is made
Liquid, solid content 38%；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition,
Hydroxyethyl cellulose is added, mercaptan, is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6, is heated to 90 DEG C, adds half
The ammonium persulfate of amount, reaction 45min is carried out under counterflow condition, remaining mix monomer emulsion and residue is added dropwise thereto again afterwards
Ammonium persulfate, after being added dropwise to complete, continue stirring reaction 100min, after reaction terminates, regulation pH is 7, is down to room temperature, is made poly-
Acrylic acid ester emulsion；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control temperature
For 40 DEG C, after ultrasonic disperse after 1h, Brij 35 carboxylic acid sodium is added dropwise, is stirred using high-shear mixer
Scattered 20min, is made heat conduction particle dispersion liquid；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added obtained poly-
In acrylic acid ester emulsion, 50 DEG C are heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
The usage amount of each component is in the step (1), in terms of parts by weight：44 parts of lauryl acrylate, metering system
55 parts of acetoacetic ester, 28 parts of (3- methacryloxypropyls) trimethyl silane, 12 parts of N- t-octyls acrylamide, N- acryloyls
7 parts of quinoline, myristyl acid methyl esters α -7 parts of sodium sulfonate, 11 parts of Brij 35 carboxylic acid sodium, 33 parts of itaconic acid, third
37 parts of olefin(e) acid.
The mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in the step (2):100；Hydroxyethyl cellulose
The mass ratio of usage amount and emulsion is 0.6:100, the usage amount of mercaptan and the mass ratio of emulsion are 0.4:100；It is added dropwise remaining
The time for adding of mix monomer emulsion and remaining ammonium persulfate is 2h.
The mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in the step (3), nano oxidized
The mass fraction of aluminium is 15%；Mixing speed when being stirred scattered using high-shear mixer is 15000r/min.
The usage amount of each component is in the step (4), in terms of parts by weight：100 parts of polyacrylate dispersion, heat conduction
26 parts of dispersion liquid of grain, 2 parts of polycarbodiimide, 2 parts of antifreezing agent, 4 parts of preservative.
Embodiment 6
A kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, comprises the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, uncle N-
Octyl acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium according to
Secondary to be added to the water, after stirring 30min, by itaconic acid, acrylic acid is added thereto, and continues to stir 30min, and mix monomer breast is made
Liquid, solid content 38%；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition,
Hydroxyethyl cellulose is added, mercaptan, is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6.5, is heated to 95 DEG C, adds one
The ammonium persulfate of half amount, reaction 40min is carried out under counterflow condition, remaining mix monomer emulsion and surplus is added dropwise thereto again afterwards
Remaining ammonium persulfate, after being added dropwise to complete, continue stirring reaction 90min, after reaction terminates, regulation pH is 7.5, is down to room temperature, is made
Obtain polyacrylate dispersion；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control temperature
For 40 DEG C, after ultrasonic disperse after 1h, Brij 35 carboxylic acid sodium is added dropwise, is stirred using high-shear mixer
Scattered 20min, is made heat conduction particle dispersion liquid；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added obtained poly-
In acrylic acid ester emulsion, 60 DEG C are heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
The usage amount of each component is in the step (1), in terms of parts by weight：56 parts of lauryl acrylate, metering system
65 parts of acetoacetic ester, 33 parts of (3- methacryloxypropyls) trimethyl silane, 13 parts of N- t-octyls acrylamide, N- acryloyls
8 parts of quinoline, myristyl acid methyl esters α -7 parts of sodium sulfonate, 12 parts of Brij 35 carboxylic acid sodium, 42 parts of itaconic acid, third
41 parts of olefin(e) acid.
The mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in the step (2):100；Hydroxyethyl cellulose
The mass ratio of usage amount and emulsion is 0.6:100, the usage amount of mercaptan and the mass ratio of emulsion are 0.4:100；It is added dropwise remaining
The time for adding of mix monomer emulsion and remaining ammonium persulfate is 3h.
The mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in the step (3), nano oxidized
The mass fraction of aluminium is 15%；Mixing speed when being stirred scattered using high-shear mixer is 12000r/min.
The usage amount of each component is in the step (4), in terms of parts by weight：100 parts of polyacrylate dispersion, heat conduction
24 parts of dispersion liquid of grain, 1 part of polycarbodiimide, 3 parts of antifreezing agent, 5 parts of preservative.
The heat conductivility of the embodiment 1-6 heat-conducting type polyacrylate pressure-sensitives prepared and comparative example is tested, tied
Fruit is as in the table below：
Thermal conductivity tests the thermal conductivity factor of measured material by heat flow method conductometer, and thermal conductivity factor is higher to show thermal conductivity more
It is good.
Comparative example is commercially available heat-conducting type polyacrylate pressure-sensitive.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example | |
| Thermal conductivity factor (W/mk) | 2.47 | 2.42 | 2.62 | 2.59 | 2.38 | 2.32 | 1.3 |
Claims (10)
1. a kind of preparation method of heat-conducting type polyacrylate pressure-sensitive, it is characterised in that comprise the following steps：
(1) by lauryl acrylate, EMA, (3- methacryloxypropyls) trimethyl silane, N- t-octyls
Acrylamide, N- acryloyl morpholines, myristyl acid methyl esters α-sodium sulfonate, Brij 35 carboxylic acid sodium add successively
Enter in water, after stirring 30-40min, by itaconic acid, acrylic acid is added thereto, and continues to stir 20-30min, and mix monomer breast is made
Liquid；
(2) take the mix monomer emulsion of half amount to add in reactor, be passed through nitrogen into reactor, under stirring condition, add
Hydroxyethyl cellulose, mercaptan, it is well mixed, adds ammoniacal liquor afterwards, regulation pH is 6-6.5, is heated to 90-95 DEG C, is added
The ammonium persulfate of half amount, reaction 40-50min is carried out under counterflow condition, remaining mix monomer breast is added dropwise thereto again afterwards
Liquid and remaining ammonium persulfate, after being added dropwise to complete, continuing stirring reaction 90-120min, after reaction terminates, regulation pH is 7-7.5,
Room temperature is down to, polyacrylate dispersion is made；
(3) micron expanded graphite powder and nano aluminium oxide are scattered in the aqueous solution of Polyethylene glycol-2000, control the temperature to be
40-50 DEG C, after ultrasonic disperse after 1-2h, Brij 35 carboxylic acid sodium is added dropwise, is carried out using high-shear mixer
15-20min is dispersed with stirring, heat conduction particle dispersion liquid is made；
(4) obtained heat conduction particle dispersion liquid, polycarbodiimide, antifreezing agent, preservative are sequentially added into obtained polypropylene
In acid esters emulsion, 50-60 DEG C is heated to, is uniformly mixed and produces the heat-conducting type polyacrylate pressure-sensitive.
2. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(1) usage amount of each component is in, in terms of parts by weight：Lauryl acrylate 40-58 parts, EMA 50-70 parts,
(3- methacryloxypropyls) trimethyl silane 24-36 parts, N- t-octyl acrylamide 10-15 parts, N- acryloyl morpholines 6-9
Part, myristyl acid methyl esters α-sodium sulfonate 6-8 parts, Brij 35 carboxylic acid sodium 9-14 parts, itaconic acid 30-50
Part, acrylic acid 32-45 parts.
3. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(1) obtained mix monomer emulsion solid content is 38% in.
4. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(2) mass ratio of the usage amount of ammonium persulfate and emulsion is 0.24 in:100.
5. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(2) mass ratio of the usage amount of hydroxyethyl cellulose and emulsion is 0.6 in:100, the usage amount of mercaptan and the mass ratio of emulsion are
0.4:100。
6. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(2) it is 2-3h that remaining mix monomer emulsion and the time for adding of remaining ammonium persulfate are added dropwise in.
7. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(3) mass fraction of micron expanded graphite powder is 22% in heat conduction particle dispersion liquid in, and the mass fraction of nano aluminium oxide is
15%.
8. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(3) mixing speed when being stirred scattered using high-shear mixer in is 10000-15000r/min.
9. the preparation method of heat-conducting type polyacrylate pressure-sensitive according to claim 1, it is characterised in that：The step
(4) usage amount of each component is in, in terms of parts by weight：100 parts of polyacrylate dispersion, heat conduction particle dispersion liquid 22-28 parts,
Polycarbodiimide 1-2 parts, antifreezing agent 2-3 parts, preservative 3-6 parts.
A kind of 10. heat-conducting type polyacrylate pressure-sensitive, it is characterised in that：As the method system described in claim any one of 1-9
It is standby to form.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527453A (en) * | 2019-09-10 | 2019-12-03 | 皇冠（太仓）胶粘制品有限公司 | The bonding sheet based on acrylic acid series copolymer for 5G antenna processing procedure |
| CN115521726A (en) * | 2022-10-21 | 2022-12-27 | 广东顶峰精密技术有限公司 | Graphite flake heat dissipation sticker and production process thereof |
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| CN102816536A (en) * | 2011-06-08 | 2012-12-12 | 苏州达同新材料有限公司 | Adhesive tape used for solar cell assembly and preparation method thereof |
| CN103073671A (en) * | 2013-01-08 | 2013-05-01 | 大连工业大学 | Adhesive emulsion for diatomite wallpaper |
| CN105950076A (en) * | 2016-04-01 | 2016-09-21 | 合肥第六元素光电科技有限公司 | Flexible thermally-conductive adhesive designed based on multi-dimension multi-scale microstructure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102816536A (en) * | 2011-06-08 | 2012-12-12 | 苏州达同新材料有限公司 | Adhesive tape used for solar cell assembly and preparation method thereof |
| CN103073671A (en) * | 2013-01-08 | 2013-05-01 | 大连工业大学 | Adhesive emulsion for diatomite wallpaper |
| CN105950076A (en) * | 2016-04-01 | 2016-09-21 | 合肥第六元素光电科技有限公司 | Flexible thermally-conductive adhesive designed based on multi-dimension multi-scale microstructure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110527453A (en) * | 2019-09-10 | 2019-12-03 | 皇冠（太仓）胶粘制品有限公司 | The bonding sheet based on acrylic acid series copolymer for 5G antenna processing procedure |
| CN115521726A (en) * | 2022-10-21 | 2022-12-27 | 广东顶峰精密技术有限公司 | Graphite flake heat dissipation sticker and production process thereof |
| CN115521726B (en) * | 2022-10-21 | 2023-07-14 | 广东顶峰精密技术有限公司 | Graphite flake heat dissipation paste and production process thereof |
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