CN104004477B - A kind of room-temperature self crosslinking polyacrylate pressure-sensitive and preparation method thereof and application - Google Patents

A kind of room-temperature self crosslinking polyacrylate pressure-sensitive and preparation method thereof and application Download PDF

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CN104004477B
CN104004477B CN201410223068.6A CN201410223068A CN104004477B CN 104004477 B CN104004477 B CN 104004477B CN 201410223068 A CN201410223068 A CN 201410223068A CN 104004477 B CN104004477 B CN 104004477B
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temperature self
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CN104004477A (en
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涂伟萍
陈任
王�锋
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South China University of Technology SCUT
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Abstract

The invention belongs to room-temperature self crosslinking Material Field, disclose a kind of room-temperature self crosslinking polyacrylate pressure-sensitive and preparation method thereof and application.In massfraction, by acrylate soft monomer 85 ~ 95 parts, hard monomer 5 ~ 15 parts, function monomer 2 ~ 5 parts, emulsifying agent 1.3 ~ 4 parts and deionized water 30 ~ 55 parts are prepared into pre-emulsion, then by pre-emulsion and deionized water, initiator, emulsifying agent, the heat temperature raising reaction together of PH buffer reagent, occur after blue light until emulsion, drip chain-transfer agent, pre-emulsion and initiator solution, add the temperature reaction together of ketocarbonyl-containing monomer again, rear cooling adjust ph to 6.5 ~ 7.0 are reacted, then add hydrazide group monomer to be uniformly mixed, obtain room-temperature self crosslinking polyacrylate pressure-sensitive.Gained room-temperature self crosslinking polyacrylate pressure-sensitive at first viscous force, hold and viscous force and stripping strength index all can reach excellent, can be used for preparing the excellent label of bond performance.

Description

A kind of room-temperature self crosslinking polyacrylate pressure-sensitive and preparation method thereof and application
Technical field
The invention belongs to room-temperature self crosslinking Material Field, be specifically related to a kind of room-temperature self crosslinking polyacrylate pressure-sensitive and preparation method thereof and application.
Background technology
Pressure sensitive adhesive is a kind of viscoelastic body simultaneously possessing Liquid Viscous character and solid elastic character, and this viscoelastic body possesses simultaneously " can bear influence factor and the character of bonding contact process and destructive process two aspect ".Popular, be exactly easily sticky glutinous, be not difficult to open, without any the phenomenon polluting adherend surface after stripping, because glue-line is not done for a long time, be also referred to as " non-setting adhesive ".
The polyacrylate pressure-sensitive of label, many or use solvent-based adhesive that is inflammable, poisonous, contaminate environment at home at present.Solvent-based adhesive not only causes the wasting of resources, causes disadvantageous effect to the health of workmen, and serious environment pollution.
It is slow generally to there is surface covered in emulsion-type polyacrylate pressure-sensitive, and rate of drying is slow, first viscous force, stripping strength and hold viscous force three mechanical properties and cannot obtain a lot of balances.Viscous force >=10 (steel ball number) at the beginning of according to the basic demand of HG-T2406-2002 to trademark adhesive being, stripping strength is >=4N/25mm, but this requires the application market that can not meet normal trademark adhesive far away, and therefore exploration can better seem particularly important by pressure sensitive adhesive.
Summary of the invention
In order to solve the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is the preparation method providing a kind of room-temperature self crosslinking polyacrylate pressure-sensitive.
Another object of the present invention is to provide a kind of room-temperature self crosslinking polyacrylate pressure-sensitive prepared by above-mentioned preparation method.
Another object of the present invention is to provide the application of above-mentioned room-temperature self crosslinking polyacrylate pressure-sensitive in forming label.
The object of the invention is achieved through the following technical solutions:
A preparation method for room-temperature self crosslinking polyacrylate pressure-sensitive, concrete operation step is as follows:
(1) in mass parts, by acrylate soft monomer 85 ~ 95 parts, hard monomer 5 ~ 15 parts, function monomer 2 ~ 5 parts, emulsifying agent 1.3 ~ 4 parts, deionized water 30 ~ 55 parts, stirs after mixing and is prepared into pre-emulsion;
(2) 0.1 ~ 0.3 mass parts initiator is dissolved in the deionized water of 4 ~ 6 mass parts, is mixed with initiator solution;
(3) in a kettle., in mass parts, add 35 ~ 50 parts of deionized waters, 0.15 ~ 0.25 part of initiator, 0.3 ~ 0.8 part of emulsifying agent and 0.3 ~ 0.5 part of pH buffer reagent, stir, then pre-emulsion 13 ~ 15 parts obtained by step (1) and the obtained initiator solution 0.5 ~ 1.0 part of step (2) is added under agitation, be warming up to 83 ~ 86 DEG C, occur after blue light until emulsion, 0.1 ~ 0.3 part of chain-transfer agent is dripped again in reactor, 88.04 ~ 127.2 parts of pre-emulsions and 2.88 ~ 4.24 parts of initiator solutions, continuous dropping 2h, again the solution that ketocarbonyl-containing monomer 0.5 ~ 2 part is dissolved in 2 ~ 5 parts of deionized waters is dripped together with 22.06 ~ 31.8 parts of pre-emulsions, after 0.5 ~ 1h drips continuously, add 0.72 ~ 1.06 part of initiator solution again, be warmed up to 86 ~ 90 DEG C and be incubated 1 ~ 1.5h, cool the temperature to less than 40 DEG C again, adjust ph to 6.5 ~ 7.0,
(4) hydrazide group monomer 0.4 ~ 1.6 mass parts is dissolved in 2 ~ 5 mass parts deionized waters, be made into hydrazide group monomer solution, then joined in the reactor of step (3), be uniformly mixed, obtained room-temperature self crosslinking polyacrylate pressure-sensitive.
Acrylate soft monomer described in step (1) is the mixture of at least one in ethyl propenoate, butyl acrylate and Isooctyl acrylate monomer, and wherein Isooctyl acrylate monomer accounts for 55% ~ 85% of acrylate soft monomer total mass.
Hard monomer described in step (1) is the mixture of any one and methyl methacrylate in vinyl acetate between to for plastic, tertiary ethylene carbonate, and wherein methyl methacrylate accounts for 70% ~ 85% of hard monomer total mass.
Function monomer described in step (1) is the mixture of at least one in Hydroxyethyl acrylate, Propylene glycol monoacrylate, glycidyl acrylate and propyloic acrylic ester.
Described in step (1) or step (3), emulsifying agent is anionic emulsifier or reactive emulsifier, wherein anionic emulsifier preferably sodium dodecyl sulfate, the preferred allyloxy hydroxypropyl azochlorosulfonate acid sodium of reactive emulsifier.
Described in step (2) or step (3), initiator is ammonium persulphate or Potassium Persulphate.
The preferred sodium bicarbonate of pH buffer reagent described in step (3); The preferred lauryl mercaptan of described chain-transfer agent or mercaptoethanol; The preferred diacetone-acryloamide(DAA) of described ketocarbonyl-containing monomer.
Agitation condition described in step (3) refers to that mixing speed is the agitation condition of 200 ~ 250r/min.
Hydrazide group monomer described in step (4) is any one in carbon acid dihydrazide, careless acid dihydrazide, succinic acid hydrazide ii, adipic dihydrazide.
A kind of room-temperature self crosslinking polyacrylate pressure-sensitive, obtains prepared by above-mentioned preparation method.Gained room-temperature self crosslinking polyacrylate pressure-sensitive at first viscous force, hold and viscous force and stripping strength index all can reach excellent.
The application of above-mentioned room-temperature self crosslinking polyacrylate pressure-sensitive in forming label, embody rule process is: be coated on by pressure sensitive adhesive prepared by the present invention on the separate paper crossed through corona treatment rapidly and uniformly with line rod spreader, the baking oven this separate paper being put into 105 DEG C subsequently dries 2min, take out after drying, the glue one side that has ivory board being attached to separate paper obtains label paper, be cut to standard specimen 250mm*25mm again, obtain the label that bond performance is excellent.
The present invention is by the kind of adjustment monomer, introduce the functional monomer propyloic acrylic ester that some are special, stripping strength is improved because its longer side carboxylic acid chain gives good flexibility, simultaneously longer alkyl chain can the surface tension of lower emulsion, interleaving paper has fabulous extravagant performance, and overcoming prior art needs to add " shank print " and dispersed " wandering away " phenomenon that the auxiliary agents such as micromolecular wetting agent occur on interleaving paper to solve emulsion.
The present invention uses the ketone hydrazine cross-linking system in carbonyl type cross-linking monomer, compared with the N substituted acrylamide derivative type cross-linking monomer comparatively commonly used with prior art, overcome the shortcoming of its hot setting, release formaldehyde, pressure sensitive adhesive can be made to have environmental protection concurrently in self-vulcanizing.
The present invention adopts chain-transfer agent and cross-linking monomer simultaneously, and the molecular weight distribution of emulsion can be made wider, at first viscous force, holds in viscous force and stripping strength etc. and all reaches higher performance.
Had the following advantages and beneficial effect by preparation method of the present invention and the product tool that obtains:
(1) the present invention adopts emulsion polymerisation process and specific reaction process, compares with other polymerization processs and technique, has reaction viscosity low, the advantage of the fast and Environmental Safety of speed of reaction;
(2) polymerization process of the present invention is stablized, and workable, facility investment is little, is conducive to large-scale industrial production;
(3) pressure sensitive adhesive obtained by Method and process of the present invention, have good first viscous force and hold viscous force, have higher stripping strength, bond performance is excellent simultaneously.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Described in embodiment, indication test method is as follows:
Tack: test by GB4852-84; Hold viscosity: test by DB4851-98; Stripping strength: test by GB2792-98.
Embodiment 1
(1) by ethyl propenoate 21.25g, butyl acrylate 17.0g, Isooctyl acrylate monomer 46.75g, methyl methacrylate 3.5g, vinyl acetate between to for plastic 1g, tertiary ethylene carbonate 0.5g, propyloic acrylic ester 1g, Hydroxyethyl acrylate 0.2g, Propylene glycol monoacrylate 0.3g, glycidyl acrylate 0.5g, sodium lauryl sulphate 1.3g, deionized water 30g, stirs and is prepared into pre-emulsion;
(2) 0.1g ammonium persulphate is dissolved in 4g deionized water, is mixed with initiator solution;
(3) in a kettle., add deionized water 35g, ammonium persulphate 0.15g, allyloxy hydroxypropyl azochlorosulfonate acid sodium 0.3g and sodium bicarbonate 0.3g, stirs, low whipping speed is add the pre-emulsion 13g in step (1) and the initiator solution 0.5g in step (2) in the condition downhill reaction still of 200r/min, be warming up to 83 DEG C, occur after blue light until emulsion, lauryl mercaptan 0.1g is dripped continuously again in reactor, 88.24g pre-emulsion and 2.88g initiator solution, after continuous dropping 2h, the solution again 2g diacetone-acryloamide(DAA) being dissolved in 5g deionized water drips together with 22.06g pre-emulsion, after 0.5h drips continuously, add 0.72g initiator solution again, be warmed up to 86 DEG C, after insulation 1h, cool the temperature to less than 40 DEG C again, adjust ph to 6.5 ~ 7.0,
(4) 0.4g grass acid dihydrazide is dissolved in 2g deionized water, is made into hydrazide group monomer solution, joins in the reactor material of step (3), stir, obtain room-temperature self crosslinking polyacrylate pressure-sensitive.
Rapidly and uniformly room-temperature self crosslinking polyacrylate pressure-sensitive obtained above is coated on line rod spreader on the separate paper crossed through corona treatment, the baking oven separate paper of gluing being put into 105 DEG C subsequently dries 2min, take out after drying, the glue one side that has ivory board being attached to separate paper obtains label paper, be cut to standard specimen 250mm*25mm again, standard specimen carries out tack after putting into the thermostatic chamber 4h of 23 ± 2 DEG C, holds the test of viscosity and stripping strength, and test result is in table 1.
Embodiment 2
(1) by ethyl propenoate 4.25g, butyl acrylate 10.0g, Isooctyl acrylate monomer 80.75g, methyl methacrylate 12.75g, vinyl acetate between to for plastic 1.75g, tertiary ethylene carbonate 0.5g, propyloic acrylic ester 2.5g, Hydroxyethyl acrylate 0.5g, Propylene glycol monoacrylate 1g, glycidyl acrylate 1g, sodium lauryl sulphate 4g, deionized water 55g, stirs and is prepared into pre-emulsion;
(2) 0.3g ammonium persulphate is dissolved in 6g deionized water, is mixed with initiator solution;
(3) in a kettle., add deionized water 50g, ammonium persulphate 0.25g, allyloxy hydroxypropyl azochlorosulfonate acid sodium 0.8g and sodium bicarbonate 0.5g, stirs, low whipping speed is add the pre-emulsion 15g in step (1) and the initiator solution 1g in step (2) in the condition downhill reaction still of 250r/min, be warming up to 86 DEG C, occur after blue light until emulsion, mercaptoethanol 0.3g is dripped continuously again in reactor, 127.2g pre-emulsion and 4.24g initiator solution, after continuous dropping 2h, the solution again 2g diacetone-acryloamide(DAA) being dissolved in 5g deionized water drips together with 24.5g pre-emulsion, after 1h drips continuously, add 1.06g initiator solution again, be warmed up to 90 DEG C, after insulation 1h, cool the temperature to less than 40 DEG C again, adjust ph to 6.5 ~ 7.0,
(4) 1.6g succinic acid hydrazide ii is dissolved in 5g deionized water, is made into hydrazide group monomer solution, join in the reactor material of step (3), stir, obtain room-temperature self crosslinking polyacrylate pressure-sensitive.
Rapidly and uniformly room-temperature self crosslinking polyacrylate pressure-sensitive obtained above is coated on line rod spreader on the separate paper crossed through corona treatment, the baking oven separate paper of gluing being put into 105 DEG C subsequently dries 2min, take out after drying, the glue one side that has ivory board being attached to separate paper obtains label paper, be cut to standard specimen 250mm*25mm again, standard specimen carries out tack after putting into the thermostatic chamber 4h of 23 ± 2 DEG C, holds the test of viscosity and stripping strength, and test result is in table 1.
Embodiment 3
(1) by butyl acrylate 14.25.0g, Isooctyl acrylate monomer 80.75g, methyl methacrylate 3.5g, vinyl acetate between to for plastic 1g, tertiary ethylene carbonate 0.5g, propyloic acrylic ester 2g, Propylene glycol monoacrylate 1.5g, glycidyl acrylate 0.5g, sodium lauryl sulphate 1.5g, deionized water 50g, stirs and is prepared into pre-emulsion;
(2) 0.2g ammonium persulphate is dissolved in 5g deionized water, is mixed with initiator solution;
(3) in a kettle., add deionized water 40g, ammonium persulphate 0.25g, allyloxy hydroxypropyl azochlorosulfonate acid sodium 0.3g and sodium bicarbonate 0.5g, stirs, low whipping speed is add the pre-emulsion 15g in step (1) and the initiator solution 0.5g in step (2) in the condition downhill reaction still of 200r/min, be warming up to 84 DEG C, occur after blue light until emulsion, lauryl mercaptan 0.2g is dripped continuously again in reactor, 112.4g pre-emulsion and 3.76g initiator solution, after continuous dropping 2h, the solution again 0.5g diacetone-acryloamide(DAA) being dissolved in 2g deionized water drips together with 28.1g pre-emulsion, after 0.5h drips continuously, add 0.94 initiator solution again, be warmed up to 87 DEG C, after insulation 1h, cool the temperature to less than 40 DEG C again, adjust ph to 6.5 ~ 7.0,
(4) 0.4g adipic acid dihydrazide is dissolved in 4g deionized water, is made into hydrazide group monomer solution, join in the reactor material of step (3), stir, obtain room-temperature self crosslinking polyacrylate pressure-sensitive.
Rapidly and uniformly room-temperature self crosslinking polyacrylate pressure-sensitive obtained above is coated on line rod spreader on the separate paper crossed through corona treatment, the baking oven separate paper of gluing being put into 105 DEG C subsequently dries 2min, take out after drying, the glue one side that has ivory board being attached to separate paper obtains label paper, be cut to standard specimen 250mm*25mm again, standard specimen carries out tack after putting into the thermostatic chamber 4h of 23 ± 2 DEG C, holds the test of viscosity and stripping strength, and test result is in table 1.
Table 1 embodiment properties of sample test result
First viscous force (steel ball number) Hold viscous force (h) 180 ° of stripping strengths (N/25mm)
Embodiment 1 17 >24 11.37, not haftplatte
Embodiment 2 15 >48 10.42, not haftplatte
Embodiment 3 15.5 >24 12.40, not haftplatte
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (7)

1. a preparation method for room-temperature self crosslinking polyacrylate pressure-sensitive, is characterized in that: comprise following operation steps:
(1) in mass parts, by acrylate soft monomer 85 ~ 95 parts, hard monomer 5 ~ 15 parts, function monomer 2 ~ 5 parts, emulsifying agent 1.3 ~ 4 parts, deionized water 30 ~ 55 parts, stirs after mixing and is prepared into pre-emulsion;
(2) 0.1 ~ 0.3 mass parts initiator is dissolved in the deionized water of 4 ~ 6 mass parts, is mixed with initiator solution;
(3) in a kettle., in mass parts, add 35 ~ 50 parts of deionized waters, 0.15 ~ 0.25 part of initiator, 0.3 ~ 0.8 part of emulsifying agent and 0.3 ~ 0.5 part of pH buffer reagent, stir, then pre-emulsion 13 ~ 15 parts in step (1) and the obtained initiator solution 0.5 ~ 1.0 part of step (2) is added under agitation, be warming up to 83 ~ 86 DEG C to react, occur after blue light until emulsion, 0.1 ~ 0.3 part of chain-transfer agent is dripped again in reactor, 88.04 ~ 127.2 parts of pre-emulsions and 2.88 ~ 4.24 parts of initiator solutions, continuous dropping 2h adds, again the solution that ketocarbonyl-containing monomer 0.5 ~ 2 part is dissolved in 2 ~ 5 parts of deionized waters is dripped together with 22.06 ~ 31.8 parts of pre-emulsions, continuous dropping 0.5 ~ 1h adds, add 0.72 ~ 1.06 part of initiator solution again, be warmed up to 86 ~ 90 DEG C and insulation reaction 1 ~ 1.5h, cool the temperature to less than 40 DEG C again, adjust ph to 6.5 ~ 7.0,
(4) hydrazide group monomer 0.4 ~ 1.6 mass parts is dissolved in 2 ~ 5 mass parts deionized waters, be made into hydrazide group monomer solution, then joined in the reactor of step (3), be uniformly mixed, obtained room-temperature self crosslinking polyacrylate pressure-sensitive;
Acrylate soft monomer described in step (1) is the mixture of at least one in ethyl propenoate, butyl acrylate and Isooctyl acrylate monomer, and wherein Isooctyl acrylate monomer accounts for 55% ~ 85% of acrylate soft monomer total mass;
Hard monomer described in step (1) is the mixture of at least one in vinyl acetate between to for plastic, tertiary ethylene carbonate and methyl methacrylate, and wherein methyl methacrylate accounts for 70% ~ 85% of hard monomer total mass;
Function monomer described in step (1) is the mixture of at least one in Hydroxyethyl acrylate, Propylene glycol monoacrylate, glycidyl acrylate and propyloic acrylic ester; Described in step (1) or step (3), emulsifying agent is anionic emulsifier or reactive emulsifier.
2. the preparation method of a kind of room-temperature self crosslinking polyacrylate pressure-sensitive according to claim 1, is characterized in that: described anionic emulsifier is sodium lauryl sulphate; Reactive emulsifier is allyloxy hydroxypropyl azochlorosulfonate acid sodium.
3. the preparation method of a kind of room-temperature self crosslinking polyacrylate pressure-sensitive according to claim 1, is characterized in that: described in step (3), pH buffer reagent is sodium bicarbonate; Described chain-transfer agent is lauryl mercaptan or mercaptoethanol; Described ketocarbonyl-containing monomer is diacetone-acryloamide(DAA).
4. the preparation method of a kind of room-temperature self crosslinking polyacrylate pressure-sensitive according to claim 1, is characterized in that: described in step (2) or step (3), initiator is ammonium persulphate or Potassium Persulphate; Hydrazide group monomer described in step (4) is any one in carbon acid dihydrazide, careless acid dihydrazide, succinic acid hydrazide ii, adipic dihydrazide.
5. the preparation method of a kind of room-temperature self crosslinking polyacrylate pressure-sensitive according to claim 1, is characterized in that: the agitation condition described in step (3) refers to that mixing speed is the condition of 200 ~ 250r/min.
6. a room-temperature self crosslinking polyacrylate pressure-sensitive, is characterized in that: obtain prepared by the preparation method according to any one of Claims 1 to 5.
7. the application of a kind of room-temperature self crosslinking polyacrylate pressure-sensitive according to claim 6 in forming label, it is characterized in that: embody rule process is: rapidly and uniformly room-temperature self crosslinking polyacrylate pressure-sensitive is coated on the separate paper crossed through corona treatment with line rod spreader, the baking oven this separate paper being put into 105 DEG C subsequently dries 2min, take out after drying, the glue one side that has ivory board being attached to separate paper obtains label paper, be cut to standard specimen 250mm*25mm again, obtain the label that bond performance is excellent.
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