CN101864258A - Low temperature resistant seal adhesive and preparation method thereof - Google Patents
Low temperature resistant seal adhesive and preparation method thereof Download PDFInfo
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- CN101864258A CN101864258A CN201010192014A CN201010192014A CN101864258A CN 101864258 A CN101864258 A CN 101864258A CN 201010192014 A CN201010192014 A CN 201010192014A CN 201010192014 A CN201010192014 A CN 201010192014A CN 101864258 A CN101864258 A CN 101864258A
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Abstract
The invention discloses a low temperature resistant seal adhesive and a preparation method thereof, belonging to the adhesive field. The adhesive comprises the following components: styrene or methyl methacrylate, vinylacetate, butyl acrylate, ethyl hexyl acrylate, acrylic acid, crosslinking monomer, adhesive force reinforcing monomer, tackifying resin, polyvinyl alcohol, emulsifier, initiator, tert-butyl hydroperoxide, buffering agent, pH regulator and deionized water. The monomers in the components are pre-emulsified through a substep pre-emulsified process to lead the tackifying resin to be distributed on the surfaces of the emulsion particles; a continuous dropwise added process is adopted to dropwise add the other components to prepare into polymer emulsion; the prepared emulsion is used for configuring and preparing a glue solution system of the seal adhesive; the emulsion has the characteristic of low glass transition temperature, thus the low temperature resistance is good, inner crosslinking monomer is introduced, and the defect that adhesive cohesive strength is not enough due to low glass transition temperature is remedied; the tackifying resin is distributed on the surfaces of emulsion particles; and the wettability of the adhesive to a base material is enhanced.
Description
Technical field
The present invention relates to adhesive area, especially relate to a kind of high strength low temperature resistant seal adhesive and preparation method thereof.
Background technology
Along with the quick growth of all kinds of consumer's goods industries, the demand of packaging seal tackiness agent is increased rapidly.Along with the raising of people's environmental consciousness and the increasingly stringent of government's environmental regulation, noxious solvent type tackiness agent has withdrawed from market gradually, and innoxious solvent type tackiness agent is because its cost height, and competitive power is not strong; The water-latex type tackiness agent because of its with water compositing dispersion medium, therefore have environment-protecting asepsis and the low advantage of cost, become the product of greatly developing.Especially in the food product pack field, the water-latex type tackiness agent has become main product.
For the food packing industry seal adhesive, important performance index also need to have lower temperature resistance, because most of food needs deepfreeze except tackiness agent cohesive strength, sticking power and wettability to base material.Therefore require the food product pack seal adhesive can not have too high second-order transition temperature, otherwise at low temperatures, embrittlement can take place in glue-line.In order to improve bonding strength, the means that adopt are to introduce the function monomer of band polar group at present, as vinylformic acid, Rocryl 410 etc., though the introducing of polar group can effectively improve the sticking power of tackiness agent and base material, but also increased the interfacial tension of tackiness agent emulsion simultaneously with base material, make that emulsion can not be well wetting by sticking base material, had a strong impact on adhesive effect, therefore it is low to introduce molecular polarity in system, the tackifying resin that molecular weight is less reduces tackiness agent and the interfacial tension of being glued substrate surface.Usually the method that adds tackifying resin is with tackifier resin emulsion and tackiness agent emulsion blending, and this method can not make tackifying resin attached to the emulsion particle surface, so modified effect is general, and has reduced the package stability of emulsion.
Summary of the invention
The purpose of the embodiment of the invention provides a kind of low temperature resistant seal adhesive and preparation method thereof, this seal adhesive has good low temperature adhesiveproperties and higher stripping strength, can overcome the problem that existing water-latex type sealing compound low-temperature adhesion performance is bad and stripping strength is low.
The purpose of the embodiment of the invention is achieved through the following technical solutions:
The embodiment of the invention provides a kind of low temperature resistant seal adhesive, and this seal adhesive comprises following component by weight percentage:
Vinylbenzene and/or methyl methacrylate 5～15%
Vinyl acetate 1～10%
Butyl acrylate 20～40%
Isooctyl acrylate monomer 1～10%
Vinylformic acid 0.5～5%
Cross-linking monomer 0.5～5%
Bonding force strengthens monomer 0.5～5%
Tackifying resin 0.5～5%
Polyvinyl alcohol 0.05～0.2%
Emulsifying agent 0.1～2%
Initiator 0.1～0.5%
Tertbutyl peroxide 0.01～0.05%
Buffer reagent 0.01～0.05%
Deionized water 40～60%
After above-mentioned each component carried out radical polymerization, add the pH regulator agent and regulate the pH value of polymerisate and be adjusted to 9～10 polymer emulsions that obtain, be low temperature resistant seal adhesive.
The embodiment of the invention also provides a kind of preparation method of low temperature resistant seal adhesive, it is characterized in that, comprising:
Measure each component by the usefulness of following prescription, wherein each component all by weight percentage;
Vinylbenzene and/or methyl methacrylate 5～15%, vinyl acetate 1～10%, butyl acrylate 20～40%, Isooctyl acrylate monomer 1～10%, vinylformic acid 0.5～5%, cross-linking monomer 0.5～5%, bonding force strengthens monomer 0.5～5%, tackifying resin 0.5～5%, polyvinyl alcohol 0.05～0.2%, emulsifying agent 0.1～2%, initiator 0.1～0.5%, tertbutyl peroxide 0.01～0.05%, buffer reagent 0.01～0.05%, pH regulator agent 0.01～0.05% and deionized water 40～60%;
Preparation process comprises the steps:
Pre-emulsification: tackifying resin is joined in whole Butyl Acrylate Monomers, tackifying resin is fully dissolved; Will be after all the other monomers (comprising: vinylbenzene and/or methyl methacrylate, vinyl acetate, Isooctyl acrylate monomer, vinylformic acid, the cross-linking monomer) component cohesive force strengthens monomer be mixed, join in the mixed solution of deionized water and emulsifying agent, under whipped state, carry out the pre-emulsification of 0.5～2h, obtain pre-emulsion A; The Butyl Acrylate Monomer that will be dissolved with tackifying resin again under whipped state splashes among the pre-emulsion A, obtains pre-emulsion B;
Polyreaction: with deionized water, polyvinyl alcohol, emulsifying agent and buffer reagent stir in reaction vessel, when heating in water bath elevates the temperature to 60～90 ℃ simultaneously, drip described pre-emulsion B and the initiator that accounts for initiator gross weight 4/5ths, dripped off in 3～4 hours, it in pre-emulsion B dripping quantity 1/2 o'clock of pre-emulsion B total amount, cohesive force is strengthened monomer to join among the pre-emulsion B that does not drip, all be added dropwise to complete the back and continue slaking 1.5～2 hours, add remaining initiator, be cooled to below 40 ℃, the pH value that adds pH regulator agent conditioned reaction product is 9～10, filter discharging and promptly obtain polymer emulsion, this polymer emulsion is seal adhesive at normal temperature.
The technical scheme that is provided by the invention described above embodiment as can be seen, pass through in the embodiment of the invention each component substep pre-emulsification technology, make tackifying resin attached to micellar surface, and the introducing cohesive force strengthens monomer, make a kind of emulsion-type seal adhesive, this seal adhesive strengthens the wettability and the tack of base material; By crosslinked function monomer in introducing, remedied the low weakness of polymer segment cohesive strength of low Tg, both guaranteed to have higher stripping strength with this seal adhesive, have good low-temperature adhesion performance again.
Embodiment
The embodiment of the invention provides a kind of low temperature resistant seal adhesive and preparation method thereof.This seal adhesive is that to strengthen monomer, tackifying resin, polyvinyl alcohol, emulsifying agent, initiator, tertbutyl peroxide, buffer reagent, pH regulator agent, deionized water with vinylbenzene or methyl methacrylate, vinyl acetate, butyl acrylate, Isooctyl acrylate monomer, vinylformic acid, cross-linking monomer, sticking power be component, by the substep pre-emulsification technology monomer is carried out pre-emulsification, make the tackifying resin substep on the emulsion particle surface, adopt continuously dropping technology that other each components are dripped and prepare a kind of emulsion-type seal adhesive.This seal adhesive has the low characteristics of second-order transition temperature, therefore resistance to low temperature is good, has introduced interior cross-linking monomer, remedies the low insufficient shortcoming of tackiness agent cohesive strength that causes of second-order transition temperature, the tackifying resin substep is on the emulsion particle surface, and the seal adhesive that increase makes is to the wettability of base material.
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
Present embodiment provides a kind of low temperature resistant seal adhesive, and this seal adhesive comprises following component, and the consumption of each component is all by the weight percent meter that accounts for total system:
Vinylbenzene and/or methyl methacrylate 5～15%
Vinyl acetate 1～10%
Butyl acrylate 20～40%
Isooctyl acrylate monomer 1～10%
Vinylformic acid 0.5～5%
Cross-linking monomer 0.5～5%
Cohesive force strengthens monomer 0.5～5%
Tackifying resin 0.5～5%
Polyvinyl alcohol 0.05～0.2%
Emulsifying agent 0.1～2%
Initiator 0.1～0.5%
Tertbutyl peroxide 0.01～0.05%
Buffer reagent 0.01～0.5%
PH regulator agent 0.01～0.05%
Deionized water 40～60%;
After above-mentioned each component carried out radical polymerization, adding the pH regulator agent, to regulate the pH value of polymerisate be 9～10, and the creamy white polymer emulsion of the band blue light that obtains is low temperature resistant seal adhesive.The second-order transition temperature of this seal adhesive is-30～0 ℃, therefore has the good low-temperature adhesiveproperties.
In the above-mentioned seal adhesive, used cross-linking monomer is the function monomer that contains crosslinkable functionality, preferably adopts N hydroxymethyl acrylamide.
It is the function monomer that contains functional group that used cohesive force strengthens monomer, preferably adopts urea lopps function monomer.
Used tackifying resin adopts any in Gum Rosin, the rare resin of terpene, and wherein, Gum Rosin preferably adopts the nilox resin resin.
Used emulsifying agent adopts the mixture of polyoxyethylene nonylphenol ether ammonium sulfate salt (as: NPES-1030 of the CO-436 that Hai'an, Jiangsu petroleum chemical plant is produced, the gas chemical industry company limited of section) and alkylphenol-polyethenoxy base ether (as: NP-10, OP-10 that XX company produces); Or emulsifying agent adopts the mixture of alkylsurfuric acid salt (as: lauryl mercaptan K-12) and alkylphenol-polyethenoxy base ether (as: alkylphenol-polyethenoxy base ether NP-10, octylphenol polyethylene oxyethylene group ether OP-10);
Used initiator adopts persulphate, preferentially adopts ammonium persulphate.
Described buffer reagent is a sodium bicarbonate.
Ammoniacal liquor is adopted in described pH regulator agent, and its consumption is adjusted to 9～10 by the pH value with polymerisate and is as the criterion.
The preparation method of above-mentioned low temperature resistant seal adhesive specifically comprises the steps:
Weight percent by consumption in the above-mentioned prescription is got each component;
Pre-emulsification: tackifying resin in the raw material is joined in whole Butyl Acrylate Monomers, tackifying resin is fully dissolved; To form monomer mixed solution except that all the other monomer components (all the other monomers comprise: vinylbenzene and/or methyl methacrylate, vinyl acetate, Isooctyl acrylate monomer, vinylformic acid and cross-linking monomer) cohesive force strengthens monomer mix the back, the monomer mixed solution that forms is joined in the mixed solution of deionized water and emulsifying agent, under whipped state, carry out the pre-emulsification of 0.5～2h, obtain pre-emulsion A; The Butyl Acrylate Monomer that will be dissolved with tackifying resin again under whipped state slowly adds among the pre-emulsion A, obtains pre-emulsion B.
Polyreaction: with deionized water, polyvinyl alcohol, emulsifying agent and buffer reagent stir in reaction vessel, when heating in water bath elevates the temperature to 60～90 ℃ simultaneously, drip above-mentioned pre-emulsifying step pre-emulsion B that makes and the initiator that accounts for initiator gross weight 4/5ths, 3～4h drips off, it in pre-emulsion B dripping quantity 1/2 o'clock of pre-emulsion B total amount, cohesive force is strengthened monomer to join among the pre-emulsion B that does not drip, all be added dropwise to complete the back and continue slaking 1.5～2h, add remaining initiator, be cooled to below 40 ℃, the pH value that adds pH regulator agent conditioned reaction product is 9～10, filter the polymer emulsion that discharging obtains, promptly get seal adhesive.The second-order transition temperature that makes seal adhesive is-30～0 ℃, is preferably-30～-10 ℃, more preferably-20～-10 ℃.
Among the above-mentioned preparation method, elevate the temperature to 60～90 ℃ of steps, heating in water bath is elevated the temperature to 70～83 ℃, more preferably heating in water bath is elevated the temperature to 78～83 ℃ at heating in water bath.
The preparation method of present embodiment by each component being used the substep pre-emulsification technology, makes tackifying resin attached to micellar surface, and introduces cohesive force enhancing monomer, makes this seal adhesive strengthen the wettability and the tack of base material; By crosslinked function monomer in introducing, remedied the low weakness of polymer segment cohesive strength of low Tg, both guaranteed that this seal adhesive had higher stripping strength, have good low-temperature adhesion performance again.
Embodiment 2
Present embodiment provides a kind of high strength low temperature resistant seal adhesive, each component of the prescription of this seal adhesive such as table 1 record:
Table 1
| Component | Consumption (g) | Component | Consumption (g) |
| MMA (methyl methacrylate) | ??48 | The rare resin of terpene (tackifying resin) | ??8 |
| VAc (vinyl acetate) | ??27 | PVA1788 (polyvinyl alcohol) | ??1 |
| BA (butyl acrylate) | ??144 | CO-436 (emulsifying agent) polyoxyethylene nonylphenol ether ammonium sulfate salt | ??3 |
| 2-EHA (the different monooctyl ester of vinylformic acid 2-) | NP-10 (emulsifying agent) alkylphenol-polyethenoxy base ether | ??2 | |
| AA (vinylformic acid) | ??16.8 | APS (initiator) | ??2 |
| ??5 | Tertbutyl peroxide | ??0.2 |
| Component | Consumption (g) | Component | Consumption (g) |
| NMA (N hydroxymethyl acrylamide) | ??5 | Sodium bicarbonate (buffer reagent) | ??1 |
| QM-1558 (urea lopps function monomer) | ??3 | ??H 2O (deionized water) | ??286 |
The preparation method of this seal adhesive comprises the steps:
Tackifying resin is joined in whole BA (butyl acrylate) monomer, make fully dissolving of tackifying resin (the rare resin of terpene).MMA (methyl methacrylate), Vac (vinyl acetate), 2-EHA (the different monooctyl ester of vinylformic acid 2-), AA (vinylformic acid), NMA (N hydroxymethyl acrylamide) component are mixed the back form monomer mixed solution, the monomer mixed solution that forms is joined in the mixed solution of deionized water and emulsifying agent, under whipped state, carry out the pre-emulsification of 0.5～2h, obtain pre-emulsion A; The Butyl Acrylate Monomer that will be dissolved with tackifying resin again under whipped state slowly adds among the pre-emulsion A, obtains pre-emulsion B;
Pre-emulsion B is finished and has rebasing liquid (deionized water to intensification, emulsifying agent, polyvinyl alcohol and buffer reagent sodium bicarbonate) four-hole bottle in drip, drip the initiator that accounts for initiator gross weight 4/5ths simultaneously, 3～4h drips off, it in pre-emulsion B dripping quantity 1/2 o'clock of pre-emulsion B total amount, QM-1558 (urea lopps function monomer) is joined among the pre-emulsion B that does not drip, all be added dropwise to complete the back and continue slaking 1.5～2h, add remaining initiator, be cooled to below 40 ℃, adding ammoniacal liquor is 9～10 as the pH value of pH regulator agent conditioned reaction product, and the emulsion polymeric product that the filtration discharging obtains is seal adhesive.The second-order transition temperature of this seal adhesive is-20 ℃, and solid content is about 49%, 180 ° stripping strength can reach 1.3N/mm.
Embodiment 3
Present embodiment provides a kind of high strength low temperature resistant seal adhesive, each component of the prescription of this seal adhesive such as table 2 record:
Table 2
| Component | Consumption (g) | Component | Consumption (g) |
| St (vinylbenzene) | ??40 | Gum Rosin (tackifying resin) | ??11 |
| VAc (vinyl acetate) | ??32 | PVA1788 (polyvinyl alcohol) | ??1 |
| BA (butyl acrylate) | ??160 | Lauryl mercaptan K-12 (emulsifying agent) alkylsurfuric acid salt | ??4 |
| OP-10 (emulsifying agent) alkylphenol-polyethenoxy base ether | ??1 | ||
| 2-EHA (the different monooctyl ester of vinylformic acid 2-) | ??20 | APS (initiator) | ??2 |
| Component | Consumption (g) | Component | Consumption (g) |
| AA (vinylformic acid) | ??5 | Tertbutyl peroxide | ??0.2 |
| NMA (N hydroxymethyl acrylamide) | ??5 | Sodium bicarbonate (buffer reagent) | ??1 |
| QM-1558 (urea lopps function monomer) | ??3 | H2O (deionized water) | ??286 |
The preparation method of this seal adhesive comprises the steps:
Gum Rosin is joined in whole BA (butyl acrylate) monomer, make fully dissolving of tackifying resin (Gum Rosin, available nilox resin resin); St (vinylbenzene), Vac (vinyl acetate), 2-EHA (the different monooctyl ester of vinylformic acid 2-), AA (vinylformic acid), NMA (N hydroxymethyl acrylamide) component are mixed the back form monomer mixed solution, the monomer mixed solution that forms is joined in the mixed solution of deionized water and emulsifying agent (K-12 and OP-10), under whipped state, carry out the pre-emulsification of 0.5～2h, obtain pre-emulsion A; The Butyl Acrylate Monomer that will be dissolved with tackifying resin again under whipped state slowly adds among the pre-emulsion A, obtains pre-emulsion B;
Pre-emulsion B is finished and has rebasing liquid (deionized water to intensification, emulsifying agent, polyvinyl alcohol and buffer reagent sodium bicarbonate) four-hole bottle in drip, drip the initiator that accounts for initiator total amount 4/5ths simultaneously, 3～4h drips off, it in pre-emulsion B dripping quantity 1/2 o'clock of pre-emulsion B total amount, QM-1558 (urea lopps function monomer) is joined among the pre-emulsion B that does not drip, all be added dropwise to complete the back and continue slaking 1.5～2h, add remaining initiator, be cooled to below 40 ℃, adding ammoniacal liquor is 9～10 as pH regulator agent adjusting pH value, the emulsion polymeric product that the filtration discharging obtains is seal adhesive, the second-order transition temperature of this seal adhesive is-29 ℃, solid content is about 50%, 180 ° of stripping strength can reach 1.1N/mm.
In sum, in the embodiment of the invention, by selecting vinylbenzene and/or methyl methacrylate for use, vinyl acetate, butyl acrylate, Isooctyl acrylate monomer, vinylformic acid, cross-linking monomer, bonding force strengthens monomer, tackifying resin, polyvinyl alcohol, emulsifying agent, initiator, tertbutyl peroxide, buffer reagent and deionized water are raw material, carry out pre-emulsification with the substep pre-emulsification technology, make tackifying resin attached to micellar surface, and the introducing cohesive force strengthens monomer, make a kind of emulsion-type seal adhesive, this seal adhesive strengthens the wettability and the tack of base material; By crosslinked function monomer in introducing, remedied the low weakness of polymer segment cohesive strength of low Tg, guaranteed that this seal adhesive had both had higher stripping strength, have good low-temperature adhesion performance again.This seal adhesive is a kind ofly can the base material good wet to be had again than strong adhesive force, has the seal adhesive than low Tg and shelf-stable simultaneously, has effectively improved the performance of this emulsion-type seal adhesive.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (10)
1. a low temperature resistant seal adhesive is characterized in that, this seal adhesive comprises following component by weight percentage:
Vinylbenzene and/or methyl methacrylate 5～15%
Vinyl acetate 1～10%
Butyl acrylate 20～40%
Isooctyl acrylate monomer 1～10%
Vinylformic acid 0.5～5%
Cross-linking monomer 0.5～5%
Bonding force strengthens monomer 0.5～5%
Tackifying resin 0.5～5%
Polyvinyl alcohol 0.05～0.2%
Emulsifying agent 0.1～2%
Initiator 0.1～0.5%
Tertbutyl peroxide 0.01～0.05%
Buffer reagent 0.01～0.5%
Deionized water 40～60%
After above-mentioned each component carried out radical polymerization, add the pH regulator agent and regulate the pH value of polymerisate and be adjusted to 9～10 polymer emulsions that obtain, be low temperature resistant seal adhesive.
2. low temperature resistant seal adhesive according to claim 1 is characterized in that, the second-order transition temperature of described seal adhesive is-30～0 ℃.
3. low temperature resistant seal adhesive according to claim 1 is characterized in that, described cross-linking monomer is the function monomer that contains crosslinkable functionality.
4. according to claim 1 or 3 described low temperature resistant seal adhesives, it is characterized in that any in described cross-linking monomer employing N hydroxymethyl acrylamide, Hydroxyethyl acrylate, Propylene glycol monoacrylate, the glycidyl acrylate or several arbitrarily.
5. low temperature resistant seal adhesive according to claim 1 is characterized in that, described cohesive force strengthens monomer and adopts urea lopps function monomer.
6. low temperature resistant seal adhesive according to claim 1 is characterized in that, described tackifying resin adopts any in Gum Rosin, the rare resin of terpene; Described Gum Rosin adopts the nilox resin resin.
7. low temperature resistant seal adhesive according to claim 1 is characterized in that, described emulsifying agent adopts the mixture of polyoxyethylene nonylphenol ether ammonium sulfate salt and alkylphenol-polyethenoxy base ether; Or the mixture of alkylsurfuric acid salt and alkylphenol-polyethenoxy base ether;
Described buffer reagent adopts sodium bicarbonate;
Ammoniacal liquor is adopted in described pH regulator agent.
8. low temperature resistant seal adhesive according to claim 1 is characterized in that, described initiator adopts any or any two kinds in persulphate, the organo-peroxide.
9. the preparation method of a low temperature resistant seal adhesive is characterized in that, comprising:
Measure each component by the usefulness of following prescription, wherein each component all by weight percentage;
Vinylbenzene and/or methyl methacrylate 5～15%, vinyl acetate 1～10%, butyl acrylate 20～40%, Isooctyl acrylate monomer 1～10%, vinylformic acid 0.5～5%, cross-linking monomer 0.5～5%, bonding force strengthens monomer 0.5～5%, tackifying resin 0.5～5%, polyvinyl alcohol 0.05～0.2%, emulsifying agent 0.1～2%, initiator 0.1～0.5%, tertbutyl peroxide 0.01～0.05%, buffer reagent 0.01～0.05%, pH regulator agent 0.01～0.05% and deionized water 40～60%;
Preparation process comprises the steps:
Pre-emulsification: tackifying resin is joined in whole Butyl Acrylate Monomers, tackifying resin is fully dissolved; After will mixing except that all the other monomer components the cohesive force enhancing monomer, join in the mixed solution of deionized water and emulsifying agent, under whipped state, carry out the pre-emulsification of 0.5～2h, obtain pre-emulsion A; The Butyl Acrylate Monomer that will be dissolved with tackifying resin again under whipped state splashes among the pre-emulsion A, obtains pre-emulsion B;
Polyreaction: with deionized water, polyvinyl alcohol, emulsifying agent and buffer reagent stir in reaction vessel, when heating in water bath elevates the temperature to 60～90 ℃ simultaneously, drip described pre-emulsion B and the initiator that accounts for initiator gross weight 4/5ths, dripped off in 3～4 hours, it in pre-emulsion B dripping quantity 1/2 o'clock of pre-emulsion B total amount, cohesive force is strengthened monomer to join among the pre-emulsion B that does not drip, all be added dropwise to complete the back and continue slaking 1.5～2 hours, add remaining initiator, be cooled to below 40 ℃, the pH value that adds pH regulator agent conditioned reaction product is 9～10, filter discharging and promptly obtain polymer emulsion, this polymer emulsion is seal adhesive at normal temperature.
10. the preparation method of low temperature resistant seal adhesive according to claim 9 is characterized in that, described heating in water bath elevates the temperature to 60～90 ℃ and comprises:
Preferred heating in water bath elevates the temperature to 70～83 ℃, and more preferably heating in water bath elevates the temperature to 78～83 ℃.
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