CN103724521A - Preparation method of single-component polyacrylate pressure-sensitive adhesive for optical protective film - Google Patents
Preparation method of single-component polyacrylate pressure-sensitive adhesive for optical protective film Download PDFInfo
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- CN103724521A CN103724521A CN201410014315.1A CN201410014315A CN103724521A CN 103724521 A CN103724521 A CN 103724521A CN 201410014315 A CN201410014315 A CN 201410014315A CN 103724521 A CN103724521 A CN 103724521A
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 229920000058 polyacrylate Polymers 0.000 title claims abstract description 29
- 230000003287 optical effect Effects 0.000 title claims abstract description 24
- 230000001681 protective effect Effects 0.000 title abstract description 17
- 239000003960 organic solvent Substances 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 60
- 238000009835 boiling Methods 0.000 claims description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 13
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 10
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 9
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 9
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 9
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- 229940043232 butyl acetate Drugs 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 6
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 5
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 5
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 3
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 claims description 3
- GILMNGUTRWPWSY-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate;2-methylprop-2-enoic acid Chemical compound CC(=C)C(O)=O.CC(O)COC(=O)C=C GILMNGUTRWPWSY-UHFFFAOYSA-N 0.000 claims description 3
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 3
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- YQHLDYVWEZKEOX-UHFFFAOYSA-N cumene hydroperoxide Chemical compound OOC(C)(C)C1=CC=CC=C1 YQHLDYVWEZKEOX-UHFFFAOYSA-N 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 46
- 239000012528 membrane Substances 0.000 description 14
- 239000010410 layer Substances 0.000 description 12
- 239000000178 monomer Substances 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000004819 Drying adhesive Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- 239000011127 biaxially oriented polypropylene Substances 0.000 description 2
- 229920006378 biaxially oriented polypropylene Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 230000009193 crawling Effects 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation method of a single-component polyacrylate pressure-sensitive adhesive for an optical protective film. The preparation method comprises the following steps: weighing a component A and a component B; uniformly mixing the component A and the component B to obtain a solution E; preparing a solution F containing a component C; weighing a component D as an organic solvent; placing part of the solutions E and F and at least 2/3 of the organic solvent into a four-neck flask; reacting under a certain conditions; then dropwise adding the remaining solutions E and F into the four-neck flask; keeping warm; dropwise adding the remaining organic solvent into the four-neck flask; cooling down; and then filtering to obtain a pressure-sensitive adhesive. The preparation method of the single-component polyacrylate pressure-sensitive adhesive for the optical protective film disclosed by the invention is simple in process, completed in one step, high in production efficiency and low in cost; and the prepared pressure-sensitive adhesive has good stability.
Description
Technical field
The present invention relates to pressure sensitive adhesive synthesis technical field, relate to particularly the preparation method of a single-component polyacrylate pressure-sensitive for optical protection layer.
Background technology
Pressure sensitive adhesive be external force gently depress just can be bonding with adherend a class glue paste, by its production method, be divided into hot-melting type, solvent-borne type, aqueous solution type, emulsion-type, calendering type and the large class of response type six.Along with improving constantly of environmental requirement, although the Application Areas of oiliness polyacrylate pressure-sensitive and consumption reduce to some extent, oiliness polypropylene ester pressure-sensitive still occupies considerable status in pressure sensitive adhesive industry, and its market demand surpasses emulsion-type pressure-sensitive.
The shortcoming of pressure-sensitive polyacrylate emulsion glue is that water tolerance and lower temperature resistance are poor in the market, and emulsion-type pressure-sensitive wettability is poor, crawling is even, and cull easily appears in protection base material (blooming), and " shadow " problem such as cannot thoroughly solve at the shortcoming.And use oiliness pressure sensitive adhesive, be mainly two component sizing agents, need to join according to a certain percentage glue, and duration of service be restricted before using, the glue of having prepared need to use at short notice.This certainly will increase production cost, reduces production efficiency.
CN101962525A patent discloses a kind of pressure sensitive adhesive and preparation method thereof and has applied the protective membrane of this pressure sensitive adhesive; wherein pressure-sensitive adhesive formula comprises: butyl methacrylate 20-30 part; 2-EHA 20-30 part; methyl methacrylate 5-10 part; Propylene glycol monoacrylate 2-5 part, fluorine-silicon modified acrylic ester resin 0-15 part, Viscoat 295 0-1 part or polyethyleneglycol diacrylate 0-1 part; polyether-modified polyisocyanates 0.2-0.5 part, esters solvent 50-60 part.This pressure sensitive adhesive is mainly coated on PE, PP protective membrane, is used for protecting optical thin film.But the shortcoming of this invention is complex process, temperature of reaction is too high, and reaction is difficult to be controlled, and uses linking agent easily to produce gel.
CN102746445A patent discloses the preparation method of solvent type polyacrylate pressure sensitive adhesive for a kind of freight container pad pasting, and wherein each monomer mass percentage ratio is: Isooctyl acrylate monomer monomer 8-16%, Butyl Acrylate Monomer 40-70%, Vinyl Acetate Monomer 20-27%, Acrylic Acid Monomer 2-6%.But the present invention is only applicable to polymer PVC protective membrane, is not suitable for PET protective membrane.
CN102533183A patent discloses a kind of solvent type organic silicone modified acrylate pressure sensitive adhesive and its preparation method and application, solvent type organic silicone modified acrylate pressure sensitive adhesive is by the polymerization and preparing in reactor of following component raw material, and its composition and ratio is counted as follows by weight: composition A:1～10, ethyl acrylate 10～30, butyl acrylate 10～30, vinylbenzene 2～5, methyl methacrylate 2～4, Propylene glycol monoacrylate 1～4, vinylformic acid 1～2, dibenzoyl peroxide 0.1～0.8, ethyl acetate 45～55; Described composition A is by octamethylcyclotetrasiloxane 50～75 weight parts, γ-methacryloxypropyl trimethoxy silane 5～15 weight parts, hexamethyldisiloxane 15～40 weight parts, Tetramethylammonium hydroxide 0.05～0.24 weight part polymerization and prepare.Protective membrane prepared by the present invention can suppress the growth of protective membrane peeling force with pressure sensitive adhesive, increase the bonding strength to low surface energy surface, but pressure sensitive adhesive molecular weight of the present invention is little, and adhesive effect is not good enough, and pressure sensitive adhesive is not suitable for PET protective membrane.
Summary of the invention
In view of this, the invention provides a kind of preparation method of the single-component polyacrylate pressure-sensitive for optical protection layer.
To achieve these goals, the technical scheme that the embodiment of the present invention provides is as follows:
For a preparation method for the single-component polyacrylate pressure-sensitive of optical protection layer, it comprises the steps:
Take and be selected from following compound: the A component of at least one in ethyl propenoate, n-butyl acrylate, isobutyl acrylate, Isooctyl acrylate monomer, stearyl methacrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, n-BMA, vinyl acetate, and be selected from following compound: the B component of at least one in vinylformic acid-2-hydroxyl ethyl ester, 2-hydroxypropyl acrylate, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate, 1,6 hexanediol diacrylate, Viscoat 295, vinylformic acid, methacrylic acid;
A component and B component are mixed and obtain E solution;
The F solution that preparation contains C component, described C component is selected from following compound: at least one in benzoyl peroxide, Diisopropyl azodicarboxylate, tertbutyl peroxide, isopropyl benzene hydroperoxide, methylethyl ketone peroxide, dicumyl peroxide;
Take D component as organic solvent;
Described 1/3 E solution, 1/3 F solution and at least 2/3 organic solvent are placed in to four-hole boiling flask, at temperature 70-85 ℃, after reaction 1-3h, in 4-8h, remaining E solution, F solution are added drop-wise in four-hole boiling flask to insulation, in 10min, remaining organic solvent is added drop-wise in four-hole boiling flask, after cooling, filters and obtain pressure sensitive adhesive.
As a further improvement on the present invention, described A component is selected from the 2-4 kind in n-butyl acrylate, Isooctyl acrylate monomer, stearyl methacrylate, methyl methacrylate, vinyl acetate, and described A component accounts for the 50-90% of A, B, C component gross weight.
As a further improvement on the present invention, described B component is selected from vinylformic acid-2-hydroxyl ethyl ester, 1,1-3 kind in 6-hexanediyl ester, Viscoat 295, vinylformic acid, methacrylic acid, described B component accounts for the 0.1-9.9% of A, B, C component gross weight.
As a further improvement on the present invention, described F solution is the ethyl acetate solution that contains C component, and the ratio of described C component and ethyl acetate is: 1:2-1:4, described C component accounts for the 0.1-2% of A, B, C component gross weight.
As a further improvement on the present invention, the described D component as organic solvent is selected from following organism: the 1-3 kind in ethyl acetate, butylacetate, acetone, butanone, the proportional range of the gross weight of described D component and A, B, C component is 1:1-1:4.
As a further improvement on the present invention, in described D component, every kind of organism of choosing accounts for the 30-400% of A, B, C gross weight.
As a further improvement on the present invention, described four-hole boiling flask is with stirring, reflux, and constant pressure funnel.
As a further improvement on the present invention, described soaking time is 1-3h.
As a further improvement on the present invention, described remaining organic solvent is added drop-wise in four-hole boiling flask after, cool to 30-40 ℃.
The quality solid content of the pressure sensitive adhesive making as a further improvement on the present invention, is 20-55%.
Compared with prior art, the invention has the beneficial effects as follows: preparation method's technique of the single-component polyacrylate pressure-sensitive for optical protection layer of the present invention is simple, settle at one go, production efficiency is high, cost is low, the pressure sensitive adhesive good stability of preparation.
Meanwhile, the single-component polyacrylate pressure-sensitive making can be applicable on the optical protection layers such as PET protective membrane, PE film, PVC film or BOPP film, and it is easy to use, and less wastage is easily peeled off, and there will not be the phenomenon of cull, " shadow " after peeling off.And above-mentioned pressure sensitive adhesive is under room temperature 25 degree, its stripping strength < 8gf/25mm; Coating drying adhesive layer 10 μ m, after 150 degree baking 2h, its stripping strength < 12gf/25mm.
Accompanying drawing explanation
Fig. 1 is the preparation method's of the single-component polyacrylate pressure-sensitive for the optical protection layer of the present invention method flow diagram of an embodiment.
Embodiment
Below the technical scheme in the embodiment of the present invention is described in detail, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, the every other embodiment that those of ordinary skills obtain under the prerequisite of not making creative work, belongs to the scope of protection of the invention.
As shown in Figure 1, be the preparation method's of the single-component polyacrylate pressure-sensitive for optical protection layer of the present invention schematic flow sheet, it comprises the steps:
(1) take mass percent be the A component of 50-90% as basic monomer, it is selected from following compound: at least one in olefin(e) acid ethyl ester, n-butyl acrylate, isobutyl acrylate, Isooctyl acrylate monomer, stearyl methacrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, n-BMA, vinyl acetate.Preferably, A component is selected from the 2-4 kind in n-butyl acrylate, Isooctyl acrylate monomer, stearyl methacrylate, methyl methacrylate, vinyl acetate.
Take mass percent and be the B component of 0.1-9.9% as modified monomer, it is selected from following compound: at least one in vinylformic acid-2-hydroxyl ethyl ester, 2-hydroxypropyl acrylate, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate, 1,6 hexanediol diacrylate, Viscoat 295, vinylformic acid, methacrylic acid.Preferably, B component is selected from the 1-3 kind in vinylformic acid-2-hydroxyl ethyl ester, 1,6 hexanediol diacrylate, Viscoat 295, vinylformic acid, methacrylic acid.
Above-mentioned A component and B component are mixed and obtain E solution.
(2) preparation contain C component F solution as initiator, described C component is selected from following compound: in benzoyl peroxide, Diisopropyl azodicarboxylate, tertbutyl peroxide, isopropyl benzene hydroperoxide, methylethyl ketone peroxide, dicumyl peroxide at least one.Particularly, above-mentioned F solution is the ethyl acetate solution that contains C component, and wherein, the ratio of C component and ethyl acetate is: 1:2-1:4.
Wherein, C component accounts for the 0.1-2% of A, B, C component gross weight, and in like manner, the mass percent of above-mentioned A component is the 50-90% that A component accounts for A, B, C component gross weight, and the mass percent of above-mentioned B component is the 0.1-9.9% that B component accounts for A, B, C component gross weight.
(3) take a certain amount of D component as organic solvent, the proportional range of the gross weight of this D component and A, B, C component is 1:1-1:4.Above-mentioned D component is selected from following organism: the 1-3 kind in ethyl acetate, butylacetate, acetone, butanone.Wherein, in D component, every kind of organism of choosing accounts for the 30-400% of A, B, C gross weight.
(4) organic solvent of above-mentioned 1/3 E solution, 1/3 F solution and at least 2/3 is placed in stirring, reflux, and in the four-hole boiling flask of constant pressure funnel.At temperature 70-85 ℃, after reaction 1-3h, in 4-8h, more remaining 2/3 E solution, 2/3 F solution are added drop-wise in four-hole boiling flask.After insulation 1-3h, in 10min, remaining organic solvent is added drop-wise in four-hole boiling flask.Cool to after 30-40 ℃, obtain after filtration single-component polyacrylate pressure-sensitive of the present invention.
The quality solid content of the single-component polyacrylate pressure-sensitive being obtained by preparation method of the present invention is 20-55%.
Below in conjunction with embodiment, the preparation method of single-component polyacrylate pressure-sensitive of the present invention is illustrated.
Embodiment 1
Proportionally preparation contains n-butyl acrylate 70g, Isooctyl acrylate monomer 22g, and the A component of stearyl methacrylate 2g, and contain vinylformic acid-2-hydroxyl ethyl ester 4g, the B component of vinylformic acid 1.9g, mixes A component and B component to obtain E solution.The C component of 0.1g benzoyl peroxide is dissolved in 0.2g ethyl acetate, is mixed with F solution.Take the D component of 100g ethyl acetate as organic solvent.By above-mentioned 1/3 E solution, 1/3 F solution, whole organic solvent, add in the four-hole boiling flask with stirring, reflux, constant pressure funnel.Be warmed up to 80 ℃, after reaction 3h, then drip remaining 2/3 E solution and 2/3 F solution, be controlled in 4h and drip off.Dropwise and be incubated again after 3h, cool to 30 ℃ and filter discharging, obtain protective membrane pressure sensitive adhesive of the present invention.In the present embodiment, the quality solid content of the pressure sensitive adhesive making is 50%.
Embodiment 2
Proportionally preparation contains n-butyl acrylate 65g, Isooctyl acrylate monomer 13g, the A component of stearyl methacrylate 3g, methyl methacrylate 8g, and contain vinylformic acid-2-hydroxyl ethyl ester 9g, the B component of vinylformic acid 1g, mixes A component and B component to obtain E solution.The C component of 1g benzoyl peroxide is dissolved in 4g ethyl acetate, is mixed with F solution.Take contain 100g ethyl acetate, 50g butylacetate D component as organic solvent.By above-mentioned 1/3 E solution, 1/3 F solution, whole organic solvent, add in the four-hole boiling flask with stirring, reflux, constant pressure funnel.Be warmed up to 85 ℃, after reaction 3h, then drip remaining 2/3 E solution and 2/3 F solution, be controlled in 6h and drip off.Dropwise and be incubated again after 1h, cool to 30 ℃ and filter discharging, obtain protective membrane pressure sensitive adhesive of the present invention.In the present embodiment, the quality solid content of the pressure sensitive adhesive making is 40%.
Embodiment 3
Proportionally preparation contains n-butyl acrylate 70g, Isooctyl acrylate monomer 16g, stearyl methacrylate 4g, the A component of vinyl acetate 4g, and contain vinylformic acid-2-hydroxyl ethyl ester 4.5g, vinylformic acid 1g, the B component of Viscoat 295 0.5g, mixes A component and B component to obtain E solution.The C component of 2g benzoyl peroxide is dissolved in 8g ethyl acetate, is mixed with F solution.Take contain 60g ethyl acetate, 20g butanone D component as organic solvent.By above-mentioned 1/3 E solution, 1/3 F solution, whole organic solvent, add in the four-hole boiling flask with stirring, reflux, constant pressure funnel.Be warmed up to 70 ℃, after reaction 3h, then drip remaining 2/3 E solution and 2/3 F solution, be controlled in 8h and drip off.Dropwise and be incubated again after 3h, cool to 30 ℃ and filter discharging, obtain protective membrane pressure sensitive adhesive of the present invention.In the present embodiment, the quality solid content of the pressure sensitive adhesive making is 55%.
Embodiment 4
Proportionally preparation contains n-butyl acrylate 70g, Isooctyl acrylate monomer 16g, stearyl methacrylate 4g, the A component of vinyl acetate 4g, and contain vinylformic acid-2-hydroxyl ethyl ester 4.5g, vinylformic acid 1g, the B component of Viscoat 295 0.5g, mixes A component and B component to obtain E solution.The C component of 2g benzoyl peroxide is dissolved in 8g ethyl acetate, is mixed with F solution.Take and contain ethyl acetate 300g, butanone 50g, butylacetate 20g, the D component of acetone 30g is as organic solvent.By above-mentioned 1/3 E solution, 1/3 F solution, whole organic solvent, add in the four-hole boiling flask with stirring, reflux, constant pressure funnel.Be warmed up to 70 ℃, after reaction 3h, then drip remaining 2/3 E solution and 2/3 F solution, be controlled in 8h and drip off.Dropwise and be incubated again after 3h, cool to 40 ℃ and filter discharging, obtain protective membrane pressure sensitive adhesive of the present invention.In the present embodiment, the quality solid content of the pressure sensitive adhesive making is 20%.
Embodiment 5
Proportionally preparation contains n-butyl acrylate 65g, Isooctyl acrylate monomer 16g, the A component of stearyl methacrylate 2g, methyl methacrylate 6g, and contain vinylformic acid-2-hydroxyl ethyl ester 9g, the B component of vinylformic acid 1g, mixes A component and B component to obtain E solution.The C component of 1g benzoyl peroxide is dissolved in 4g ethyl acetate, is mixed with F solution.Take and contain ethyl acetate 100g, the D component of butylacetate 50g is as organic solvent.By above-mentioned 1/3 E solution, 1/3 F solution, 2/3 organic solvent, add in the four-hole boiling flask with stirring, reflux, constant pressure funnel.Be warmed up to 85 ℃, after reaction 3h, then drip remaining 2/3 E solution and 2/3 F solution, be controlled in 6h and drip off.Dropwise and be incubated again after 1h, in 10min, drip remaining 1/3 organic solvent in four-hole boiling flask.Be cooled to again 30 ℃ and filter discharging, obtain protective membrane pressure sensitive adhesive of the present invention.In the present embodiment, the quality solid content of the pressure sensitive adhesive making is 40%.
The pressure sensitive adhesive that the present invention also makes above-described embodiment 1 to embodiment 5 has carried out relevant test experiments, and the result of test experiments is as shown in the table:
Preparation method's technique of the single-component polyacrylate pressure-sensitive for optical protection layer of the present invention is simple, settle at one go, and production efficiency is high, cost is low, the pressure sensitive adhesive good stability of preparation.Because, in preparation method of the present invention, modification and synthesizing propylene acid oligomer synchronously carry out, and react more thorough, and molecular weight is unlikely to because very large variation occurs in adding of modified monomer, effectively control the generation of macromolecular substance gel, obtained IPN or crosslinked stable pressure sensitive adhesive product.
Meanwhile, the single-component polyacrylate pressure-sensitive making can be applicable on the optical protection layers such as PET protective membrane, PE film, PVC film or BOPP film, and it is easy to use, and less wastage is easily peeled off, and there will not be the phenomenon of cull, " shadow " after peeling off.And above-mentioned pressure sensitive adhesive is under room temperature 25 degree, its stripping strength < 8gf/25mm; Coating drying adhesive layer 10 μ m, after 150 degree baking 2h, its stripping strength < 12gf/25mm.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, is therefore intended to include in the present invention dropping on the implication that is equal to important document of claim and all changes in scope.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (10)
1. for a preparation method for the single-component polyacrylate pressure-sensitive of optical protection layer, it is characterized in that, described preparation method comprises the steps:
Take and be selected from following compound: the A component of at least one in ethyl propenoate, n-butyl acrylate, isobutyl acrylate, Isooctyl acrylate monomer, stearyl methacrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, n-BMA, vinyl acetate, and be selected from following compound: the B component of at least one in vinylformic acid-2-hydroxyl ethyl ester, 2-hydroxypropyl acrylate, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate, 1,6 hexanediol diacrylate, Viscoat 295, vinylformic acid, methacrylic acid;
A component and B component are mixed and obtain E solution;
The F solution that preparation contains C component, described C component is selected from following compound: at least one in benzoyl peroxide, Diisopropyl azodicarboxylate, tertbutyl peroxide, isopropyl benzene hydroperoxide, methylethyl ketone peroxide, dicumyl peroxide;
Take D component as organic solvent;
Described 1/3 E solution, 1/3 F solution and at least 2/3 organic solvent are placed in to four-hole boiling flask, at temperature 70-85 ℃, after reaction 1-3h, in 4-8h, remaining E solution, F solution are added drop-wise in four-hole boiling flask to insulation, in 10min, remaining organic solvent is added drop-wise in four-hole boiling flask, after cooling, filters and obtain pressure sensitive adhesive.
2. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1; it is characterized in that; described A component is selected from the 2-4 kind in n-butyl acrylate, Isooctyl acrylate monomer, stearyl methacrylate, methyl methacrylate, vinyl acetate, and described A component accounts for the 50-90% of A, B, C component gross weight.
3. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1; it is characterized in that; described B component is selected from vinylformic acid-2-hydroxyl ethyl ester, 1; 1-3 kind in 6-hexanediyl ester, Viscoat 295, vinylformic acid, methacrylic acid, described B component accounts for the 0.1-9.9% of A, B, C component gross weight.
4. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1; it is characterized in that; described F solution is the ethyl acetate solution that contains C component; the ratio of described C component and ethyl acetate is: 1:2-1:4, described C component accounts for the 0.1-2% of A, B, C component gross weight.
5. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1; it is characterized in that; the described D component as organic solvent is selected from following organism: the 1-3 kind in ethyl acetate, butylacetate, acetone, butanone, the proportional range of the gross weight of described D component and A, B, C component is 1:1-1:4.
6. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 5, is characterized in that, in described D component, every kind of organism of choosing accounts for the 30-400% of A, B, C gross weight.
7. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1, is characterized in that, described four-hole boiling flask is with stirring, reflux, and constant pressure funnel.
8. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1, is characterized in that, described soaking time is 1-3h.
9. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1, is characterized in that, described remaining organic solvent is added drop-wise in four-hole boiling flask after, cool to 30-40 ℃.
10. the preparation method of a kind of single-component polyacrylate pressure-sensitive for optical protection layer according to claim 1, is characterized in that, the quality solid content of the pressure sensitive adhesive making is 20-55%.
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Application publication date: 20140416 |