CN102260477A - Pressure-sensitive adhesive for biaxially-oriented polypropylene (BOPP) protective film and preparation method thereof - Google Patents
Pressure-sensitive adhesive for biaxially-oriented polypropylene (BOPP) protective film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a pressure-sensitive adhesive for a biaxially-oriented polypropylene (BOPP) protective film and a preparation method thereof. The pressure-sensitive adhesive comprises the following raw materials in parts by weight: 100 parts of acrylate copolymer A and/or acrylate copolymer B, 0.01-15 parts of crosslinking agent, 0.001-5 parts of silane coupling agent, 0.001-5 parts of plasticizer and 20-45 parts of solvent. The pressure-sensitive adhesive for the BOPP protective film has a strong adaptability to a BOPP base film, has the characteristics of high bonding property, high temperature resistance and the like and can be widely applied to BOPP protective films. The invention also provides a preparation method of the pressure-sensitive adhesive for the BOPP protective film.
Description
Technical field
The present invention relates to a kind of pressure sensitive adhesive and preparation method thereof, relate in particular to a kind of BOPP of being used for protective membrane pressure sensitive adhesive and preparation method thereof.The invention still further relates to BOPP protective membrane that utilizes the pressure sensitive adhesive preparation and preparation method thereof.
Background technology
The BOPP protective membrane is a kind of non-toxic and non-pollution ep-type material, and characteristics such as have the transparency height, glossiness is good, the product planeness is good, brilliant point is little, high temperature resistant, wear-resisting are used for the surface protection of five metals, plastic cement, electronic product more.The BOPP protective membrane is mainly formed through processes such as coating, drying, slakings by BOPP film and pressure sensitive adhesive (pressure sensitive adhesive), and wherein, the quality of pressure sensitive adhesive plays a decisive role to the quality of BOPP protective membrane.Because the surface energy of BOPP film is little, adopt the general pressure sensitive adhesive of being sold on the market, be difficult to moistening its surface.In order to improve its sticking power, at present in the method that adopts, the one, the BOPP film is carried out corona treatment, improve its surface tension, but there are shortcomings such as poor stability, amount of investment are big in this method; The 2nd, the BOPP film is carried out primary coat handle, improve its surface tension, but this method exists shortcomings such as technology is loaded down with trivial details, cost height.
In order to overcome above-mentioned shortcoming, research and develop a kind of cheap, technology is simple, performance is good BOPP protective membrane and the production and the Application Areas of surface protection film had very realistic meanings with pressure sensitive adhesive.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of pressure sensitive adhesive of the BOPP of being used for protective membrane, this pressure sensitive adhesive is a kind of high temperature resistant, pressure sensitive adhesive that binding property is high.
The present invention also aims to provide the preparation method of above-mentioned pressure sensitive adhesive.
For achieving the above object, the invention provides a kind of pressure sensitive adhesive of the BOPP of being used for protective membrane, it has following raw material and forms:
Acrylate copolymer A and/or acrylate copolymer B, 100 weight parts, linking agent, 0.01-15 weight part, silane coupling agent, 0.001-5 weight part, softening agent, 0.001-5 weight part, solvent, 20-45 weight part.
In above-mentioned pressure sensitive adhesive, preferably, the amount of acrylate copolymer A is the 30-100 weight part, and the amount of acrylate copolymer B is the 0-70 weight part; More preferably, the amount of acrylate copolymer A is more than or equal to 30 weight parts, less than 100 weight parts, and the amount of acrylate copolymer B is greater than 0 weight part, smaller or equal to 70 weight parts.
In above-mentioned pressure sensitive adhesive provided by the invention, the molecular weight of described acrylate copolymer A is 250-300 ten thousand, it can be by the second-order transition temperature of 1-20 weight part (methyl) acrylate monomer that is used to prepare homopolymer for-45 ℃ to 10 ℃, the second-order transition temperature of 60-90 weight part is (methyl) acrylate monomer that is used to prepare homopolymer of-90 ℃ to-50 ℃, the Acrylic Acid Monomer with functional group of 1-20 weight part, 0.01-10 the organic solvent copolymerization of the initiator of weight part and 70-100 weight part prepares, and, after preparing, get the raw material of this acrylate copolymer of 30-100 weight part A as pressure sensitive adhesive;
The molecular weight of described acrylate copolymer B is 30-70 ten thousand, it can be by the second-order transition temperature of 5-25 weight part (methyl) acrylate monomer that is used to prepare homopolymer for-45 ℃ to 10 ℃, the second-order transition temperature of 60-90 weight part is (methyl) acrylate monomer that is used to prepare homopolymer of-90 ℃ to-50 ℃, the Acrylic Acid Monomer with functional group of 1-20 weight part, 0.01-10 the organic solvent copolymerization of the initiator of weight part and 70-100 weight part prepares, and, after preparing, get the raw material of this acrylate copolymer of 0-70 weight part B as pressure sensitive adhesive.
Wherein, the functional group that has in the Acrylic Acid Monomer of functional group is preferably the functional group that can be crosslinked, and can be hydroxyl, carboxyl, amide group and/or acid anhydrides etc.
In the present invention, (methyl) acrylate monomer is meant methacrylate monomer and acrylate monomer, and this is common literary style, and the compound title of other similar literary styles also all has the above-mentioned similar meaning, enumerates no longer one by one here.
In pressure sensitive adhesive provided by the invention, preferably, described acrylate copolymer A prepares (methyl) acrylate monomer of homopolymer for the second-order transition temperature of (methyl) acrylate monomer that is used to prepare homopolymer of-45 ℃ to 10 ℃, 60-80 weight part for-90 ℃ to-50 ℃ be used to and the Acrylic Acid Monomer copolymerization with functional group of 5-15 weight part prepares by the second-order transition temperature of 5-15 weight part;
Described acrylate copolymer B prepares (methyl) acrylate monomer of homopolymer for the second-order transition temperature of (methyl) acrylate monomer that is used to prepare homopolymer of-45 ℃ to 10 ℃, 70-80 weight part for-90 ℃ to-50 ℃ be used to and the Acrylic Acid Monomer copolymerization with functional group of 5-25 weight part prepares by the second-order transition temperature of 10-20 weight part.
In pressure sensitive adhesive provided by the invention, preferably, the solvent that is adopted comprises one or more in ethyl acetate, toluene, dimethylbenzene and the butanone etc.; The organic solvent that is adopted during the preparation acrylate copolymer comprises one or more in ethyl acetate, butanone, methyl alcohol and the toluene etc.
In acrylate copolymer, (methyl) acrylate monomer that the second-order transition temperature that is adopted prepares homopolymer for-45 ℃ to 10 ℃ be used to can strengthen force of cohesion, but with performances such as the adhesion durability of keeping pressure sensitive adhesive and cuttings; It preferably includes in (methyl) isobutyl acrylate, (methyl) n-butyl acrylate, (methyl) propyl acrylate, (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) vinylformic acid 3-methyl butyl ester, n octyl methacrylate and the methacrylic acid n-tetradecane base ester etc. one or more.
In acrylate copolymer, (methyl) acrylate monomer that the second-order transition temperature that is adopted prepares homopolymer for-90 ℃ to-50 ℃ be used to can increase the polymkeric substance chain flexibility, thereby gives prepared pressure sensitive adhesive with voltage-dependent characteristic; It preferably includes in (methyl) vinylformic acid pentyl ester, (methyl) 2-EHA, methacrylic acid ester in the positive last of the ten Heavenly stems, (methyl) vinylformic acid 2-ethyl butyl ester, (methyl) Ethyl acrylate, (methyl) vinylformic acid n-octyl, (methyl) vinylformic acid heptyl ester, (methyl) vinylformic acid ester in the ninth of the ten Heavenly Stems and the methacrylic acid dodecyl ester etc. one or more.
In acrylate copolymer, acrylate monomer can improve the force of cohesion of polymkeric substance, thereby improve the performance of pressure sensitive adhesive by providing cohesive force with the linking agent reaction.Acrylic Acid Monomer of the present invention can be independent a kind of Acrylic Acid Monomer, it also can be the mixture of multiple Acrylic Acid Monomer, preferably, Acrylic Acid Monomer with functional group of the present invention comprises that the 0.3-5 weight part has the Acrylic Acid Monomer of hydroxyl, 0.2-4 have the Acrylic Acid Monomer of epoxy group(ing) and the Acrylic Acid Monomer that 0.5-1 has carboxyl, more preferably, above-mentioned Acrylic Acid Monomer with hydroxyl can comprise (methyl) vinylformic acid 2-hydroxyl ethyl ester, in (methyl) vinylformic acid 2-hydroxypropyl acrylate and (methyl) vinylformic acid 2-hydroxyl glycol ester etc. one or more, above-mentioned Acrylic Acid Monomer with epoxy group(ing) can be (methyl) acrylic acid epoxy propyl ester, and above-mentioned Acrylic Acid Monomer with carboxyl can comprise (methyl) vinylformic acid, in toxilic acid and the maleic anhydride etc. one or more.By adopting the combination of multiple Acrylic Acid Monomer, can improve the adaptability of BOPP film greatly, and can reduce production cost of products.
In pressure sensitive adhesive provided by the invention, linking agent can with functional group reactions among acrylate copolymer A and the B to increase the force of cohesion of pressure sensitive adhesive; The linking agent that is adopted preferably includes isocyanic ester, epoxy compounds, nitrogen third is stung with metallo-chelate etc. in one or more, wherein, be good with isocyanic ester.Particularly, above-mentioned isocyanic ester can comprise one or more in toluene-2,4-diisocyanate, xylene diisocyanate, two isocyanic acid phenylbenzene methyl esters, two isocyanic acids, six methylene esters, isomery vulcabond and the two isocyanic acid tetramethyl xylene esters etc.; Above-mentioned epoxy compounds can comprise one or more in ethylene glycol diglycidylether, triglycidyl ether and the trihydroxymethylpropanyltri diglycidyl ether etc.; Above-mentioned nitrogen third is stung and can be comprised N, and N '-Toluene-2,4-diisocyanate .4-two (1-nitrogen third is stung carbonyl), N, N '-ditan-4,4 '-two (1-nitrogen third is stung carbonyl), triethylene trimeric cyanamide and oxidation three-1-a word used for translation third sting one or more in basic phosphine etc.; Above-mentioned metallo-chelate can comprise one or more in polyvalent metals such as aluminium, iron, tin, titanium, antimony, magnesium or vanadium and the coordinate compounds such as methyl ethyl diketone or ethylacetoacetone(EAA,HEAA).
In pressure sensitive adhesive provided by the invention, the initiator that is adopted is preferably dibenzoyl peroxide and/or Diisopropyl azodicarboxylate etc.
In pressure sensitive adhesive provided by the invention, silane coupling agent can improve the adhesion stability and the resistance toheat of pressure sensitive adhesive.Silane coupling agent of the present invention preferably includes one or more in vinyltrimethoxy silane, vinyltriethoxysilane, γ-glycidyl ether propyl trimethoxy silicane and the γ-methacryloxypropyl trimethoxy silane etc.
In pressure sensitive adhesive provided by the invention, softening agent can improve acrylic acid flowability, improves the bounding force of pressure sensitive adhesive and BOPP base material.Softening agent of the present invention preferably includes one or more in dioctyl sebacate, dioctyl terephthalate, tributyl citrate, tributyl acetylcitrate and the tributyl phosphate etc.
The present invention also provides the preparation method of the pressure sensitive adhesive of the above-mentioned BOPP of being used for protective membrane, and it may further comprise the steps:
Step 1: preparation acrylate copolymer A
The second-order transition temperature of 1-10 weight part is put into reactor for (methyl) acrylate monomer that is used for preparing homopolymer of-45 ℃ to 10 ℃, the second-order transition temperature of 10-30 weight part for-90 ℃ to-50 ℃ (methyl) acrylate monomer that is used to prepare homopolymer, the initiator of 0.01-0.5 weight part and the organic solvent of 20-40 weight part, be heated to 60-80 ℃ and insulation reaction 10-60 minute;
Remaining second-order transition temperature is prepared mixed being incorporated in of (methyl) acrylate monomer of homopolymer, the Acrylic Acid Monomer with functional group, initiator and organic solvent and is added drop-wise to reactor in 1-3 hour for-90 ℃ to-50 ℃ be used to for (methyl) acrylate monomer that is used for preparing homopolymer of-45 ℃ to 10 ℃, second-order transition temperature, be heated to 60-70 ℃ and insulation reaction 2-5 hour then, obtain acrylate copolymer A;
Step 2: preparation acrylate copolymer B
The second-order transition temperature of 5-25 weight part is put into reactor for (methyl) acrylate monomer that is used for preparing homopolymer of-45 ℃ to 10 ℃, the second-order transition temperature of 60-90 weight part for-90 ℃ to-50 ℃ (methyl) acrylate monomer that is used to prepare homopolymer, the Acrylic Acid Monomer with functional group of 1-20 weight part, the initiator of 0.005-0.5 weight part and the organic solvent of 40-60 weight part, be heated to 60-80 ℃ and insulation reaction 10-60 minute;
With remaining initiator and solvent and in 0.5-1 hour, be added drop-wise in the reactor, be heated to 60-70 ℃ and insulation reaction 2-5 hour then, obtain acrylate copolymer B;
Step 3: mix and stir
30-100 parts by weight of acrylic ester copolymer A and 0-70 parts by weight of acrylic ester copolymer B are mixed; obtain the mixture of 100 parts by weight of acrylic ester copolymer A and acrylate copolymer B; again the softening agent of the silane coupling agent of 0.001-5 weight part and 0.001-5 weight part being put into reactor mixes; when stirring, add the solvent and the 0.01-15 parts by weight of cross-linking agent of 20-40 weight part, obtain the pressure sensitive adhesive of the described BOPP of being used for protective membrane.
The present invention also provides a kind of BOPP protective membrane, and it is made up of BOPP film and the pressure-sensitive adhesive layer that is coated on the described BOPP film, and wherein, described pressure-sensitive adhesive layer is to be made by the pressure sensitive adhesive of the BOPP of being used for protective membrane provided by the invention.
The present invention also provides the preparation method of above-mentioned BOPP protective membrane, and it may further comprise the steps:
Adopt 50-70 purpose coating roll, the pressure sensitive adhesive of the BOPP of being used for protective membrane provided by the invention is applied to the surface of BOPP film, be heated to 80-100 ℃ of dry 0.5-1 minute in the mode of scraper coating;
After drying is finished,, form pressure-sensitive adhesive layer, obtain the BOPP protective membrane 50 ℃ of slakings 24 hours.
The preparation method of above-mentioned BOPP protective membrane provided by the invention only is the preferred embodiment among the various preparation methods of this protective membrane; those skilled in the art can expect carrying out according to other ordinary methods of this area the preparation of BOPP protective membrane, perhaps according to routine operation, parameter the preparation method of BOPP protective membrane are adjusted.
The pressure sensitive adhesive that is used for the BOPP protective membrane provided by the invention is strong to the adaptability of BOPP basement membrane, has high characteristics such as bonding, high temperature resistant, can widespread use in the BOPP protective membrane.
Embodiment
Understand for technical characterictic of the present invention, purpose and beneficial effect being had more clearly, existing technical scheme of the present invention is carried out following detailed description, but but can not be interpreted as qualification practical range of the present invention.
Embodiment 1
Present embodiment provides pressure sensitive adhesive of a kind of BOPP of being used for protective membrane and preparation method thereof, and wherein, the raw material of pressure sensitive adhesive is formed as shown in table 1.
Table 1
| Feed composition | Weight (kg) |
| Acrylate copolymer A | 10 |
| Acrylate copolymer B | 20 |
| Ethyl acetate | 7 |
| Vinyltriethoxysilane | 0.005 |
| Tributyl acetylcitrate | 0.005 |
| Toluene-2,4-diisocyanate | 0.7 |
The preparation method of the pressure sensitive adhesive that present embodiment provides is as follows:
Step 1, preparation acrylate copolymer A
1): 3 kilograms of 2-EHAs, 4 kilograms of butyl acrylates, 2 kilograms of methyl methacrylates, 7 kilograms of ethyl acetate and 0.03 kilogram of dibenzoyl peroxide are joined in the reactor, be heated to 70 ℃ of insulation reaction 30 minutes;
2): 6 kilograms of 2-EHAs, 8 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 1.2 kilograms of vinylformic acid 2-hydroxyl ethyl esters, 0.6 kilogram of toxilic acid, 2 kilograms of acrylic acid epoxy propyl ester, 14 kilograms of ethyl acetate and 0.05 kilogram of dibenzoyl peroxide are mixed; in 2 hours, be added drop-wise in the aforesaid reaction vessel in the mode that drips; after being added dropwise to complete; be heated to 65 ℃; and when stirring insulation reaction 3 hours, obtain acrylate copolymer A.
Step 2, preparation acrylate copolymer B
1): with 10 kilograms of 2-EHAs, 4 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 3 kilograms of methacrylic acid 2-hydroxyl ethyl esters, 0.5 kilogram of vinylformic acid, 1 kilogram of acrylic acid epoxy propyl ester, 10 kilograms of ethyl acetate and 0.03 kilogram of Diisopropyl azodicarboxylate, join in the reactor, be heated to 68 ℃ of insulation reaction 30 minutes;
2): 2 kilograms of ethyl acetate and 0.05 kilogram of Diisopropyl azodicarboxylate are mixed, in 1 hour, be added drop-wise in the aforesaid reaction vessel in the mode that drips, after being added dropwise to complete, be heated to 67 ℃, and when stirring insulation reaction 3 hours, obtain acrylate copolymer B.
Step 3, mix
10 kilograms of acrylate copolymer A, 20 kilograms of acrylate copolymer B, 0.005 kilogram of vinyltriethoxysilane, 0.005 kilogram of tributyl acetylcitrate and 7 kilograms of ethyl acetate are joined in the reactor, mix, add 0.7 kilogram of toluene-2,4-diisocyanate again, stir, obtain the pressure sensitive adhesive of present embodiment.
The preparation method of BOPP protective membrane:
Adopt 70 order coating rolls, above-mentioned pressure sensitive adhesive is applied to the surface of the thick BOPP film of 50 μ m, be heated to 100 ℃ of dryings 1 minute in the mode of scraper coating; rolling; slaking 24 hours in 50 ℃ curing chamber then, forming thickness is the pressure-sensitive adhesive layer of 10 μ m, obtains the BOPP protective membrane.
Embodiment 2
Present embodiment provides pressure sensitive adhesive of a kind of BOPP of being used for protective membrane and preparation method thereof, and wherein, the raw material of pressure sensitive adhesive is formed as shown in table 2.
Table 2
| Feed composition | Weight (kg) |
| Acrylate copolymer A | 10 |
| Acrylate copolymer B | 24 |
| Ethyl acetate | 10 |
| Vinyltriethoxysilane | 0.006 |
| Tributyl acetylcitrate | 0.007 |
| Toluene-2,4-diisocyanate | 0.5 |
The preparation method of the pressure sensitive adhesive that present embodiment provides is as follows:
Step 1, preparation acrylate copolymer A:
1): 4 kilograms of 2-EHAs, 3 kilograms of butyl acrylates, 2 kilograms of methyl methacrylates, 7 kilograms of ethyl acetate and 0.03 kilogram of dibenzoyl peroxide are joined in the reactor, be heated to 72 ℃ of insulation reaction 20 minutes;
2): 8 kilograms of 2-EHAs, 6 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 3 kilograms of methacrylic acid 2-hydroxyl ethyl esters, 1 kilogram of vinylformic acid, 1 kilogram of acrylic acid epoxy propyl ester, 14 kilograms of ethyl acetate and 0.05 kilogram of dibenzoyl peroxide are mixed; in 2 hours, be added drop-wise in the reactor in the mode that drips; after being added dropwise to complete; be heated to 67 ℃; and when stirring insulation reaction 3 hours, obtain acrylate copolymer A.
Step 2, preparation acrylate copolymer B
1): with 7 kilograms of 2-EHAs, 8 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 1.2 kilograms of vinylformic acid 2-hydroxyl ethyl esters, 0.6 kilogram of toxilic acid, 2 kilograms of acrylic acid epoxy propyl ester, 10 kilograms of ethyl acetate and 0.04 kilogram of Diisopropyl azodicarboxylate, join in the reactor, be heated to 68 ℃ of insulation reaction 30 minutes;
2): 4 kilograms of ethyl acetate and 0.06 kilogram of Diisopropyl azodicarboxylate are mixed, be added drop-wise in the aforesaid reaction vessel in 30 minutes in the mode that drips, after being added dropwise to complete, be heated to 64 ℃, and when stirring insulation reaction 4 hours, obtain acrylate copolymer B.
Step 3, mix
10 kilograms of acrylate copolymer A, 24 kilograms of acrylate copolymer B, 0.006 kilogram of vinyltriethoxysilane, 0.007 kilogram of tributyl acetylcitrate and 10 kilograms of ethyl acetate are joined in the reactor, mix, add 0.5 kilogram of toluene-2,4-diisocyanate again, stir, obtain the pressure sensitive adhesive of present embodiment.
The preparation method of BOPP protective membrane:
Adopt 70 order coating rolls, above-mentioned pressure sensitive adhesive is applied to the surface of the thick BOPP film of 50 μ m, be heated to 100 ℃ of dryings 1 minute in the mode of scraper coating; rolling; slaking 24 hours in 50 ℃ curing chamber then, forming thickness is the pressure-sensitive adhesive layer of 10 μ m, obtains the BOPP protective membrane.
Embodiment 3
Present embodiment provides a kind of pressure sensitive adhesive and preparation method of the BOPP of being used for protective membrane, and wherein, the raw material of pressure sensitive adhesive is formed as shown in table 3.
Table 3
| Feed composition | Weight (kg) |
| Acrylate copolymer A | 10 |
| Acrylate copolymer B | 20 |
| Ethyl acetate | 10 |
| Vinyltriethoxysilane | 0.006 |
| Tributyl acetylcitrate | 0.007 |
| Xylene diisocyanate | 0.3 |
The preparation method of the pressure sensitive adhesive that present embodiment provides is as follows:
Step 1, preparation acrylate copolymer A:
1): 4 kilograms of 2-EHAs, 3 kilograms of butyl acrylates, 2 kilograms of methyl methacrylates, 7 kilograms of ethyl acetate and 0.03 kilogram of dibenzoyl peroxide are joined in the reactor, be heated to 72 ℃ of insulation reaction 20 minutes;
2): 8 kilograms of 2-EHAs, 6 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 3 kilograms of vinylformic acid 2-hydroxy methacrylates, 1.5 kilograms of vinylformic acid, 3 kilograms of acrylic acid epoxy propyl ester, 14 kilograms of ethyl acetate and 0.05 kilogram of dibenzoyl peroxide are mixed; in 2 hours, be added drop-wise in the reactor in the mode that drips; after being added dropwise to complete; be heated to 70 ℃; and when stirring insulation reaction 3 hours, obtain acrylate copolymer A.
Step 2, preparation acrylate copolymer B:
1): with 7 kilograms of 2-EHAs, 8 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 1 kilogram of methacrylic acid-2 hydroxy methacrylate, 0.6 kilogram of vinylformic acid, 3 kilograms of acrylic acid epoxy propyl ester, 10 kilograms of ethyl acetate and 0.04 kilogram of Diisopropyl azodicarboxylate, join in the reactor, be heated to 70 ℃ of insulation reaction 30 minutes;
2): 4 kilograms of ethyl acetate and 0.06 kilogram of Diisopropyl azodicarboxylate are mixed, be added drop-wise in the aforesaid reaction vessel in 35 minutes in the mode that drips, after being added dropwise to complete, be heated to 69 ℃, and when stirring insulation reaction 4 hours, obtain acrylate copolymer B.
Step 3, mix
At last, 10 kilograms of acrylate copolymer A, 20 kilograms of acrylate copolymer B, 0.006 kilogram of vinyltriethoxysilane, 0.007 kilogram of tributyl acetylcitrate and 10 kilograms of ethyl acetate are joined in the reactor, mix, add 0.6 kilogram of xylene diisocyanate again, stir, obtain the pressure sensitive adhesive of present embodiment.
The preparation method of BOPP protective membrane:
Adopt 70 order coating rolls, above-mentioned pressure sensitive adhesive is applied to the surface of the thick BOPP film of 50 μ m, be heated to 100 ℃ of dryings 1 minute in the mode of scraper coating; rolling; slaking 24 hours in 50 ℃ curing chamber then, forming thickness is the pressure-sensitive adhesive layer of 10 μ m, obtains the BOPP protective membrane.
Embodiment 4
Present embodiment provides pressure sensitive adhesive of a kind of BOPP of being used for protective membrane and preparation method thereof, and wherein, the raw material of pressure sensitive adhesive is formed as shown in table 4.
Table 4
| Feed composition | Weight (kg) |
| Acrylate copolymer A | 10 |
| Acrylate copolymer B | 25 |
| Ethyl acetate | 15 |
| Vinyltriethoxysilane | 0.005 |
| Tributyl acetylcitrate | 0.005 |
| Toluene-2,4-diisocyanate | 1 |
The preparation method of the pressure sensitive adhesive that present embodiment provides is as follows:
Step 1, preparation acrylate copolymer A
1): 4 kilograms of 2-EHAs, 3 kilograms of butyl acrylates, 2 kilograms of methyl methacrylates, 7 kilograms of ethyl acetate and 0.03 kilogram of dibenzoyl peroxide are joined in the reactor, be heated to 68 ℃ of insulation reaction 20 minutes;
2): 8 kilograms of 2-EHAs, 6 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 1 kilogram of methacrylic acid-2 hydroxy methacrylate, 2 kilograms of vinylformic acid, 2 kilograms of acrylic acid epoxy propyl ester, 14 kilograms of ethyl acetate and 0.05 kilogram of dibenzoyl peroxide are mixed; in 2 hours, be added drop-wise in the reactor in the mode that drips; after being added dropwise to complete; be heated to 65 ℃; and when stirring insulation reaction 3 hours, obtain acrylate copolymer A.
Step 2, preparation acrylate copolymer B
1): with 7 kilograms of 2-EHAs, 8 kilograms of butyl acrylates, 4 kilograms of methyl methacrylates, 3 kilograms of vinylformic acid 2-hydroxy methacrylates, 0.5 kilogram of vinylformic acid, 3 kilograms of acrylic acid epoxy propyl ester, 10 kilograms of ethyl acetate and 0.04 kilogram of Diisopropyl azodicarboxylate, join in the reactor, be heated to 70 ℃ of insulation reaction 30 minutes;
2): 4 kilograms of ethyl acetate and 0.06 kilogram of Diisopropyl azodicarboxylate are mixed, in 1 hour, be added drop-wise in the aforesaid reaction vessel in the mode that drips, after being added dropwise to complete, be heated to 67 ℃, and when stirring insulation reaction 4 hours, obtain acrylate copolymer B.
Step 3, mix
10 kilograms of acrylate copolymer A, 25 kilograms of acrylate copolymer B, 0.005 kilogram of vinyltriethoxysilane, 0.005 kilogram of tributyl acetylcitrate and 15 kilograms of ethyl acetate are joined in the reactor, mix, add 1 kilogram of toluene-2,4-diisocyanate again, stir, obtain the pressure sensitive adhesive of present embodiment.
The preparation method of BOPP protective membrane:
Adopt 70 order coating rolls, above-mentioned pressure sensitive adhesive is applied to the surface of the thick BOPP film of 50 μ m, be heated to 100 ℃ of dryings 1 minute in the mode of scraper coating; rolling; slaking 24 hours in 50 ℃ curing chamber then, forming thickness is the pressure-sensitive adhesive layer of 10 μ m, obtains the BOPP protective membrane.
Embodiment 5
Present embodiment provides pressure sensitive adhesive of a kind of BOPP of being used for protective membrane and preparation method thereof, and wherein, the raw material of pressure sensitive adhesive is formed as shown in table 5.
Table 5
| Feed composition | Weight (kg) |
| Acrylate copolymer A | 10 |
| Acrylate copolymer B | 20 |
| Ethyl acetate | 10 |
| Vinyltriethoxysilane | 0.005 |
| Tributyl acetylcitrate | 0.005 |
| N, N '-ditan-4,4 '-two (1-nitrogen third is stung carbonyl) | 1 |
The preparation method of the pressure sensitive adhesive that present embodiment provides is as follows:
Step 1, preparation acrylate copolymer A
1): 3 kilograms of 2-EHAs, 3 kilograms of butyl acrylates, 2 kilograms of methyl methacrylates, 7 kilograms of ethyl acetate and 0.03 kilogram of dibenzoyl peroxide are joined in the reactor, be heated to 72 ℃ of insulation reaction 10 minutes;
2): 7 kilograms of 2-EHAs, 8 kilograms of butyl acrylates, 6 kilograms of methyl methacrylates, 4 kilograms of 2-hydroxyethyl methacrylates, 1.5 kilograms of vinylformic acid, 2 kilograms of acrylic acid epoxy propyl ester, 21 kilograms of ethyl acetate and 0.07 kilogram of dibenzoyl peroxide are mixed; in 3 hours, be added drop-wise in the reactor in the mode that drips; after being added dropwise to complete; be heated to 70 ℃; and when stirring insulation reaction 2 hours, obtain acrylate copolymer A.
Step 2, preparation acrylate copolymer B
1): with 9 kilograms of 2-EHAs, 6 kilograms of butyl acrylates, 7 kilograms of methyl methacrylates, 3 kilograms of 2-hydroxyethyl methacrylates, 0.6 kilogram of vinylformic acid, 2 kilograms of acrylic acid epoxy propyl ester, 10 kilograms of ethyl acetate and 0.04 kilogram of Diisopropyl azodicarboxylate, join in the reactor, be heated to 69 ℃ of insulation reaction 30 minutes;
2): 4 kilograms of ethyl acetate and 0.06 kilogram of Diisopropyl azodicarboxylate are mixed, be added drop-wise in the aforesaid reaction vessel in 40 minutes in the mode that drips, after being added dropwise to complete, be heated to 69 ℃, and when stirring insulation reaction 4 hours, obtain acrylate copolymer B.
Step 3, mix
10 kilograms of acrylate copolymer A, 20 kilograms of acrylate copolymer B, 0.005 kilogram of vinyltriethoxysilane, 0.005 kilogram of tributyl acetylcitrate and 10 kilograms of ethyl acetate are joined in the reactor, mix, add 1 kilogram of N again, N '-ditan-4,4 '-two (1-nitrogen third is stung carbonyl), stir, obtain the pressure sensitive adhesive of present embodiment.
The preparation method of BOPP protective membrane:
Adopt 70 order coating rolls, above-mentioned pressure sensitive adhesive is applied to the surface of the thick BOPP film of 50 μ m, be heated to 100 ℃ of dryings 1 minute in the mode of scraper coating; rolling; slaking 24 hours in 50 ℃ curing chamber then, forming thickness is the pressure-sensitive adhesive layer of 10 μ m, obtains the BOPP protective membrane.
Comparative Examples 1
This Comparative Examples provides a kind of BOPP protective membrane, and wherein, the 005B type PE protective membrane of producing with commercially available Kailanda Industry Co., Ltd., Shanghai prepares pressure-sensitive adhesive layer with high bonding pressure sensitive adhesive at the BOPP film surface, and its preparation method is as follows:
Adopt 70 order coating rolls, above-mentioned glue is applied to the surface of the thick BOPP film of 50 μ m, be heated to 100 ℃ of dryings 1 minute in the mode of scraper coating; rolling; slaking 24 hours in 50 ℃ curing chamber then, forming thickness is the pressure-sensitive adhesive layer of 10 μ m, obtains the BOPP protective membrane.
Comparative Examples 2
This Comparative Examples provides a kind of BOPP protective membrane, and wherein, the 007B type PVC protective membrane of producing with commercially available Kailanda Industry Co., Ltd., Shanghai prepares pressure-sensitive adhesive layer with high bonding pressure sensitive adhesive at the BOPP film surface, and its preparation method is as follows:
Adopt 70 order coating rolls, above-mentioned glue is applied to the surface of the thick BOPP film of 50 μ m, be heated to 100 ℃ of dryings 1 minute in the mode of scraper coating; rolling; slaking 24 hours in 50 ℃ curing chamber then, forming thickness is the pressure-sensitive adhesive layer of 10 μ m, obtains the BOPP protective membrane.
Performance test:
The performance of the BOPP protective membrane that embodiment 1-5 and Comparative Examples 1-2 are provided detects in accordance with the following methods, and test result is as shown in table 6:
180 ° of peel strength tests: test according to GB2792-81;
Resistance to elevated temperatures test: it is on 10 the stainless steel plate that protective membrane is attached to surfaceness; placing temperature then is in 80 ℃ the baking oven aging 12 hours, takes out steel plate, is cooled to room temperature naturally; test 180 ° of stripping strengths, and observe on the steel plate whether cull or offset printing are arranged.
Table 6 The performance test results
From test result as can be seen; the BOPP protective membrane that utilizes pressure sensitive adhesive provided by the invention to make has higher stripping strength and higher resistance to elevated temperatures; this explanation, pressure sensitive adhesive provided by the invention has high adherence, resistance to elevated temperatures, is fit to be used as BOPP protective membrane pressure sensitive adhesive.As can be seen, the BOPP protective membrane substitutes with high bonding pressure sensitive adhesive with PE and the PVC protective membrane that pressure sensitive adhesive can not adopt on the market to be sold from the The performance test results of Comparative Examples 1 and 2.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is specific embodiments of the invention; and be not intended to limit the scope of the invention; within the spirit and principles in the present invention all, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. pressure sensitive adhesive that is used for the BOPP protective membrane, it has following raw material and forms:
Acrylate copolymer A and/or acrylate copolymer B, 100 weight parts, linking agent, 0.01-15 weight part, silane coupling agent, 0.001-5 weight part, softening agent, 0.001-5 weight part, solvent, 20-45 weight part;
The molecular weight of described acrylate copolymer A is 250-300 ten thousand, it is by the second-order transition temperature of 1-20 weight part (methyl) acrylate monomer that is used to prepare homopolymer for-45 ℃ to 10 ℃, the second-order transition temperature of 60-90 weight part is (methyl) acrylate monomer that is used to prepare homopolymer of-90 ℃ to-50 ℃, the Acrylic Acid Monomer with functional group of 1-20 weight part, 0.01-10 the organic solvent copolymerization of the initiator of weight part and 70-100 weight part prepares, and, after preparing, get the raw material of this acrylate copolymer of 30-100 weight part A as pressure sensitive adhesive;
The molecular weight of described acrylate copolymer B is 30-70 ten thousand, it is by the second-order transition temperature of 5-25 weight part (methyl) acrylate monomer that is used to prepare homopolymer for-45 ℃ to 10 ℃, the second-order transition temperature of 60-90 weight part is (methyl) acrylate monomer that is used to prepare homopolymer of-90 ℃ to-50 ℃, the Acrylic Acid Monomer with functional group of 1-20 weight part, 0.01-10 the organic solvent copolymerization of the initiator of weight part and 70-100 weight part prepares, and, after preparing, get the raw material of this acrylate copolymer of 0-70 weight part B as pressure sensitive adhesive.
2. pressure sensitive adhesive as claimed in claim 1, wherein, described solvent comprises one or more in ethyl acetate, toluene, dimethylbenzene and the butanone; Described organic solvent comprises one or more in ethyl acetate, butanone, methyl alcohol and the toluene.
3. pressure sensitive adhesive as claimed in claim 1 or 2, wherein, described second-order transition temperature (methyl) acrylate monomer of preparing homopolymer for-45 ℃ to 10 ℃ be used for comprises one or more of (methyl) isobutyl acrylate, (methyl) n-butyl acrylate, (methyl) propyl acrylate, (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) vinylformic acid 3-methyl butyl ester, n octyl methacrylate and methacrylic acid n-tetradecane base ester;
(methyl) acrylate monomer that described second-order transition temperature prepares homopolymer for-90 ℃ to-50 ℃ be used for comprises one or more of (methyl) vinylformic acid pentyl ester, (methyl) 2-EHA, methacrylic acid ester in the positive last of the ten Heavenly stems, (methyl) vinylformic acid 2-ethyl butyl ester, (methyl) Ethyl acrylate, (methyl) vinylformic acid n-octyl, (methyl) vinylformic acid heptyl ester, (methyl) vinylformic acid ester in the ninth of the ten Heavenly Stems and methacrylic acid dodecyl ester;
Described Acrylic Acid Monomer composition with functional group comprises that the 0.3-5 weight part has the Acrylic Acid Monomer of hydroxyl, 0.2-10 have the Acrylic Acid Monomer of epoxy group(ing) and the Acrylic Acid Monomer that 0.5-5 has carboxyl, wherein, described Acrylic Acid Monomer with hydroxyl comprises (methyl) vinylformic acid 2-hydroxyl ethyl ester, in (methyl) vinylformic acid 2-hydroxypropyl acrylate and (methyl) vinylformic acid 2-hydroxyl glycol ester one or more, described Acrylic Acid Monomer with epoxy group(ing) is (methyl) acrylic acid epoxy propyl ester, and described Acrylic Acid Monomer with carboxyl comprises (methyl) vinylformic acid, in toxilic acid and the maleic anhydride one or more.
4. pressure sensitive adhesive as claimed in claim 1 or 2, wherein, described linking agent comprise isocyanic ester, epoxy compounds, nitrogen third sting with metallo-chelate in one or more; Described isocyanic ester comprises one or more in toluene-2,4-diisocyanate, xylene diisocyanate, two isocyanic acid phenylbenzene methyl esters, two isocyanic acids, six methylene esters, isomery vulcabond and the two isocyanic acid tetramethyl xylene esters;
Described epoxy compounds comprises one or more in ethylene glycol diglycidylether, triglycidyl ether and the trihydroxymethylpropanyltri diglycidyl ether;
Described nitrogen third is stung and is comprised N, N '-Toluene-2,4-diisocyanate .4-two (1-nitrogen third is stung carbonyl), N, and N '-ditan-4,4 '-two (1-nitrogen third is stung carbonyl), triethylene trimeric cyanamide and oxidation three-1-a word used for translation third are stung one or more in the basic phosphine;
Described metallo-chelate comprises one or more in aluminium, iron, tin, titanium, antimony, magnesium or vanadium and methyl ethyl diketone or the ethylacetoacetone(EAA,HEAA) coordinate compound.
5. pressure sensitive adhesive as claimed in claim 1 or 2, wherein, described initiator is dibenzoyl peroxide and/or Diisopropyl azodicarboxylate.
6. pressure sensitive adhesive as claimed in claim 1 or 2, wherein, described silane coupling agent comprises one or more in vinyltrimethoxy silane, vinyltriethoxysilane, γ-glycidyl ether propyl trimethoxy silicane and the γ-methacryloxypropyl trimethoxy silane.
7. pressure sensitive adhesive as claimed in claim 1 or 2, wherein, described softening agent comprises one or more in dioctyl sebacate, dioctyl terephthalate, tributyl citrate, tributyl acetylcitrate and the tributyl phosphate.
8. each described preparation method who is used for the pressure sensitive adhesive of BOPP protective membrane of claim 1-7, it may further comprise the steps:
Step 1: preparation acrylate copolymer A
The second-order transition temperature of 1-10 weight part is put into reactor for (methyl) acrylate monomer that is used for preparing homopolymer of-45 ℃ to 10 ℃, the second-order transition temperature of 10-30 weight part for-90 ℃ to-50 ℃ (methyl) acrylate monomer that is used to prepare homopolymer, the initiator of 0.01-0.5 weight part and the organic solvent of 20-40 weight part, be heated to 60-80 ℃ and insulation reaction 10-60 minute;
Remaining second-order transition temperature is prepared mixed being incorporated in of (methyl) acrylate monomer of homopolymer, the Acrylic Acid Monomer with functional group, initiator and organic solvent and is added drop-wise to reactor in 1-3 hour for-90 ℃ to-50 ℃ be used to for (methyl) acrylate monomer that is used for preparing homopolymer of-45 ℃ to 10 ℃, second-order transition temperature, be heated to 60-70 ℃ and insulation reaction 2-5 hour then, obtain acrylate copolymer A;
Step 2: preparation acrylate copolymer B
The second-order transition temperature of 5-25 weight part is put into reactor for (methyl) acrylate monomer that is used for preparing homopolymer of-45 ℃ to 10 ℃, the second-order transition temperature of 60-90 weight part for-90 ℃ to-50 ℃ (methyl) acrylate monomer that is used to prepare homopolymer, the Acrylic Acid Monomer with functional group of 1-20 weight part, the initiator of 0.005-0.5 weight part and the organic solvent of 40-60 weight part, be heated to 60-80 ℃ and insulation reaction 10-60 minute;
With remaining initiator and solvent and in 0.5-1 hour, be added drop-wise in the reactor, be heated to 60-70 ℃ and insulation reaction 2-5 hour then, obtain acrylate copolymer B;
Step 3: mix and stir
30-100 parts by weight of acrylic ester copolymer A and 0-70 parts by weight of acrylic ester copolymer B are mixed; obtain the mixture of 100 parts by weight of acrylic ester copolymer A and acrylate copolymer B; again the softening agent of the silane coupling agent of 0.001-5 weight part and 0.001-5 weight part being put into reactor mixes; when stirring, add the solvent and the 0.01-15 parts by weight of cross-linking agent of 20-40 weight part, obtain the pressure sensitive adhesive of the described BOPP of being used for protective membrane.
9. BOPP protective membrane, it is made up of BOPP film and the pressure-sensitive adhesive layer that is coated on the described BOPP film, and wherein, described pressure-sensitive adhesive layer is to be made by the pressure sensitive adhesive of each the described BOPP of being used for protective membrane of claim 1-7.
10. the preparation method of the described BOPP protective membrane of claim 9, it may further comprise the steps:
Adopt 50-70 purpose coating roll, the pressure sensitive adhesive of each the described BOPP of being used for protective membrane of claim 1-7 is applied to the surface of BOPP film, be heated to 80-100 ℃ of dry 0.5-1 minute in the mode of scraper coating;
After drying is finished,, form pressure-sensitive adhesive layer, obtain described BOPP protective membrane 50 ℃ of slakings 24 hours.
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Inventor after: Jin Qingsong Inventor after: Wang Qing Inventor after: Li Cuan Inventor after: Zhang Xianfeng Inventor after: Jin Chengri Inventor before: Jin Qingsong Inventor before: Wang Qing Inventor before: Li Cuan Inventor before: Zhang Xianfeng Inventor before: Jin Chengri |
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Address after: 201507, Shanghai, Jinshan District Tong Jing Zhen Road, No. 188 Patentee after: Shanghai painted Mstar Technology Ltd Address before: 201507, Shanghai, Jinshan District Town, East Industrial Zone Patentee before: Kailanda Industry Co., Ltd., Shanghai |
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