CN103756603A - Solvent type thermal active acrylate pressure sensitive adhesive and preparation method for solvent type thermal active acrylate pressure sensitive adhesive product - Google Patents

Solvent type thermal active acrylate pressure sensitive adhesive and preparation method for solvent type thermal active acrylate pressure sensitive adhesive product Download PDF

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CN103756603A
CN103756603A CN201410037153.3A CN201410037153A CN103756603A CN 103756603 A CN103756603 A CN 103756603A CN 201410037153 A CN201410037153 A CN 201410037153A CN 103756603 A CN103756603 A CN 103756603A
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sensitive adhesive
pressure sensitive
parts
solvent
thermal active
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CN103756603B (en
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陈晓理
焦桂英
聂锡铭
孔庆媛
葛玲娟
马国申
刘萍
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SHANDONG NORTH MODERN CHEMISTRY INDUSTRY Co Ltd
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SHANDONG NORTH MODERN CHEMISTRY INDUSTRY Co Ltd
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Abstract

The invention belongs to the field of pressure sensitive adhesives and particularly relates to a solvent type thermal active acrylate pressure sensitive adhesive and a preparation method for a solvent type thermal active acrylate pressure sensitive adhesive. The pressure sensitive adhesive comprises the following comonomers in parts by weight: 30 to 50 parts of butyl acrylate, 20 to 55 parts of 2-ethylhexyl acrylate, 2 to 4 parts of chloroprene, 25 to 35 parts of methyl methacrylate, 1 to 3 parts of acrylic acid, 1 to 5 parts of ethoxyl acrylate and 0.5 to 3 parts of acrylic glycidyl ether. The solvent type thermal active acrylate pressure sensitive adhesive has the effects that at normal temperature, the solvent type thermal active acrylate pressure sensitive adhesive sticky product has ultralow initial adhesive force and peeling strength; the pressure sensitive adhesive products can be stacked together without release paper, and are not adhered mutually. In the using process, the solvent type thermal active acrylate pressure sensitive adhesive is adhered to other materials at the temperature of 110 DEG C to 120 DEG C under the pressurizing condition; the peeling strength is greatly improved; the solvent type thermal active acrylate pressure sensitive adhesive obtains an excellent pressure sensitive adhesive property, can be repeatedly adhered at the temperature of 110 DEG C to 120 DEG C, has reversibility and is not influenced on the aspect of use performance.

Description

The preparation method of solvent-based thermal active crylic acid ester pressure-sensitive and goods thereof
Technical field
The invention belongs to pressure sensitive adhesive field, refer more particularly to the preparation method of solvent-based thermal active crylic acid ester pressure-sensitive and goods thereof.
Background technology
Existing solvent-type acrylic ester pressure-sensitive preparation, or when synthetic, add cross-linking monomer to improve cohesive strength, as " the synthesizing of cross-linked acrylic acid ester pressure-sensitive " of Li Ming research, expense Yongcheng adopts self-crosslinking N hydroxymethyl acrylamide polymerization technique to synthesize " solvent-type acrylic pressure sensitive adhesive ", or after synthetic type acrylate pressure-sensitive adhesive, add linking agent or tackifying resin: in patent 201010246332 " transparent polyester film door sticker of high-temperature-resistant microwave oven acrylate solvent-based pressure sensitive adhersive ", to adopt to add terpolycyantoamino-formaldehyde resin as linking agent, the research of Wang Chonggao is " take modified rosin prepare solvent-type acrylic ester pressure-sensitive for tackifying resin ".
After solvent-type acrylic ester pressure-sensitive film forming, under normal temperature, initial bonding strength is large, and initial bonding strength ball number is generally greater than 10# ball, and stripping strength is high, and under normal temperature, stripping strength is greater than 5N/2.5cm.Glued membrane inevitably can have certain pressure-sensitive adhesive to other materials, at the necessary compound one deck interleaving paper of the process of depositing, during use, interleaving paper need be taken off.
Summary of the invention
The object of the present invention is to provide a kind of solvent-based thermal active crylic acid ester pressure-sensitive, this pressure sensitive adhesive does not need interleaving paper just pressure sensitive adhesive goods can be stacked together and not stick together, good pressure-sensitive adhesive performance during use, stripping strength is large, can repeatedly paste.
The present invention also provides the preparation method of above-mentioned pressure sensitive adhesive.
The invention discloses a kind of solvent-based thermal active crylic acid ester pressure-sensitive, the weight part of its comonomer is:
Butyl acrylate: 30~50
Isooctyl acrylate monomer: 20~55
Chloroprene: 2~4
Methyl methacrylate: 25~35
Vinylformic acid: 1~3
Hydroxy ethyl methacrylate: 1~5
Vinylformic acid glycidyl ether: 0.5~3.
The solvent-based thermal active crylic acid ester pressure-sensitive of the invention described above, preferred, also contain weight part and be 2~6 hot active material, described hot active material is selected from least one in stearic amide, hexanediamine carbamate, Zinic stearas and lanolin.
The solvent-based thermal active crylic acid ester pressure-sensitive of the invention described above, preferred: the solvent that adopts following weight part: toluene: 70~100, ethyl acetate: 20~40; Adopt the catalyzer of following weight part: benzoyl peroxide: 0.2~0.4.
The preparation method who the invention also discloses above-mentioned solvent-based thermal active crylic acid ester pressure-sensitive, is characterized in that adopting following steps:
(1) ethyl acetate of total amount 3/4ths and toluene are added in reactor;
(2) vinylformic acid glycidyl ether, chloroprene, butyl acrylate, Isooctyl acrylate monomer, hydroxy ethyl methacrylate, vinylformic acid, methyl methacrylate and initiator B PO are together added with the header tank stirring, and start stirring;
(3) open reactor and stir, and heating, when the temperature in reactor rises to 85 ℃, start to drip mix monomer and initiator by header tank, and keep temperature to be no more than 88 ℃, within 2 hours, dropwise, and be incubated 4 hours at 85 ℃~88 ℃ temperature;
(4) reactive monomer is dissolved in remaining ethyl acetate and toluene, at 90 ℃ of heating and meltings;
(5) temperature of reaction kettle is risen to 95 ℃, the active material after dissolving is added in reactor, after stirring, be cooled to below 45 ℃, filter blowing, obtain solvent-based thermal active crylic acid pressure sensitive adhesive.
Patent solvent-based thermal active crylic acid ester pressure-sensitive of the present invention has adopted monomer chloroprene to carry out copolymerization as linking agent and acrylate monomer in building-up process, has improved force of cohesion and the activity of acrylate pressure-sensitive adhesive.
This patent has adopted following hot active material: stearic amide, hexanediamine carbamate, Zinic stearas and lanolin.Adding of above-mentioned materials reduces the initial bonding strength of solvent-type acrylic ester pressure-sensitive greatly, the open hour of pressure sensitive adhesive have greatly been shortened simultaneously, when heat-activated, can instantaneously paste, solved large, the easy adhesion of solvent-type acrylic pressure sensitive adhesive initial bonding strength, the necessary compound one deck interleaving paper of the process of depositing and the poor problem of high thermal resistance.
What this patent was distinguished to some extent with the preparation method that other solvent-type acrylic ester pressure-sensitive adopts is all polymerization single polymerization monomers to be mixed with initiator and together from header tank, drip.
Technical indicator:
Viscosity: 1000mpa.s~5000 mpa.s;
Solids content: 41%~54%;
Stripping strength (before thermal activation): 0.1N/2.5cm~0.2 N/2.5cm;
Stripping strength (thermal activation is forward and backward): be greater than 12.5 N/2.5cm.
The solvent-based thermal active crylic acid ester pressure-sensitive being made by this method has the quick cementability of good hot pressing to urethane, polyvinyl chloride, paper, leather, fabric etc., is specially adapted to the hot pressure-sensitive adhesive of the materials such as clothes, fabric, paper, leather.
A preparation method for the active pressure-sensitive adhesive article of heat, gets the active pressure sensitive adhesive of above-mentioned heat, is evenly applied on various base materials, dry glue thickness 30 μ m, and heating, drying at 60 ℃ of-70 ℃ of temperature, makes the active pressure-sensitive adhesive article of heat.
Compared with prior art, effect of the present invention is, under normal temperature, solvent-based thermal active crylic acid ester pressure-sensitive is sticked with product, and under normal temperature, its initial bonding strength and stripping strength are extremely low, do not need interleaving paper just pressure sensitive adhesive goods can be stacked together and not stick together.During use, bonding with other materials in 110 ℃~120 ℃ temperature pressurization, stripping strength greatly improves, and obtains good pressure-sensitive adhesive performance, and can repeatedly paste under said temperature, has reversibility, and does not affect the use properties of glue.
Patent goods of the present invention are deposited process does not need interleaving paper to isolate, in the time of on being coated on the materials such as leather, foam, fabric, paper, after solvent evaporates, can form the glued membrane of the extremely low pressure-sensitive of one deck, its glued membrane does not come off, during use, direct heating pressurization can be bonding preferably with other materials, and have hot pressure-sensitive.Owing to not needing interleaving paper, reduced production and use cost, reduced working link, saved man-hour, improved working efficiency.Due to adding of active material stearic amide, hexanediamine carbamate, Zinic stearas, lanolin, under heating condition, promoted the crosslinked of acrylate, temperature tolerance, cohesive strength and the adhesive property of acrylate pressure-sensitive adhesive have been improved greatly, and at 110 ℃~120 ℃ temperature, can repeatedly paste, and there is good reversibility.
embodiment:
Embodiment 1
The active pressure sensitive adhesive tackiness agent of heat, it has following weight part is unit, through copolymerization, forms.
(1) Isooctyl acrylate monomer is 20 parts
(2) chloroprene is 2 parts
(3) vinylformic acid is 2 parts
(4) methyl methacrylate is 25 parts
(5) butyl acrylate is 30 parts
(6) hydroxy ethyl methacrylate is 1 part
(7) vinylformic acid glycidyl ether is 0.5 part
(8) stearic amide is 2 parts
(9) toluene is 70 parts
(10) ethyl acetate is 30 parts
(11) benzoyl peroxide is 0.2 part
(1)~(7) are added to header tank, 0.2 part of 10 parts of ethyl acetate and benzoyl peroxide is mixed and adds header tank, 3/4ths (9), (10) are joined to reactor, reactor temperature rise to 85 ℃, drip 2 hours, 86 ± 2 ℃ are reacted 4 hours, make pressure sensitive adhesive.Reactive monomer stearic amide is dissolved in the ethyl acetate and toluene of solvent total amount 1/4th.Temperature of reaction kettle is risen to 95 ℃, the active material after dissolving is added in reactor, after stirring, be cooled to below 45 ℃, filter blowing, obtain solvent-based thermal active crylic acid pressure sensitive adhesive.
Coat on aluminium sheet and dry, dry glue thickness 30 μ m, heating is used front pressure-sensitive low, and normal temperature stripping strength is only 0.1 N/2.5cm, is covered with after nylon heating and pressurizing 7min stripping strength >=13.0N/2.5cm at 110 ℃.
Embodiment 2
(1) Isooctyl acrylate monomer is 50 parts
(2) chloroprene is 4 parts
(3) vinylformic acid is 3 parts
(4) methyl methacrylate is 35 parts
(5) butyl acrylate is 50 parts
(6) hydroxy ethyl methacrylate is 5 parts
(7) vinylformic acid glycidyl ether is 3 parts
(8) 4 parts of hexanediamine carbamates, 2 parts, lanolin
(9) toluene is 100 parts
(10) ethyl acetate is 40 parts
(11) benzoyl peroxide is 0.4 part
(1)~(7) are added to header tank, 0.4 part of 10 parts of ethyl acetate and benzoyl peroxide is mixed and adds header tank, 3/4ths (9), (10) are joined to reactor, reactor temperature rise to 85 ℃, drip 2 hours, 86 ± 2 ℃ are reacted 4 hours, make pressure sensitive adhesive.Reactive monomer hexanediamine carbamate is dissolved in the ethyl acetate and toluene of solvent total amount 1/4th.Temperature of reaction kettle is risen to 95 ℃, the active material after dissolving is added in reactor, after stirring, be cooled to below 45 ℃, filter blowing, obtain solvent-based thermal active crylic acid pressure sensitive adhesive.
Coat on PVC base material, make hot active pressure sensitive adhesive goods, dry glue thickness 30 μ m, normal temperature stripping strength is only 0.15 N/2.5cm, at 115 ℃, is covered with terylene heating and pressurizing 10min, stripping strength 15N/2.5cm.
Embodiment 3
(1) Isooctyl acrylate monomer is 30 parts
(2) chloroprene is 3 parts
(3) vinylformic acid is 2.5 parts
(4) methyl methacrylate is 30 parts
(5) butyl acrylate is 40 parts
(6) hydroxy ethyl methacrylate is 3 parts
(7) vinylformic acid glycidyl ether is 2 parts
(8) Zinic stearas is 4 parts
(9) toluene is 80 parts
(10) ethyl acetate is 30 parts
(11) benzoyl peroxide is 0.25 part
(1)~(7) are added to header tank, 0.25 part of 10 parts of ethyl acetate and benzoyl peroxide is mixed and adds header tank, 3/4ths (9), (10) are joined to reactor, reactor temperature rise to 85 ℃, drip 2 hours, 86 ± 2 ℃ are reacted 4 hours, make pressure sensitive adhesive.Reactive monomer Zinic stearas, lanolin are dissolved in the ethyl acetate and toluene of solvent total amount 1/4th.Temperature of reaction kettle is risen to 95 ℃, the active material after dissolving is added in reactor, after stirring, be cooled to below 45 ℃, filter blowing, obtain solvent-based thermal active crylic acid pressure sensitive adhesive.
By above-mentioned solvent-based thermal active crylic acid ester pressure-sensitive.Coat 60 ℃ of oven dry on steel plate, dry glue thickness 30 μ m, normal temperature is toughness slightly, and glued membrane does not destroy, and is covered with nylon heating and pressurizing 7min, stripping strength >=13.0N/2.5cm in the time of 110 ℃.

Claims (4)

1. a solvent-based thermal active crylic acid ester pressure-sensitive, is characterized in that: the weight part of its comonomer is:
Butyl acrylate: 30~50
Isooctyl acrylate monomer: 20~55
Chloroprene: 2~4
Methyl methacrylate: 25~35
Vinylformic acid: 1~3
Hydroxy ethyl methacrylate: 1~5
Vinylformic acid glycidyl ether: 0.5~3.
2. solvent-based thermal active crylic acid ester pressure-sensitive according to claim 1, it is characterized in that: also contain weight part and be 2~6 hot active material, described hot active material is selected from least one in stearic amide, hexanediamine carbamate, Zinic stearas and lanolin.
3. solvent-based thermal active crylic acid ester pressure-sensitive according to claim 1 and 2, is characterized in that:
Adopt the solvent of following weight part: toluene: 70~100, ethyl acetate: 20~40;
Adopt the catalyzer of following weight part: benzoyl peroxide: 0.2~0.4.
4. a preparation method for solvent-based thermal active crylic acid ester pressure-sensitive claimed in claim 3, is characterized in that adopting following steps:
(1) ethyl acetate of total amount 3/4ths and toluene are added in reactor;
(2) vinylformic acid glycidyl ether, chloroprene, butyl acrylate, Isooctyl acrylate monomer, hydroxy ethyl methacrylate, vinylformic acid, methyl methacrylate and initiator B PO are together added with the header tank stirring, and start stirring;
(3) open reactor and stir, and heating, when the temperature in reactor rises to 85 ℃, start to drip mix monomer and initiator by header tank, and keep temperature to be no more than 88 ℃, within 2 hours, dropwise, and be incubated 4 hours at 85 ℃~88 ℃ temperature;
(4) reactive monomer is dissolved in remaining ethyl acetate and toluene, at 90 ℃ of heating and meltings;
(5) temperature of reaction kettle is risen to 95 ℃, the active material after dissolving is added in reactor, after stirring, be cooled to below 45 ℃, filter blowing, obtain solvent-based thermal active crylic acid pressure sensitive adhesive.
CN201410037153.3A 2014-01-26 2014-01-26 The preparation method of solvent-based thermal active crylic acid ester pressure-sensitive and goods thereof Active CN103756603B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106795397A (en) * 2014-09-16 2017-05-31 株式会社Lg化学 Adhesive composition, optical bonding film and touch panel for touch panel
CN112226183A (en) * 2020-10-26 2021-01-15 浙江龙游道明光学有限公司 Removable pressure sensitive adhesive composition
CN113980181A (en) * 2021-10-28 2022-01-28 山纳合成橡胶有限责任公司 Preparation method of chloroprene and methyl methacrylate copolymer

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05112618A (en) * 1991-10-21 1993-05-07 Sekisui Chem Co Ltd Production of solvent type acrylic tacky agent
CN102533164A (en) * 2011-12-07 2012-07-04 新丰杰力电工材料有限公司 Thermo-sensitive acrylate pressure-sensitive adhesive and adhesive tape and preparation method of adhesive and adhesive tape
CN102559101A (en) * 2011-12-07 2012-07-11 新丰杰力电工材料有限公司 Thermal-spalling acrylic ester pressure-sensitive adhesive, adhesive tape and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05112618A (en) * 1991-10-21 1993-05-07 Sekisui Chem Co Ltd Production of solvent type acrylic tacky agent
CN102533164A (en) * 2011-12-07 2012-07-04 新丰杰力电工材料有限公司 Thermo-sensitive acrylate pressure-sensitive adhesive and adhesive tape and preparation method of adhesive and adhesive tape
CN102559101A (en) * 2011-12-07 2012-07-11 新丰杰力电工材料有限公司 Thermal-spalling acrylic ester pressure-sensitive adhesive, adhesive tape and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106795397A (en) * 2014-09-16 2017-05-31 株式会社Lg化学 Adhesive composition, optical bonding film and touch panel for touch panel
CN112226183A (en) * 2020-10-26 2021-01-15 浙江龙游道明光学有限公司 Removable pressure sensitive adhesive composition
CN113980181A (en) * 2021-10-28 2022-01-28 山纳合成橡胶有限责任公司 Preparation method of chloroprene and methyl methacrylate copolymer
CN113980181B (en) * 2021-10-28 2023-12-29 山纳合成橡胶有限责任公司 Preparation method of chloroprene and methyl methacrylate copolymer

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