CN113997657B - Oil-resistant acid foam, preparation method and application thereof - Google Patents

Oil-resistant acid foam, preparation method and application thereof Download PDF

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CN113997657B
CN113997657B CN202111171658.5A CN202111171658A CN113997657B CN 113997657 B CN113997657 B CN 113997657B CN 202111171658 A CN202111171658 A CN 202111171658A CN 113997657 B CN113997657 B CN 113997657B
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foam
parts
crosslinking degree
core material
foam core
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CN113997657A (en
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顾正青
夏有贵
耿洪斌
周奎任
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Suzhou Shinuo New Material Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B25/042—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of natural rubber or synthetic rubber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/14—Layered products comprising a layer of natural or synthetic rubber comprising synthetic rubber copolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/022—Mechanical properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L51/08—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/02—Polyalkylene oxides
    • C08L71/03—Polyepihalohydrins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/29—Laminated material
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/558—Impact strength, toughness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/726—Permeability to liquids, absorption
    • B32B2307/7265—Non-permeable
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/16—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Laminated Bodies (AREA)
  • Adhesive Tapes (AREA)

Abstract

The invention discloses an oil-resistant acid foam, a preparation method and application thereof; the oil-resistant acid foam comprises a foam core material with high crosslinking degree, a foam core material with low crosslinking degree and an adhesive layer, wherein the oil-resistant acid foam is symmetrically arranged with the foam core material with high crosslinking degree as the center, and the foam core materials with low crosslinking degree on two sides are adhered by the adhesive layer, and comprises the following steps: s1: preparing a foam core material with high crosslinking degree; s2: preparing a foam core material with low crosslinking degree; s3: tearing off release films on two sides of a foam core material with high crosslinking degree, respectively attaching adhesive layers on two sides, attaching a foam core material with low crosslinking degree on the other side of the adhesive layers to obtain oleic acid-resistant foam, and attaching adhesive surface layers on the upper and lower sides of the oleic acid-resistant foam to obtain the oleic acid-resistant foam adhesive tape.

Description

Oil-resistant acid foam, preparation method and application thereof
Technical Field
The invention relates to the technical field of adhesives, in particular to an oil-resistant acid foam, a preparation method and application thereof.
Background
The foam adhesive tape has excellent wettability, holding viscosity, weather resistance, waterproof property, sealing property, compression deformation resistance, flame retardance and the like, is widely applied to the fields of electronic appliances, mechanical parts, various small household appliances, mobile phone accessories, industrial instruments, computers, peripheral equipment, automobile accessories, video and audio equipment, toys, cosmetics and the like according to different thickness and function selections, and has very wide market. The double-sided adhesive tape used for sticking a machine body and a display on a smart phone, a tablet computer is one of applications of foam adhesive tapes, and the foam adhesive tapes are required to have high bonding strength while having impact resistance, shearing resistance and waterproof performance. At present, the foam double-sided adhesive tape is used in a plurality of manufacturers at home and abroad, such as apples, samsung, huacheng, OPPO, VIVO, millet and the like.
The foam double-sided adhesive tape which is firstly applied to the mobile phone electronic client is PE foam double-sided adhesive tape, has the advantages of water resistance, high bonding strength and re-peelability, but has common anti-buffering performance, and cannot meet the performance requirements of increasingly thinned electronic fields; along with the development of narrow frames in the mobile phone industry, the requirements on double-sided adhesive tapes for bonding front glass, outer frames and middle frames of mobile phones are more and more severe, the requirements on buffering performance of large-screen glass are more and more strong, and meanwhile, electronic products such as mobile phones are frequently contacted with fingers in daily life, so that a multiplicable machine is provided for oleic acid sweat and the like on the surfaces of the fingers to permeate into gaps of the mobile phones, further, bonding failure of mobile phone frames is caused, and a novel waterproof buffering oleic acid-resistant foam adhesive tape is generated.
At present, the foam double-sided adhesive tape applied to the bonding of the outer frame of a mobile phone is mainly 3M, tesa, nitto, anyone and the like, wherein 3M is mainly 864XX series, and is characterized in that a styrene-isoprene-styrene block copolymer and acrylic ester prepolymer blending extrusion process is adopted, so that the foam double-sided adhesive tape has excellent impact resistance and re-strippable performance, but has poor die cutting performance and does not have oleic acid resistance; tesa adopts acrylic ester foam, and has good die cutting property and good oil and acid resistance due to larger storage modulus at normal temperature, but has poor impact resistance and water resistance; nitto is still in the research and development stage at present, and is mainly formed by foaming and laminating chemical-resistant PSA, and is mainly characterized by good oil-acid resistance, but general impact resistance and re-strippable performance; the double-sided foam adhesive tape of Anyong mainly adopts polyurethane foaming, has excellent impact resistance and water resistance, is not resistant to oleic acid, has poor re-strippability, and cannot meet the requirements of heavy industry.
Disclosure of Invention
The invention aims to provide oil acid foam resistant, a preparation method and application thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
the oil-resistant acid foam cotton comprises a foam core material with high crosslinking degree, a foam core material with low crosslinking degree and an adhesive layer, wherein the oil-resistant acid foam cotton takes the foam core material with high crosslinking degree as the center, the foam core materials with low crosslinking degree on two sides are symmetrically arranged, and the foam core materials with high crosslinking density and the foam core materials with low crosslinking degree are adhered through the adhesive layer.
As an optimization, the high-crosslinking-degree foam core material comprises the following materials in parts by weight: 100 parts of chloroether rubber, 0.3-2 parts of cross-linking agent A, 0.3-1.5 parts of cross-linking agent B, 0.2-2 parts of microsphere filler, 0.5-2 parts of aging agent, 0.1-1 part of light stabilizer, 0.5-2 parts of pigment and 250-350 parts of solvent.
As an optimization, the materials required by the foam core material with low crosslinking degree comprise the following components in weight percent: 100 parts of ternary chloroether elastomer, 10-20 parts of acrylic ester segmented copolymer, 10-30 parts of long-chain alkyl monomer, 0.5-3 parts of functional monomer, 0.1-0.5 part of thermal initiator, 1-2 parts of antioxidant, 0.2-2 parts of microsphere filler, 0.5-2 parts of pigment, 0.5-1.5 parts of curing agent and 600 parts of solvent.
As optimization, the microsphere filler of the foam core material with high crosslinking degree and the microsphere filler of the foam core material with low crosslinking degree are one or more of hollow glass microspheres, perlite expanded rock, expanded acrylonitrile polymer microspheres and unexpanded acrylonitrile polymer microspheres, the solvent is one or more of toluene, xylene, tetrahydrofuran, cyclohexanone and acetone, and the pigment is one or more of alkaline black slurry, white slurry and color slurry.
As optimization, the chloroether rubber is one or more of epichlorohydrin homo-polymer rubber elastomer, binary epichlorohydrin, ethylene oxide-chloroethane copolymer rubber elastomer and ternary chloroether elastomer.
As optimization, the light stabilizer is one or more of o-hydroxybenzophenones, benzotriazoles, salicylates, triazines, substituted acrylonitriles and hindered amines, the cross-linking agent A is one or more of amine cross-linking agents including ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, metaphenylene diamine, diaminodiphenylmethane, benzidine and bilateral amino ether, the cross-linking agent B is one or more of hydrogen peroxide, tertiary butyl hydroperoxide, benzoyl peroxide, dicumyl peroxide, di-tertiary butyl peroxide, azodiisobutyronitrile, azodiisovaleronitrile, azodiisoheptanenitrile, dimethyl azodiisobutyrate and azodicyclohexyl carbonitrile, and the ageing agent is one or more of octadecyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenylpropionate and tris (2, 4-di-tertiary butylphenyl) phosphite.
Preferably, the acrylate block copolymer is a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer.
Preferably, the long-chain alkyl monomer is alkyl (methyl) acrylate containing 4-10 carbons, including one or more of butyl (methyl) acrylate, 2-ethylhexyl (methyl) acrylate, isooctyl (methyl) acrylate and n-octyl (methyl) acrylate.
As optimization, the curing agent is one or more of isocyanate curing agent, epoxy curing agent and amine curing agent, and the antioxidant is one or more of 2, 6-di-tert-butyl-p-cresol, styrenated phenol, 2, 5-di-tert-butyl hydroquinone, 2' -dimethylene bis- (4-methyl-6-tert-butyl phenol), 2, 4-trimethyl-1, 2-dihydroquinoline polymer, octadecyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxy-phenyl propionate, tetra [ beta- (3, 5-di-tert-butyl-4-hydroxy-phenyl) propionic acid ] pentaerythritol ester, tri (2, 4-di-tert-butylphenyl) phosphite and 2-mercaptobenzimidazole.
Preferably, the functional monomer is one or more of (methyl) acrylic acid, itaconic acid, glycidyl (methyl) acrylate, hydroxyethyl (methyl) acrylate, hydroxypropyl (methyl) acrylate, acrylamide and N-methylolacrylamide.
Preferably, the thermal initiator is one or more of benzoyl peroxide, tert-butyl hydroperoxide, azodiisobutyronitrile and azodiisoheptonitrile.
As an optimization, the method comprises the following steps:
s1: dissolving the chlorohydrin rubber with a solvent, adding microsphere filler, an aging agent, a light stabilizer, pigment, a cross-linking agent A and a cross-linking agent B, uniformly mixing, removing bubbles, coating on a PET release substrate 3, pre-drying at 40-100 ℃, removing the solvent, and baking at 160 ℃ for 5-10min to obtain a foam core material with high cross-linking degree;
s2: dissolving the ternary chloroether elastomer and the acrylic ester segmented copolymer by using a solvent, heating to 80-90 ℃, introducing nitrogen while stirring to purge the liquid level for 60min, adding a long-chain alkyl monomer, a functional monomer and a thermal initiator, uniformly mixing, reacting for 4h, stopping introducing nitrogen, adding an antioxidant, cooling, adding microsphere filler, pigment and a curing agent, uniformly mixing, removing bubbles, coating on a PET release substrate 3, pre-baking at 40-100 ℃, removing the solvent, and baking at 160 ℃ for 5-10min to obtain the foam core material with low crosslinking degree;
s3: tearing off release films on two sides of the foam core material with high crosslinking degree, respectively attaching adhesive layers on two sides, and attaching foam core material with low crosslinking degree on the other side of the adhesive layers to obtain the oleic acid-resistant foam.
As optimization, the two sides of the foam core material with low crosslinking degree should be corona treated, and the dyne value is more than 48dyn/cm.
As optimization, the oleic acid-resistant foam tape is obtained by tearing off the upper and lower side release films according to any one of the above materials and attaching a glue surface layer.
Compared with the prior art, the invention has the following beneficial effects: the invention adopts the ternary chlorohydrin elastomer as a main body to prepare the foam core material with high crosslinking degree and the foam core material with low crosslinking degree, and the ternary chlorohydrin elastomer has high elasticity and softness which are inferior to natural rubber, but has the performances of air tightness, oil resistance, solvent resistance, high temperature resistance, low temperature resistance, ozone resistance, aging resistance and the like which are not possessed by the natural rubber, and meanwhile, the side chain contains allyl glycerol ether obtained by ring opening polymerization, so that the secondary thermal crosslinking reaction can be carried out.
The polyamine and peroxide mixed cross-linking agent is adopted, the amine carries out chlorine substitution reaction on the ternary chlorinated polyether rubber elastomer molecules, and then bridging reaction is formed on the two chlorinated polyether elastomer macromolecules, meanwhile, the chlorine content is reduced, the peroxide is heated and cracked, free radicals are generated to attack C=C double bonds on allyl groups, the C=C double bonds on the allyl groups on side chains on the rubber macromolecules are further linked, network cross-linking is generated, and the high elasticity, the re-stripping performance, the oil resistance, the solvent resistance and the ageing resistance of the ternary chlorinated polyether rubber elastomer are greatly improved.
The foam core material with low crosslinking degree adopts the acrylic ester modified ternary chloroether elastomer as a main body, improves the softness and impact resistance of the foam core with low crosslinking degree, is attached to two sides of the foam core material with high crosslinking degree, enhances the overall impact resistance of the foam adhesive tape, and gives consideration to the oleic acid resistance.
The foam core material with high crosslinking degree is used as the middle core material and is matched with the polymer microsphere, so that the re-stripping performance and the waterproof performance of the foam core material are greatly improved, and the impact resistance is improved.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
Fig. 1 is a laminated structure diagram of an oil-resistant acid foam tape.
In the figure: 1-PET release liner 2, 2-adhesive surface layer, 3-foam core material with low crosslinking degree, 4-adhesive layer, 5-foam core material with high crosslinking degree and 6-PET release liner 1.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Material sources in the examples:
abbreviations for materials Material name Source
H1100 Ternary chloroether rubber Rion Corp.
CG-102 Ternary chloroether rubber Japanese Dasoh Co Ltd
Epion301 Ternary chloroether rubber Japanese Dasoh Co Ltd
TETE Triethylene tetramine Alatine
EDA Ethylenediamine Alatine
BPO Benzoyl peroxide Group of Chinese medicine
DCP Dicumyl peroxide Group of Chinese medicine
920DE80d30 Polymer microsphere Ackersu
F-50 Polymer microsphere Japanese pine oil
1076 Octadecyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenyl propionate Basiff chemical Co Ltd
168 Tris (2, 4-di-tert-butylphenyl) phosphite Basiff chemical Co Ltd
292 Bis (1, 2, 6-pentamethylpiperidinol) sebacate Basiff chemical Co Ltd
B117 Alkaline black pigment Shanghai with cautions for chemical industry
LA2140 Acrylic ester block copolymers Japanese colali Co Ltd
2-EHA 2-ethylhexyl acrylate Satellite petrochemical industry
HEA Hydroxy ethyl acrylate Satellite petrochemical industry
TOL Industrial toluene Satellite petrochemical industry
l-75 Isocyanate curing agent BAYER AG
PET release liner 1 75 mu m PET release substrate YANGZHOU ALVIN FILM Co.,Ltd.
PET release liner 2 50 mu m PET release liner YANGZHOU ALVIN FILM Co.,Ltd.
PET release liner 3 25 mu m PET release liner YANGZHOU ALVIN FILM Co.,Ltd.
Take example A1 as an example:
s1: dissolving the ternary chloroether elastomer and the acrylic ester segmented copolymer by using toluene, heating to 82 ℃, introducing nitrogen while stirring to purge the liquid level for 60min, adding 2-ethyl acrylate, hydroxyethyl acrylate and benzoyl peroxide, uniformly mixing, reacting for 4h, stopping introducing nitrogen, adding octadecyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxy phenylpropionate and tris (2, 4-di-tert-butylphenyl) phosphite, cooling, adding polymer microspheres, alkaline black pigment and isocyanate curing agent, uniformly mixing, removing bubbles, coating on a PET release substrate 3, pre-baking at 100 ℃, removing a toluene solvent, and baking at 160 ℃ for 10min to obtain the low-crosslinking foam core material.
Examples A1 to A3, comparative examples CA1 to CA3: according to the replacement of conditions such as the compound and the content in the example A1, the specific content data are shown in Table 1, and the prepared foam core material with low crosslinking degree is detected, and the specific detection data are shown in Table 2.
TABLE 1 examples A1-A3 and comparative examples CA1-CA4 medium and low crosslinking foam cores
Figure BDA0003293543950000061
Figure BDA0003293543950000071
TABLE 2 influence of examples A1-A3 and comparative examples CA1-CA4 on storage modulus and compatibility
Figure BDA0003293543950000072
Conclusion: on the premise of ensuring good system compatibility, the more the acrylic ester block copolymer is added, the lower the normal-temperature storage modulus is, and the shock resistance of the foam adhesive tape is enhanced.
Using example B1 as an example, oleic acid-resistant foam was prepared by combining the low-crosslinking-degree foam core material prepared in example A2
S1: dissolving a ternary chloroether elastomer by using toluene, adding polymer microspheres, octadecyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxy phenylpropionate, tris (2, 4-di-tert-butylphenyl) phosphite ester, bis (1, 2, 6-pentamethylpiperidinol) sebacate, alkaline black pigment, triethylene tetramine, ethylenediamine, benzoyl peroxide and dicumyl peroxide, uniformly mixing, removing bubbles, coating on a PET release substrate 3, prebaking at 80 ℃, removing a solvent, and baking at 160 ℃ for 8min to obtain a high-crosslinking-degree foam core material;
s2: preparing a foam core material with low crosslinking degree;
s3: tearing off release films on two sides of the foam core material with high crosslinking degree, respectively attaching An Zuo chemically produced adhesive layers on two sides, and attaching low crosslinking degree foam core material (corona treatment is carried out on two sides of the foam core material with low crosslinking degree, and the dyne value is more than 48 dyn/cm) on the other sides of the adhesive layers to obtain the oleic acid-resistant foam.
S4: tearing off release films on the upper side and the lower side of the oleic acid-resistant foam, coating adhesive surface layers produced by Anzuki chemistry on PET release substrates, and respectively attaching the PET release substrates on the upper side and the lower side of the oleic acid-resistant foam to obtain the oil acid-resistant foam adhesive tape.
Examples B1 to B13, comparative examples CB1 to CB6: specific content data are shown in Table 3, based on the change of conditions such as compound and content in example B1.
TABLE 3 oil and acid resistant foam tapes of examples B1-B13 and comparative examples CB1-CB6
Figure BDA0003293543950000081
Figure BDA0003293543950000091
Detection test:
performance measurements were carried out on examples B1 to B13 and comparative examples CB1 to CB6, and the specific measurement methods are shown in Table 4.
Foam density testing: cutting foam into 10cm samples, weighing M, recording the thickness H of the samples, calculating the density of the foam by using a density formula of ρ=M/(S×H) =M/(10×10×H) =M/(100×H), and testing the average value of the three groups in parallel to obtain the foam density.
Gel fraction test: weighing about 0.5g of adhesive film, and recording weight M 1 Then using about 100g toluene to make dissolution for 24 hr, then using 400 mesh goldBelongs to the filtering of a filter screen, and simultaneously the weight M of the filter screen is weighed before the filtering 2 After the solvent mixture is filtered, the filter screen and the residue on the filter screen are put into a baking oven at 130 ℃ to be baked for 1h to constant weight, and then are put into a drying dish to be cooled to room temperature and then are weighed M 3 Finally according to the formula
Figure BDA0003293543950000092
Calculating the gel fraction of the adhesive film; the average value obtained by the parallel test of the three groups is the gel fraction of the adhesive film.
Ball drop impact test: the impact resistance of the tape samples was measured according to ASTM D5628, 180mm2 zigzag (outer frame 24.5mm, inner frame 20.5mm,2.0mm width) samples were applied between stainless steel sheets (24.5 mm x 3 mm) and 3mm zigzag stainless steel sheets (outer frame 40mm, inner frame 20 mm), then a weight of 6.2Kg was placed on top of the bonded article for 10 seconds, then removed, after which the bonded article was allowed to stand at 23 ℃ and 50% Relative Humidity (RH) for 48 hours. Next, the total impact energy (total energy) required to debond the stainless steel substrate was measured and recorded by striking the bonded article with an Instron CEAST9340 by dropping 3.00Kg (standard beam + weight) from a height of 100 cm. Three measurements were made for each example and the average was calculated.
Re-peelability: the coupon was cut into rectangles (150 mm 60mm, width 0.5 mm), then attached to a clean stainless steel plate and left at 23 ℃ and 50% Relative Humidity (RH) for 24 hours, after which the coupon was lifted off by any part of the stainless steel tweezers and wound several turns around the tips of the tweezers, the tape was peeled off at 45 °, 90 ° etc. beginning at a speed of not less than 5 cm/s, the tape was not broken and no adhesive residue remained on the plate, the re-peelability was good, three test strips were tested in each example, and any one of the stretch-break or adhesive residue meant poor re-peelability.
Oil resistant acid: removing the light release film from the sample, attaching the adhesive surface to a 50 mu m PET base film, cutting into 25mm and 50mm sample strips, removing the second surface release film, slowly attaching the adhesive surface to an SUS steel plate, storing at room temperature for 24 hours, placing the SUS steel plate attached with foam sample strips in oleic acid at 65 ℃, taking out the sample after sealing and storing for 72 hours, wiping the surface of the sample with paper to remain oleic acid, recovering at room temperature for 2 hours, observing the swelling degree of the sample strips and whether the sample strips are easy to fall off
TABLE 4 influence of examples B1-B13 and comparative examples CB1-CB6 on various properties
Figure BDA0003293543950000101
Figure BDA0003293543950000111
Conclusion: when the tensile strength and the tensile rate of the foam reach 3MPa and above 600 percent respectively, the re-peeling performance tends to be better, and if the tensile strength or the tensile rate is reduced, the re-peeling performance is also reduced; meanwhile, in the embodiment, when the addition amount of the polymer microsphere is less than 0.2 part, the foam has poor falling ball impact property, and when the addition amount is more than 2 parts, the tensile strength is too low, so that the re-peeling property is poor; in the examples, although the chlorohydrin rubber and the solvent-resistant PSA surface layer with better grease resistance are adopted, the crosslinking degree (gel fraction) of the foam also affects the overall oil acid resistance and impact resistance, when the gel fraction is higher than 70%, the oleic acid resistance and the re-peeling resistance are obviously improved, and the impact resistance is reduced, and when the gel fraction is lower than 50%, the oleic acid resistance and the re-peeling resistance are reduced, and the impact resistance is enhanced.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. An oil resistant acid foam which is characterized in that: the oil-resistant acid foam comprises a foam core material with high crosslinking degree, a foam core material with low crosslinking degree and an adhesive layer, wherein the oil-resistant acid foam takes the foam core material with high crosslinking degree as the center, the foam core materials with low crosslinking degree on two sides are symmetrically arranged, and the foam core materials with high crosslinking degree and the foam core materials with low crosslinking degree are adhered through the adhesive layer;
the foam core material with high crosslinking degree comprises the following materials in parts by weight: 100 parts of ternary chloroether elastomer, 0.5-2 parts of cross-linking agent A, 0.3-1.5 parts of cross-linking agent B, 0.2-2 parts of microsphere filler, 0.5-2 parts of ageing agent, 0.1-1 part of light stabilizer, 0.5-2 parts of pigment and 250-350 parts of solvent;
the foam core material with low crosslinking degree comprises the following materials in parts by weight: 100 parts of ternary chloroether elastomer, 10-20 parts of acrylic ester segmented copolymer, 10-30 parts of long-chain alkyl monomer, 0.5-3 parts of functional monomer, 0.1-0.5 part of thermal initiator, 1-2 parts of antioxidant, 0.2-2 parts of microsphere filler, 0.5-2 parts of pigment, 0.5-1.5 parts of curing agent and 600 parts of solvent;
the side chain of the ternary chloroether elastomer contains allyl glycerol ether obtained by ring-opening polymerization;
the microsphere filler is one or more of 920DE80d30 and F-50;
the cross-linking agent A is an amine cross-linking agent and comprises one or more of ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, m-phenylenediamine, diaminodiphenylmethane, benzidine and bilateral amino ether, and the cross-linking agent B is one or more of hydrogen peroxide, tertiary butyl hydroperoxide, benzoyl peroxide, dicumyl peroxide, di-tertiary butyl peroxide, azodiisobutyronitrile, azodiisovaleronitrile, azodiisoheptonitrile, dimethyl azodiisobutyrate and azodicyclohexyl carbonitrile.
2. The oil resistant acid foam of claim 1, wherein: the solvent is one or more of toluene, xylene, tetrahydrofuran, cyclohexanone and acetone, and the pigment is color slurry.
3. The oil resistant acid foam of claim 1, wherein: the light stabilizer is one or more of o-hydroxybenzophenone, benzotriazole, salicylate, triazine, substituted acrylonitrile and hindered amine, and the aging agent is one or more of octadecyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxy benzene propionate and tris (2, 4-di-tert-butylphenyl) phosphite.
4. The oil resistant acid foam of claim 1, wherein: the acrylic ester block copolymer is methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer.
5. The oil resistant acid foam of claim 1, wherein: the long-chain alkyl monomer is alkyl (methyl) acrylate containing 4-10 carbons, and comprises one or more of butyl (methyl) acrylate, 2-ethylhexyl (methyl) acrylate, isooctyl (methyl) acrylate and n-octyl (methyl) acrylate.
6. The oil resistant acid foam of claim 1, wherein: the functional monomer is one or more of (methyl) acrylic acid, itaconic acid, glycidyl (methyl) acrylate, hydroxyethyl (methyl) acrylate, hydroxypropyl (methyl) acrylate, acrylamide and N-methylolacrylamide.
7. The oil resistant acid foam of claim 1, wherein: the curing agent is one or more of isocyanate curing agent, epoxy curing agent and amine curing agent, and the antioxidant is one or more of 2, 6-di-tert-butyl-p-cresol, styrenated phenol, 2, 5-di-tert-butyl hydroquinone, 2' -dimethylene bis- (4-methyl-6-tert-butylphenol), 2, 4-trimethyl-1, 2-dihydroquinoline polymer, octadecyl-3, 5-bis (1, 1-dimethylethyl) -4-hydroxyphenylpropionate, tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tri (2, 4-di-tert-butylphenyl) phosphite and 2-mercaptobenzimidazole.
8. The oil resistant acid foam of claim 1 wherein the thermal initiator is one or more of benzoyl peroxide, t-butyl hydroperoxide, azobisisobutyronitrile, azobisisoheptonitrile.
9. A method for preparing the oil resistant acid foam according to any one of claims 1 to 8, characterized in that: the method comprises the following steps:
s1: dissolving the ternary chloroether elastomer by using a solvent, adding microsphere filler, an aging agent, a light stabilizer, pigment, a cross-linking agent A and a cross-linking agent B, uniformly mixing, removing bubbles, coating on a PET release substrate 3, pre-drying at 40-100 ℃, removing the solvent, and baking at 160 ℃ for 5-10min to obtain a foam core material with high cross-linking degree;
s2: dissolving the ternary chloroether elastomer and the acrylic ester segmented copolymer by using a solvent, heating to 80-90 ℃, introducing nitrogen while stirring to purge the liquid level for 60min, adding a long-chain alkyl monomer, a functional monomer and a thermal initiator, uniformly mixing, reacting for 4h, stopping introducing nitrogen, adding an antioxidant, cooling, adding microsphere filler, pigment and a curing agent, uniformly mixing, removing bubbles, coating on a PET release substrate 3, pre-baking at 40-100 ℃, removing the solvent, and baking at 160 ℃ for 5-10min to obtain the foam core material with low crosslinking degree;
s3: tearing off release films on two sides of the foam core material with high crosslinking degree, respectively attaching adhesive layers on two sides, and attaching foam core material with low crosslinking degree on the other side of the adhesive layers to obtain the oleic acid-resistant foam.
10. Use of the oleic acid resistant foam of any one of claims 1 to 9, characterized in that: tearing off the release films on the upper side and the lower side of the oleic acid-resistant foam, and attaching an adhesive surface layer to obtain the oleic acid-resistant foam adhesive tape.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5447992A (en) * 1994-06-13 1995-09-05 The Goodyear Tire & Rubber Company Heat and ozone resistant NBR/epichlorohydrin blends
JPH10140109A (en) * 1996-11-14 1998-05-26 Nitto Denko Corp Pressure-sensitive adhesive sheet or the like with foam support
JPH10204401A (en) * 1997-01-24 1998-08-04 Nippon Synthetic Chem Ind Co Ltd:The Pressure sensitive adhesive composition
JP2001003025A (en) * 1999-04-23 2001-01-09 Sekisui Chem Co Ltd Preparation of acrylic adhesive, and acrylic pressure- sensitive adhesive and sticky-processed product
CN104220544A (en) * 2012-04-04 2014-12-17 日东电工株式会社 Pressure-sensitive adhesive tape and tape roll
CN109880543A (en) * 2018-12-27 2019-06-14 新纶科技（常州）有限公司 A kind of foam substrate and double faced adhesive tape

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5447992A (en) * 1994-06-13 1995-09-05 The Goodyear Tire & Rubber Company Heat and ozone resistant NBR/epichlorohydrin blends
JPH10140109A (en) * 1996-11-14 1998-05-26 Nitto Denko Corp Pressure-sensitive adhesive sheet or the like with foam support
JPH10204401A (en) * 1997-01-24 1998-08-04 Nippon Synthetic Chem Ind Co Ltd:The Pressure sensitive adhesive composition
JP2001003025A (en) * 1999-04-23 2001-01-09 Sekisui Chem Co Ltd Preparation of acrylic adhesive, and acrylic pressure- sensitive adhesive and sticky-processed product
CN104220544A (en) * 2012-04-04 2014-12-17 日东电工株式会社 Pressure-sensitive adhesive tape and tape roll
CN109880543A (en) * 2018-12-27 2019-06-14 新纶科技（常州）有限公司 A kind of foam substrate and double faced adhesive tape

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