CN110628345A - Film material for cutting optical glass - Google Patents
Film material for cutting optical glass Download PDFInfo
- Publication number
- CN110628345A CN110628345A CN201910963762.4A CN201910963762A CN110628345A CN 110628345 A CN110628345 A CN 110628345A CN 201910963762 A CN201910963762 A CN 201910963762A CN 110628345 A CN110628345 A CN 110628345A
- Authority
- CN
- China
- Prior art keywords
- parts
- film material
- optical glass
- film
- glass cutting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000010703 silicon Substances 0.000 claims description 14
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms
- C08L23/0815—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms with aliphatic 1-olefins containing one carbon-to-carbon double bond
-
- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
-
- 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
- C09J7/22—Plastics; Metallised plastics
- C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/241—Polyolefin, e.g.rubber
-
- 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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
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- 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
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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- 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
- C09J2301/41—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the carrier layer
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- C09J2423/00—Presence of polyolefin
- C09J2423/04—Presence of homo or copolymers of ethene
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Abstract
The invention relates to the technical field of protective films, in particular to a film material for cutting optical glass. The film material for optical glass cutting comprises a core layer and a glue layer; the core layer is a PO film and is prepared from the following raw materials in parts by weight: 60-70 parts of polyolefin, 18-25 parts of elastomer, 6-10 parts of antistatic agent, 4-8 parts of antioxidant and 3-5 parts of polyoxyethylene-acrylic acid copolymer. The film material for cutting the optical glass has the advantages of safety, environmental protection, excellent aging resistance, antistatic property and stable viscous force, and meanwhile, the film material has good heat dissipation capacity and can meet the application requirements of the film material in various fields.
Description
Technical Field
The invention belongs to the technical field of protective films, and particularly relates to a film material for cutting optical glass.
Background
The protective film is widely applied in various fields, such as electronic products, household appliances, building materials, decorative materials and the like, and the protective film is used in the processes of semi-finished product and finished product assembly and logistics transportation. Especially, the glass plays an important role in protecting optical glass and high-end metal plates.
The optical glass is a basic and important component of the photoelectric technology industry, and along with the continuous fusion development of optics, electronic information science and new material science, the application of the optical glass as a photoelectric basic material in three fields of optical transmission, optical storage and photoelectric display is more rapid, and the optical glass becomes one of the basic conditions for the development of social informatization, particularly the photoelectric information technology. Because of the strict optical imaging requirement of the optical glass, a layer of protective film is required to be adhered to the upper surface and the lower surface of a glass plate in the post-processing process so as to prevent the cutting scraps from directly contacting and adhering to the optical glass and avoid scratches in the transportation and carrying processes.
At present, a plurality of products similar to the protective film with different colors and full of limes are available on the market, but most of the products have incomplete performances and cannot meet the requirements of safety and environmental protection, in addition, the protective film is not aging-resistant, easy to generate static electricity, poor in permanent adhesion and heat dissipation capacity, and easy to have residual glue or ghost after being torn off. Therefore, the development and production of a protective film having stable adhesion, aging resistance, good antistatic and heat dissipating capabilities, safety and environmental protection are urgently needed.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a film material for optical glass cutting, including a core layer and a glue layer; the core layer is a PO film and is prepared from the following raw materials in parts by weight: 60-70 parts of polyolefin, 18-25 parts of elastomer, 6-10 parts of antistatic agent and 4-8 parts of antioxidant.
As a preferable technical solution, the film material for optical glass cutting further comprises a silicon oil layer; the silicon oil layer is positioned on the lower surface of the core layer.
As a preferable technical solution, the film material for optical glass cutting further comprises a PET layer; the PET layer is located the upper surface of glue film.
As a preferred technical solution, the core layer further includes a polyethylene oxide-acrylic acid copolymer.
As a preferable technical solution, the mass ratio of the polyoxyethylene-acrylic acid copolymer to the antistatic agent is 1: (1-3).
As a preferred technical solution, the polyolefin is selected from one or more of polyethylene, polypropylene, ethylene-propylene copolymer, polybutene-1, poly-4-methylpentene-1, ethylene-vinyl acetate copolymer, ethylene-ethyl (meth) acrylate copolymer, ethylene-methyl (meth) acrylate copolymer, and ethylene-acrylic acid copolymer.
As a more preferable technical solution, the polyethylene is modified polyethylene.
As a most preferred technical scheme, the preparation raw materials of the modified polyethylene comprise: linear low-density polyethylene, silane coupling agent, phytic acid, aluminum oxide and wollastonite.
As a preferred embodiment, the elastomer is an ethylene-based elastomer or a propylene-based elastomer.
As a preferred embodiment, the antistatic agent is a fatty acid amide.
As a preferable technical scheme, the antioxidant is 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester.
The second aspect of the present invention provides a method for preparing a film material for semiconductor grinding and packaging as described above, which can be classified into a direct coating method and a spin coating method.
The third aspect of the invention provides an application of the film material for cutting optical glass in the surface protection of optical glass, ceramics, LED display screens, 5G mobile phone screens and metal plates.
Has the advantages that: the invention provides a film material for optical glass cutting. By optimizing and improving the raw materials for preparing the core layer, the film material has excellent aging resistance, antistatic property and stable viscous force on the basis of meeting the safety and environmental protection performance, and meanwhile, the film material has good heat dissipation capacity and can meet the application requirements of the film material in various fields.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "including". As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase will render the claim closed except for the materials described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein in the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received by modifying or otherwise modifying such quantity without substantially changing the basic function to which it is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In view of the above technical problems, the first aspect of the present invention provides a film material for optical glass cutting, comprising a core layer and a glue layer; the core layer is a PO film and is prepared from the following raw materials in parts by weight: 60-70 parts of polyolefin, 18-25 parts of elastomer, 6-10 parts of antistatic agent and 4-8 parts of antioxidant.
In one embodiment, the present invention provides in a first aspect a film material for optical glass cutting, comprising a core layer and a glue layer; the core layer is a PO film and is prepared from the following raw materials in parts by weight: 65 parts of polyolefin, 22 parts of elastomer, 8 parts of antistatic agent and 6 parts of antioxidant.
[ Silicone oil layer ]
In one embodiment, the film material for optical glass cutting further comprises a silicone oil layer; the silicon oil layer is positioned on the lower surface of the core layer.
In one embodiment, the silicon oil layer is obtained by drying raw materials used for the silicon oil layer.
In one embodiment, the preparation method of the raw materials for the silicon oil layer comprises the following steps: pouring 40-60 parts of simethicone into the diluent at a constant speed, stirring simultaneously, adding 3-5 parts of curing agent after stirring for 10-14min, stirring at a constant speed for 20-40min, adding 3-5 parts of stabilizer, and stirring at a constant speed for 20-30min to obtain the product.
In a preferred embodiment, the diluent is toluene.
In a preferred embodiment, the curing agent is an n-butyl alcohol etherified melamine resin.
In a preferred embodiment, the stabilizer is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
In the examples, n-butanol etherified melamine formaldehyde resins were purchased from Shanghai Xinhua resins Co., Ltd; in the examples pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (CAS: 6683-19-8) was purchased from plastication technology Co., Ltd, Sheng, Dongguan; examples Dimethicone (CAS: 9006-65-9) was purchased from Guangzhou Weber chemical Co., Ltd.
[ PET layer ]
In one embodiment, the film material for optical glass cutting further comprises a PET layer; the PET layer is located the upper surface of glue film.
In a preferred embodiment, the PET layer is a PET film.
The PET film is a PET release film. The high-temperature-resistant printing ink has the characteristics of high temperature resistance, good printing, easy processing, good voltage-resistant insulating property and environment friendliness, and passes SGS and ROSH certification. The film is colorless, transparent and glossy, and has the advantages of excellent mechanical performance, high rigidity, hardness and toughness, puncture resistance, friction resistance, high temperature resistance, low temperature resistance, chemical resistance, oil resistance, air tightness and fragrance retention.
In the examples, the PET film was purchased from Shantou Runkang Plastic film Co., Ltd, and was designated PET-19.
[ polyoxyethylene-acrylic acid ] copolymerPolymer-
In one embodiment, the core layer further comprises a polyethylene oxide-acrylic acid copolymer.
In a preferred embodiment, the mass ratio of the polyoxyethylene-acrylic acid copolymer to the antistatic agent is 1: (1-3).
In one embodiment, the polyoxyethylene-acrylic acid copolymer is prepared by the method comprising: adding 14-18 parts of water, 2-4 parts of tert-butyl alcohol, 0.2-0.4 part of acrylic acid solution and 0.3-0.7 part of polyethylene oxide into an autoclave, stirring and heating to 60-100 ℃, and pumping 5g/100mL of H2Potassium persulfate solution of O, after 0.5-1.5H, 1.25g/100mL of H is added2And (3) continuing the polymerization reaction for about 4-8h by using a potassium persulfate solution of O. Samples were taken from time to time during the reaction and the kettle was analyzed for solids content. When the total solid content reaches 18-22%, the autoclave is cooled to finish the reaction, and emulsion is obtained. Adding water, sodium hydroxide solution and sodium chloride into the emulsion, stirring, adding hydrochloric acid, heating to 45-55 deg.C, cooling to room temperature, filtering to obtain condensate, pulping with water, filtering, and drying under air flow.
[ polyolefins ]
The polyolefin of the present invention generally refers to a polymer of ethylene, propylene or higher olefins. English is abbreviated as PO. Of which polyethylene and polypropylene are the most important. The polymer material has the advantages of abundant raw materials, low price, easy processing and forming and excellent comprehensive performance, so the polymer material has the largest output and very wide application.
In one embodiment, the polyolefin is selected from one or more of polyethylene, polypropylene, ethylene-propylene copolymers, polybutene-1, poly-4-methylpentene-1, ethylene-vinyl acetate copolymers, ethylene-ethyl (meth) acrylate copolymers, ethylene-methyl (meth) acrylate copolymers, ethylene-acrylic acid copolymers.
In a more preferred embodiment, the polyolefin is a modified polyethylene.
In a most preferred embodiment, the modified polyethylene is prepared from the following raw materials: linear low-density polyethylene, silane coupling agent, phytic acid, aluminum oxide and wollastonite.
In a preferred embodiment, the silane coupling agent is N- β - (aminoethyl) - γ -aminopropylmethyldimethoxysilane.
Linear low density polyethylene
The linear low-density polyethylene is non-toxic, tasteless and odorless milky white particles. The high-strength high-toughness high-strength high-toughness high-heat-resistance high-cold-resistance high-strength high-toughness high-strength high-toughness high-strength.
In the examples, the linear low density polyethylene was purchased from Guangdong petrochemical division of China oil and gas Co., Ltd under the designation 7042 powder.
Silane coupling agent
The molecular structural formula of the silane coupling agent is generally as follows: Y-R-Si (OR)3(wherein Y-organic functional group, SiOR-siloxy). The siloxy group is reactive with inorganic species and the organofunctional group is reactive or compatible with organic species. Thus, when a silane coupling agent intervenes between the inorganic and organic interfaces, a bonding layer of organic matrix-silane coupling agent-inorganic matrix may be formed.
Examples N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane (CAS: 3069-29-2) was purchased from Shanghai Pont chemical industries, Inc.
Phytic acid
The phytic acid is chemically named as phytic acid and is an organic phosphoric acid compound extracted from plant seeds.
Examples phytic acid (CAS: 83-86-3) was purchased from Guangzhou Chengyang Kongkushi Koncki Co.
Aluminum oxide
The aluminum oxide is a high-hardness compound, has a melting point of 2054 ℃ and a boiling point of 2980 ℃, can be ionized at a high temperature, and is commonly used for manufacturing refractory materials.
Examples alumina (CAS: 1344-28-1) was purchased from Guangzhou Chengyang Kongkushi Co., Ltd.
Wollastonite
The wollastonite is a common calcium metasilicate mineral and belongs to a single-chain silicate mineral. The natural wollastonite usually has the glass luster to the pearl luster, and the color is from white to grey white, the density is high, and the hardness value is high. Compared with other inorganic fillers, the wollastonite powder not only plays a role in filling, but also can partially replace asbestos and glass fiber for reinforcing materials in the plastic industry. The composite material has excellent electrical insulating property, high thermal deformation temperature, low flammability, good permeability, acid and alkali corrosion resistance, and simultaneously has two-dimensional reinforcement, can enhance the modulus, rigidity, hardness, heat resistance and dimensional stability of a plastic matrix, and has particularly remarkable research and application values in the field of novel polymer composite materials.
Examples wollastonite was purchased from Clonoland wollastonite mining GmbH, Panshi, Jilin province, with an average particle size of 4.8. mu.m.
In one embodiment, the modified polyolefin is prepared by the process comprising:
(1) adding 6-8 parts of phytic acid, 3-6 parts of aluminum oxide and 1-3 parts of wollastonite into water, stirring and grinding until the average particle size is smaller than 1 mu m, adding 8-12 parts of silane coupling agent, continuously grinding for 13 h for surface treatment, filtering, washing with water until the pH value is 7, and drying to obtain the filler subjected to surface modification treatment.
Adding 40-60 parts of linear low-density polyethylene into an open mill, wherein the roll temperature is 140-180 ℃, adding a filler subjected to surface modification treatment after the linear low-density polyethylene is coated on a roll, discharging sheets after melt blending, and performing compression molding by a QLD-D type flat vulcanizing machine at the temperature of 150-240 ℃ to obtain the polyethylene.
[ ELASTOMERS ]
The elastomer is a high polymer material which has obvious deformation under weak stress and can be quickly recovered to be close to the original state and size after the stress is relaxed.
In one embodiment, the elastomer is an ethylene-based elastomer or a propylene-based elastomer.
In a preferred embodiment, the elastomer is a propylene-based elastomer.
In the examples, the propylene-based elastomer was purchased from hong Koghai plastics, Inc. of Dongguan, under the designation 6202 FL.
[ antistatic Agents ]
The antistatic agent of the present invention is an additive which is added into plastics or coated on the surface of a molded article for the purpose of reducing static accumulation. Antistatic agents can be classified into two major types, internal type and external type, depending on the method of use, and the main type used for plastics is internal type antistatic agent. They can also be classified into two broad categories, temporary and permanent, according to the nature of the antistatic agent.
In one embodiment, the antistatic agent is a fatty acid amide.
In a preferred embodiment, the antistatic agent is erucamide.
The inventor finds that the phytic acid can enable the antistatic effect of the antistatic agent to be optimal. The possible reason is that phosphate groups in the phytic acid are easily combined with the N end of the antistatic agent, after combination, when other phosphate groups in the phytic acid are complexed with metal, a layer of compact monomolecular protective film is formed on the surface, the processed metal surface is conducted with current by a monomolecular hole electron conducting layer and a passive metal film, so that the antistatic effect is achieved, and the phytic acid and the antistatic agent cooperate to perform double comprehensive antistatic protection.
Example erucamide (CAS: 112-84-5) was purchased from Guangzhou Chengyang Kongkushi, Inc.
[ ANTIOXIDANTS ]
The antioxidants of the present invention are chemical substances which, when present in the polymer system in only small amounts, retard or inhibit the progress of the oxidation process of the polymer, thereby preventing the aging of the polymer and extending its useful life, also known as "age resistors". Antioxidants help protect the above-mentioned polymers and the overall binder system from the effects of thermal and oxidative degradation that often occur during the manufacture and application of film compositions and in the ambient environment to which the final product is normally exposed, primarily as a result of deterioration in the appearance, physical properties, etc. of the composition.
In one embodiment, the antioxidant is n-octadecyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.
Example n-octadecyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (CAS: 2082-79-3) was purchased from American plastication technology Co., Ltd, Dongguan.
In one embodiment, the core layer is prepared by a method comprising: weighing the raw materials according to the formula, uniformly mixing the raw materials by a high-speed mixer, feeding the mixture into an extruder for heating and melting, extruding the mixture by a T-shaped die head, casting the mixture onto a steel roller during melting, cooling and forming, flattening and rolling to obtain the core layer.
[ subbing layer ]
In one embodiment, the glue layer is obtained by drying raw materials used for the glue layer.
In one embodiment, the method for preparing the raw material for the glue layer comprises the following steps:
1. weighing 20-25 parts of butyl acrylate, 9-11 parts of isooctyl acrylate, 1-3 parts of acrylic acid, 2-4 parts of hydroxyethyl acrylate, 1-3 parts of piperidine ethyl methacrylate, 6-14 parts of epoxy resin cross-linking agent and 0.15-0.35 part of initiator, adding into a head tank, and uniformly stirring to obtain a mixed material;
2. weighing 40-60% of solvent of the mixed material, putting into a reaction kettle, and heating to a reflux state;
3. quickly adding one third of the mixed material into a reaction kettle, and keeping reflux reaction for 1-1.5 h;
4. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dripping to be finished within 3-3.5h, and carrying out reflux and heat preservation for 0.5-1.5h after the dripping is finished to obtain a polymer;
5. and (3) uniformly stirring the polymer and 2-4 parts of curing agent to obtain the curing agent.
In a preferred embodiment, the initiator is preferably dibenzoyl peroxide and/or azobisisobutyronitrile.
In a preferred embodiment, the solvent is one or more of ethyl acetate, butyl acetate, and butanone.
In a preferred embodiment, the curing agent is an n-butyl alcohol etherified melamine resin.
Examples butyl acrylate, isooctyl acrylate, acrylic acid, hydroxyethyl acrylate, piperidineethyl methacrylate were purchased from Shanghai Huayi acrylic acid, Inc.; the epoxy resin cross-linking agent was purchased from Dongguan new Ye New Material science and technology Co.
The second aspect of the present invention provides a method for preparing a film material for semiconductor grinding and packaging as described above, which can be classified into a direct coating method and a spin coating method.
In one embodiment, the direct coating method comprises the steps of: firstly, corona-coating the lower surface of the core layer with raw materials for a silicon oil layer, then corona-coating the upper surface of the core layer with raw materials for a glue layer, and placing the core layer in an oven for about 10 days to be stable.
In one embodiment, the spin coating method comprises the steps of:
a: coating the raw material for the glue layer on the upper surface of the PET layer to obtain a transfer coating;
b: and (3) pressing and treating the corona and the transfer coating on the upper surface of the substrate film, and standing for 15 days for stabilization.
In one embodiment, the film material for semiconductor grinding and packaging has a thickness of 5-500 μm.
In a preferred embodiment, the thickness of the film material for semiconductor grinding and packaging is 50-200 μm.
The third aspect of the invention provides an application of the film material for cutting optical glass in the surface protection of optical glass, ceramics, LED display screens, 5G mobile phone screens and metal plates.
Examples
In order to better understand the above technical solutions, the following detailed descriptions will be provided with reference to specific embodiments. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the starting materials used are all commercially available, unless otherwise specified.
Example 1
Example 1 provides a film material for optical glass cutting, comprising a core layer and a glue layer; the core layer is a PO film and is prepared from the following raw materials in parts by weight: 65 parts of polyolefin, 17 parts of elastomer, 8 parts of antistatic agent, 6 parts of antioxidant and 4 parts of polyoxyethylene-acrylic acid copolymer.
The film material for optical glass cutting also comprises a silicon oil layer.
The silicon oil layer is positioned on the lower surface of the core layer.
The silicon oil layer is obtained by drying raw materials used by the silicon oil layer.
The preparation method of the raw materials used by the silicon oil layer comprises the following steps: and pouring 50 parts of simethicone into the toluene at a constant speed, stirring simultaneously, adding 4 parts of n-butyl alcohol etherified melamine resin after stirring for 12min, stirring at a constant speed for 30min, then adding 4 parts of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, and stirring at a constant speed for 25min to obtain the product.
The preparation method of the core layer comprises the following steps: weighing the raw materials according to the formula, uniformly mixing the raw materials by a high-speed mixer, feeding the mixture into an extruder for heating and melting, extruding the mixture by a T-shaped die head, casting the mixture onto a steel roller during melting, cooling and forming, flattening and rolling to obtain the core layer.
The polyolefin is modified polyethylene.
The preparation method of the modified polyolefin comprises the following steps:
(1) adding 7 parts of phytic acid, 4.5 parts of aluminum oxide and 2 parts of wollastonite into water, stirring and grinding the mixture to enable the average particle size of the mixture to be less than 1 mu m, adding 10 parts of N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxysilane, continuously grinding the mixture for 2h for surface treatment, filtering the mixture, washing the mixture with water to enable the pH value to be 7, and drying the mixture to obtain the filler with the modified surface.
(2) Adding 50 parts of linear low-density polyethylene into an open mill, wherein the roll temperature is 160 ℃, adding a surface modified filler after the linear low-density polyethylene is coated on a roll, melting and blending, then discharging, and carrying out compression molding by a QLD-D type flat vulcanizing machine at the temperature of 195 ℃ to obtain the polyethylene.
The linear low density polyethylene is powder T30S.
The elastomer is a propylene-based elastomer.
The propylene-based elastomer is under the designation 6202 FL.
The antistatic agent is erucamide.
The antioxidant is 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate.
The preparation method of the polyoxyethylene-acrylic acid copolymer comprises the following steps: 16 parts of pure water, 3 parts of t-butanol and 0.3 part of acrylic acid solution and 0.5 part of polyethylene oxide were charged into an autoclave, stirred, heated to 80 ℃ and then pumped with 5g/100mL of H2Potassium persulfate solution of O, 1H later, 1.25g/100mL of H2And (3) continuing the polymerization for about 6 hours by using a potassium persulfate solution of O. Samples were taken from time to time during the reaction and the kettle was analyzed for solids content. When the total solid content reached 20%, the autoclave was cooled to end the reaction and the product was evacuated. The product was a white fluid, polymer emulsion containing a small amount of dispersible particles. Adding water, 10% sodium hydroxide solution and sodium chloride into the emulsion, stirring strongly, adding hydrochloric acid, heating to 50 deg.C, cooling to room temperature, and filtering to obtain condensate. And pulping the filter cake with water, filtering, and drying the filter cake (copolymer) under air flow to obtain the copolymer.
The adhesive layer is obtained by drying raw materials used for the adhesive layer.
The preparation method of the raw materials used for the adhesive layer comprises the following steps:
1. weighing 23 parts of butyl acrylate, 10 parts of isooctyl acrylate, 2 parts of acrylic acid, 3 parts of hydroxyethyl acrylate, 2 parts of piperidine methacrylate, 10 parts of epoxy resin cross-linking agent and 0.25 part of dibenzoyl peroxide, adding into a head tank, and uniformly stirring to obtain a mixed material;
2. weighing 60 parts of butyl acetate, and putting the butyl acetate into a reaction kettle to be heated to a reflux state;
3. quickly feeding one third of the mixed material into a reaction kettle, and keeping reflux reaction for 1.5 hours;
4. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dripping to be finished within 3.5h, and carrying out reflux and heat preservation for 1h after the dripping is finished to obtain a polymer;
5. and (3) uniformly stirring the polymer and 3 parts of n-butyl alcohol etherified melamine resin to obtain the polyether polyol.
The preparation method of the film material for cutting the optical glass comprises the following steps: firstly, corona-coating the lower surface of the core layer with raw materials for a silicon oil layer, then corona-coating the upper surface of the core layer with raw materials for a glue layer, and placing the core layer into an oven for 10 days for stabilization.
Example 2
Example 2 is essentially the same as example 1, except that: the core layer is a PO film and is prepared from the following raw materials in parts by weight: 60 parts of polyolefin, 18 parts of elastomer, 6 parts of antistatic agent, 4 parts of antioxidant and 3 parts of polyoxyethylene-acrylic acid copolymer.
Example 3
Example 3 is essentially the same as example 1, except that: the core layer is a PO film and is prepared from the following raw materials in parts by weight: 70 parts of polyolefin, 25 parts of elastomer, 10 parts of antistatic agent, 8 parts of antioxidant and 5 parts of polyoxyethylene-acrylic acid copolymer.
Example 4
Example 4 is essentially the same as example 1, except that: the film material for optical glass cutting further comprises a PET layer.
The PET layer is located the upper surface of glue film.
The PET layer is a PET film.
The preparation method of the film material for cutting the optical glass comprises the following steps:
a: coating the raw material for the glue layer on the upper surface of the PET layer to obtain a transfer coating;
b: and (3) pressing and treating the corona and the transfer coating on the upper surface of the substrate film, and standing for 15 days for stabilization.
Comparative example 1
Comparative example 1 is essentially the same as example 1 except that: the polyolefin is a linear low density polyethylene.
Comparative example 2
Comparative example 2 is essentially the same as example 1 except that:
the preparation method of the modified polyolefin comprises the following steps:
(1) adding 4.5 parts of aluminum oxide and 2 parts of wollastonite into water, stirring and grinding the mixture to enable the average particle size of the mixture to be less than 1 mu m, adding 10 parts of N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxysilane, continuously grinding the mixture for 2 hours for surface treatment, filtering the mixture, washing the mixture with water to enable the pH value to be 7, and drying the mixture to obtain the filler with the modified surface.
(2) Adding 50 parts of linear low-density polyethylene into an open mill, wherein the roll temperature is 160 ℃, adding a surface modified filler after the linear low-density polyethylene is coated on a roll, melting and blending, then discharging, and carrying out compression molding by a QLD-D type flat vulcanizing machine at the temperature of 195 ℃ to obtain the polyethylene.
Comparative example 3
Comparative example 3 is essentially the same as example 1 except that:
the preparation method of the modified polyolefin comprises the following steps:
(1) adding 7 parts of methacrylic acid-beta-hydroxyethyl ester resin, 4.5 parts of aluminum oxide and 2 parts of wollastonite into water, stirring and grinding the mixture to enable the average particle size of the mixture to be less than 1 mu m, adding 10 parts of N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxysilane, continuously grinding the mixture for 2 hours for surface treatment, filtering the mixture, washing the mixture with water to enable the pH value to be 7, and drying the mixture to obtain the filler with the modified surface.
(2) Adding 50 parts of linear low-density polyethylene into an open mill, wherein the roll temperature is 160 ℃, adding a surface modified filler after the linear low-density polyethylene is coated on a roll, melting and blending, then discharging, and carrying out compression molding by a QLD-D type flat vulcanizing machine at the temperature of 195 ℃ to obtain the polyethylene.
Comparative example 4
Comparative example 4 is essentially the same as example 1 except that:
the preparation method of the modified polyolefin comprises the following steps:
(1) adding 7 parts of phytic acid and 4.5 parts of aluminum oxide into water, stirring and grinding the mixture until the average particle size of the mixture is smaller than 1 mu m, adding 10 parts of N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxysilane, continuously grinding the mixture for 2 hours for surface treatment, filtering the mixture, washing the mixture with water to enable the pH value to be 7, and drying the mixture to obtain the filler with the modified surface.
(2) Adding 50 parts of linear low-density polyethylene into an open mill, wherein the roll temperature is 160 ℃, adding a surface modified filler after the linear low-density polyethylene is coated on a roll, melting and blending, then discharging, and carrying out compression molding by a QLD-D type flat vulcanizing machine at the temperature of 195 ℃ to obtain the polyethylene.
Comparative example 5
Comparative example 5 is essentially the same as example 1, except that:
the preparation method of the modified polyolefin comprises the following steps:
(1) adding 7 parts of phytic acid, 4.5 parts of aluminum oxide and 2 parts of wollastonite into water, stirring and grinding the mixture until the average particle size of the mixture is smaller than 1 mu m, adding 10 parts of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, continuously grinding the mixture for 2 hours for surface treatment, filtering the mixture, washing the mixture with water until the pH value is 7, and drying the mixture to obtain the filler subjected to surface modification treatment.
(2) Adding 50 parts of linear low-density polyethylene into an open mill, wherein the roll temperature is 160 ℃, adding a surface modified filler after the linear low-density polyethylene is coated on a roll, melting and blending, then discharging, and carrying out compression molding by a QLD-D type flat vulcanizing machine at the temperature of 195 ℃ to obtain the polyethylene.
Comparative example 6
Comparative example 6 is essentially the same as example 1, except that:
the core layer is a PO film and is prepared from the following raw materials in parts by weight: 65 parts of polyolefin, 17 parts of elastomer, 8 parts of antistatic agent and 6 parts of antioxidant.
Comparative example 7
Comparative example 7 is essentially the same as example 1 except that: the core layer is a PO film and is prepared from the following raw materials in parts by weight: 65 parts of polyolefin, 17 parts of elastomer, 8 parts of antistatic agent, 6 parts of antioxidant and 1 part of polyoxyethylene-acrylic acid copolymer.
Comparative example 8
Comparative example 8 is essentially the same as example 1 except that: the core layer is a PO film and is prepared from the following raw materials in parts by weight: 65 parts of polyolefin, 17 parts of elastomer, 1 part of antistatic agent, 6 parts of antioxidant and 10 parts of polyoxyethylene-acrylic acid copolymer.
The foregoing examples are merely illustrative and are provided to illustrate some of the features of the present disclosure. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. And that advances in science and technology will result in possible equivalents or sub-substitutes not currently contemplated for reasons of inaccuracy in language representation, and such changes should also be construed where possible to be covered by the appended claims.
Evaluation of Performance
(1) Permanent adhesion: the films were tested for their tack strength with reference to the GB/T7124 method.
(2) Aging resistance:
a: polishing the surface of the copper rod smoothly and wiping the surface of the copper rod cleanly;
b: cutting the film into uniform strip samples, and winding the samples on a copper bar;
c: baking the copper bar wound with the sample at the constant temperature of 80-200 ℃, observing the surface condition of the film at intervals, recording the appearance condition of the film, and obtaining the aging resistant time of the film when the surface of the film is pulverized.
(3) Antistatic: the surface resistance of the membrane was measured with reference to the GB/T1410-78 standard.
(4) Heat dissipation: the film thickness was 1mm and the thermal conductivity of the film was tested according to ASTM D5470.
The results of the experiment are shown in the following table:
table 1: performance test data of film materials obtained in examples and comparative examples
As can be seen from Table 1, the film material prepared by the invention has large permanent adhesion and stable adhesion; the embrittlement time is long, and the aging resistance is good; the surface resistance value is low, and the antistatic property is good; meanwhile, the film material has high thermal conductivity, and the film material is proved to have excellent heat dissipation performance.
The film material prepared in the embodiment 1 has the thickness of 70 +/-3 mu m, the light transmittance is more than or equal to 75 percent, the tensile strength is more than or equal to 15MPa, the wetting tension is more than or equal to 36mN/m, and the breaking elongation is more than or equal to 500MD (%). In contrast, the performance data for the membrane materials made from the remaining examples were inferior to that of example 1.
Claims (10)
1. The film material for cutting the optical glass is characterized by comprising a core layer and an adhesive layer from top to bottom in sequence; the core layer is a PO film and is prepared from the following raw materials in parts by weight: 60-70 parts of polyolefin, 18-25 parts of elastomer, 6-10 parts of antistatic agent and 4-8 parts of antioxidant.
2. The film material for optical glass cutting according to claim 1, wherein the film material for optical glass cutting further comprises a silicone oil layer; the silicon oil layer is positioned on the lower surface of the core layer.
3. The film material for optical glass cutting as claimed in claim 1, wherein the film material for optical glass cutting further comprises a PET layer; the PET layer is located the upper surface of glue film.
4. The film material for optical glass cutting according to claim 1, wherein the raw material for preparing the core layer further comprises a polyethylene oxide-acrylic acid copolymer.
5. The film material for optical glass cutting according to claim 1, wherein the polyolefin is selected from one or more of polyethylene, polypropylene, ethylene-propylene copolymer, polybutene-1, poly-4-methylpentene-1, ethylene-vinyl acetate copolymer, ethylene-ethyl (meth) acrylate copolymer, ethylene-methyl (meth) acrylate copolymer, and ethylene-acrylic acid copolymer.
6. The film material for optical glass cutting according to claim 1, wherein the elastomer is an ethylene-based elastomer or a propylene-based elastomer.
7. The film material for optical glass cutting as defined in claim 1, wherein the antistatic agent is a fatty acid amide.
8. The film material for optical glass cutting according to claim 1, wherein the adhesive layer is prepared from the following raw materials in parts by weight: 20-25 parts of butyl acrylate, 9-11 parts of isooctyl acrylate, 1-3 parts of acrylic acid, 2-4 parts of hydroxyethyl acrylate, 1-3 parts of piperidine ethanol methacrylate, 6-14 parts of an epoxy resin cross-linking agent, 0.15-0.35 part of an initiator, 58-62 parts of a solvent and 2-4 parts of a curing agent.
9. A method for preparing a film material for grinding and packaging semiconductors according to any one of claims 1 to 8, wherein the method is classified into a direct coating method and a rotary coating method.
10. Use of the film material for optical glass cutting according to any one of claims 1 to 8 for surface protection of optical glass, ceramics, LED display screens, 5G mobile phone screens, metal plates.
Priority Applications (1)
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CN201910963762.4A CN110628345A (en) | 2019-10-11 | 2019-10-11 | Film material for cutting optical glass |
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CN201910963762.4A CN110628345A (en) | 2019-10-11 | 2019-10-11 | Film material for cutting optical glass |
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