WO2023236784A1 - 一种阻隔热封纤维素膜及其制备方法和应用 - Google Patents

一种阻隔热封纤维素膜及其制备方法和应用 Download PDF

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Publication number
WO2023236784A1
WO2023236784A1 PCT/CN2023/096422 CN2023096422W WO2023236784A1 WO 2023236784 A1 WO2023236784 A1 WO 2023236784A1 CN 2023096422 W CN2023096422 W CN 2023096422W WO 2023236784 A1 WO2023236784 A1 WO 2023236784A1
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Prior art keywords
barrier
coating
adhesive
cellulose film
heat
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PCT/CN2023/096422
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English (en)
French (fr)
Inventor
李柯璇
王新
邱金江
王超
江修才
李萌
陈玉苹
石拓
刘敏
李连波
刘法光
姚瑞先
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山东恒联新材料股份有限公司
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Priority to GB2315180.6A priority Critical patent/GB2623887A/en
Publication of WO2023236784A1 publication Critical patent/WO2023236784A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/68—Particle size between 100-1000 nm
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/048—Forming gas barrier coatings
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D127/00—Coating compositions 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 a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions 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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/04—Coating compositions 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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C09D127/08—Homopolymers or copolymers of vinylidene chloride
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/02—Emulsion paints including aerosols
    • C09D5/024—Emulsion paints including aerosols characterised by the additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • 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
    • 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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • 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
    • C09J7/201—Adhesives in the form of films or foils characterised by their carriers characterised by the release coating composition on 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
    • 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
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02—Cellulose; Modified cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2427/00—Characterised by the use of 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 a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/04—Characterised by the use of 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2427/08—Homopolymers or copolymers of vinylidene chloride
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • C09J2301/12—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
    • 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
    • C09J2401/00—Presence of cellulose
    • C09J2401/006—Presence of cellulose in the substrate
    • 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
    • C09J2427/00—Presence of halogenated polymer
    • C09J2427/001—Presence of halogenated polymer in the barrier 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
    • C09J2427/00—Presence of halogenated polymer
    • C09J2427/005—Presence of halogenated polymer in the release coating
    • 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
    • C09J2433/00—Presence of (meth)acrylic polymer
    • 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
    • C09J2475/00—Presence of polyurethane

Definitions

  • the invention relates to the technical field of functional cellulose membranes, and in particular to a barrier heat-sealing cellulose membrane and its preparation method and application.
  • Regenerated cellulose membrane made from natural cellulose is biodegradable, green and environmentally friendly, and is an ideal environmentally friendly material.
  • the regenerated cellulose film as the base film, it is coated by dipping or scraping solvent-based coatings to produce a cellulose film with heat-sealing and barrier properties that can meet non-load-bearing and heat-sealing strength requirements of no more than 350g. /37mm application scenarios.
  • the object of the present invention is to provide a barrier heat-sealing cellulose film and its preparation method and application.
  • the bonding strength is high and meets the usage requirements; the water-based emulsion coating is applied, and the production process is environmentally friendly.
  • the invention provides a barrier heat-sealing cellulose film, which includes a barrier layer, a regenerated cellulose base film and an adhesive layer laminated in sequence;
  • the barrier layer is formed of a barrier coating, the barrier coating includes polyvinylidene chloride emulsion, a first anti-sticking agent and water;
  • the adhesive layer is formed from an adhesive coating, which includes an emulsion, a second anti-adhesive agent and water; the emulsion includes an acrylic emulsion and/or a polyurethane emulsion;
  • the mass ratio of the regenerated cellulose base film, barrier layer and adhesive layer is 77-87:4-8:9-15.
  • the moisture content of the barrier heat-sealing cellulose film is 5 to 6%.
  • the mass ratio of the polyvinylidene chloride emulsion and the first anti-adhesive agent in the barrier coating is 100:1-3.
  • the mass ratio of the acrylic emulsion and the second anti-adhesive agent in the adhesive coating is 100:0.5-1.5.
  • the basis weight of the regenerated cellulose base film is 30-60g/m 2 .
  • the invention provides a method for preparing the barrier heat-sealing cellulose film described in the above technical solution, which includes the following steps:
  • the barrier coating and adhesive coating are used to simultaneously double-side coat the two sides of the regenerated cellulose base film to form a barrier layer and an adhesive layer respectively, thereby obtaining a barrier heat-sealing cellulose film.
  • the simultaneous double-sided coating includes the following steps: using a pneumatic diaphragm pump to pump the barrier coating and the adhesive coating into the first coating tank and the second coating tank respectively, and using anilox roller coating to regenerate the fibers.
  • the base film is coated on both sides simultaneously.
  • the operating speed of the anilox roller coating is 70-95m/min;
  • the mesh number of the anilox roller for coating the barrier coating is 100 to 250 mesh; the dry coating amount of the barrier coating is 3 to 5g/m 2 ;
  • the mesh number of the anilox roller coated with the adhesive emulsion is 100 to 180 mesh; the dry coating amount of the adhesive coating is 4 to 7 g/m 2 .
  • the present invention provides the application of the barrier heat-sealing cellulose film described in the above technical solution or the barrier heat-sealing cellulose film obtained by the preparation method described in the above technical solution in the field of packaging.
  • the invention provides a barrier heat-sealing cellulose film, which includes a barrier layer, a regenerated cellulose base film and an adhesive layer laminated in sequence;
  • the barrier layer is formed of barrier coating, and the barrier coating includes polyvinylidene chloride emulsion , a first anti-adhesive agent and water;
  • the adhesive layer is formed of an adhesive coating, the adhesive coating includes an emulsion, a second anti-adhesive agent and water;
  • the emulsion includes an acrylic emulsion and/or a polyurethane emulsion.
  • Barrier heat sealing cellulose film has both high adhesion and barrier properties, and can be directly heat-pressed with paper products.
  • the provided barrier heat-sealing cellulose film has high self-adhesion and can be heat-pressed by itself to make packaging bags.
  • the packaging bags have high edge sealing strength and have good application prospects as packaging materials.
  • the basis weight of the barrier heat-sealing cellulose film provided by the present invention is 40-60g/m 2
  • the longitudinal tensile strength is >36N/15mm
  • the longitudinal elongation is >18%
  • the adhesive layer is consistent with the paper.
  • the adhesive strength of the product is >6N/15mm
  • the self-adhesive strength of the adhesive layer is >7N/15mm
  • the oxygen transmittance is ⁇ 5mL/(m 2 ⁇ 24h)
  • the water vapor permeability is ⁇ 12g/(m 2 ⁇ 24h)
  • the barrier layer Surface tension ⁇ 42 dyne, moisture content ⁇ 5.5wt%.
  • the present invention provides a method for preparing the barrier heat-sealing cellulose film described in the above technical solution.
  • the preparation method provided by the invention has simple operation, wide sources of preparation raw materials and low cost, and is suitable for industrial production.
  • the invention provides a barrier heat-sealing cellulose film, which includes a barrier layer, a regenerated cellulose base film and an adhesive layer laminated in sequence.
  • the barrier layer is formed from a barrier coating that includes polyvinylidene chloride emulsion, a first anti-sticking agent and water.
  • the polyvinylidene chloride (PVDC) emulsion is preferably purchased from Solvay in the United States.
  • the solid content of the polyvinylidene chloride emulsion is preferably 30 to 45%, more preferably 35 to 40%.
  • the first anti-adhesive agent preferably includes one or both of a wax anti-adhesive agent and a silica powder anti-adhesive agent;
  • the wax anti-adhesive agent is preferably Poligen WE-1 (BASF wax emulsion);
  • the particle size of the first anti-adhesive agent is preferably 100 to 300 nm, more preferably 150 to 200 nm.
  • the water preferably includes demineralized water.
  • the mass ratio of the polyvinylidene chloride emulsion and the first anti-adhesive agent in the barrier coating is preferably 100:1-3, more preferably 100:1.5-2.5, and further preferably 100:2.
  • the preparation method of the barrier coating preferably includes the following steps: mixing polyvinylidene chloride emulsion, a first anti-adhesive agent and water to obtain a barrier coating.
  • the mixing sequence is preferably to premix the first anti-sticking agent with water, and mix the obtained first anti-sticking agent liquid with the PVDC emulsion; the temperature of the pre-mixing is preferably room temperature, and the pre-mixing temperature is preferably room temperature.
  • the speed is preferably 500 ⁇ 1000r/min, more preferably 700 ⁇ 800r/min, the premixing time is preferably 5 ⁇ 15min, more preferably 10min, the premixing temperature is preferably room temperature; the mixed The speed is preferably 60-120r/min, more preferably 80-100r/min, and the mixing time is preferably 15-25min, more preferably It is preferably 20 minutes; the mixing temperature is preferably room temperature.
  • the thickness of the barrier layer is preferably 2 to 7 ⁇ m, more preferably 3 to 6 ⁇ m, and even more preferably 4 to 5 ⁇ m.
  • the adhesive layer is formed from an adhesive coating, which includes an emulsion, a second anti-adhesive agent and water; the emulsion includes an acrylic emulsion and/or a polyurethane emulsion.
  • the optional type and particle size of the second anti-adhesive agent are preferably the same as those of the first anti-adhesive agent, which will not be described again here.
  • the acrylic emulsion is preferably DSM water-based acrylic emulsion.
  • the solid content of the acrylic emulsion is preferably 30 to 45%, more preferably 35 to 40%.
  • the water preferably includes demineralized water.
  • the mass ratio of the acrylate emulsion and the second anti-adhesive agent in the adhesive coating is preferably 100:0.5-1.5, more preferably 100:0.8-1.2, and further preferably 100:1.
  • the preparation method of the adhesive coating preferably includes the following steps: mixing acrylate emulsion, a second anti-adhesive agent and water to obtain an adhesive coating.
  • the mixing sequence is preferably to premix the second anti-adhesive agent with water, and mix the obtained second anti-adhesive agent liquid with the acrylic emulsion;
  • the pre-mixing temperature is preferably room temperature, and the pre-mixing temperature is preferably room temperature.
  • the mixing speed is preferably 500 ⁇ 1000r/min, more preferably 700 ⁇ 800r/min, the premixing time is preferably 5 ⁇ 15min, more preferably 10min, the premixing temperature is preferably room temperature;
  • the mixing speed is preferably 60 to 120 r/min, more preferably 80 to 100 r/min, the mixing time is preferably 15 to 25 min, more preferably 20 min; the mixing temperature is preferably room temperature.
  • the thickness of the adhesive layer is preferably 4 to 7 ⁇ m, more preferably 4.5 to 6.5 ⁇ m, and even more preferably 5 to 6 ⁇ m.
  • the basis weight of the regenerated cellulose base film is preferably 30 to 60 g/m 2 , more preferably 35 to 55 g/m 2 , even more preferably 40 to 50 g/m 2 ; the regenerated cellulose base film
  • the thickness is preferably 20 to 40 ⁇ m, more preferably 27 to 35 ⁇ m.
  • the mass ratio of the regenerated cellulose base film, barrier layer and adhesive layer in the barrier heat-sealing cellulose film is preferably 77-87:4-8:9-15, more preferably 80-85: 5 to 7: 10 to 14, more preferably 82 to 83: 6 to 6.5: 12 to 13.
  • the moisture content of the barrier heat-sealing cellulose film is preferably 5 to 6%, more preferably 5.2 to 5.8%, and even more preferably 5.4 to 5.5%.
  • the invention provides a method for preparing the barrier heat-sealing cellulose film described in the above technical solution, which includes the following steps:
  • the present invention has no special limitations on the preparation method of the regenerated cellulose base film. It can be prepared by using preparation methods well known to those skilled in the art, such as carbon disulfide viscose method, literature (Jia Xiangjuan. NMMO/H 2 O solution method for preparing high adsorption Research on regenerated cellulose materials [D]. Shaanxi University of Science and Technology. The preparation method of regenerated cellulose membrane disclosed in ) or the direct dissolution of fiber through ionic liquid jointly developed by the Chinese Academy of Sciences and Shandong Henglian New Materials Co., Ltd. has achieved industrial production A method for producing a regenerated cellulose membrane is carried out.
  • the regenerated cellulose base film is preferably produced by the carbon disulfide viscose method.
  • the specific steps are as follows: alkalize the cellulose raw material and then yellow it to obtain cellulose xanthate, that is, viscose liquid;
  • the viscose liquid is sprayed into a film, and then placed in an acid coagulation regeneration bath for acid coagulation and regeneration to obtain a regenerated cellulose film.
  • the fiber raw material preferably includes cotton pulp, softwood or hardwood pulp.
  • the alkali solution for alkalization preferably includes sodium hydroxide solution; the concentration of the alkali solution is preferably 17.5 to 18.5 wt%, more preferably 18 wt%; the temperature of the alkalinization Preferably it is 45-65°C, more preferably 50-60°C.
  • the alkalization time is preferably 10-30 min, more preferably 15-25 min; during the alkalization process, cellulose and sodium hydroxide generate alkali cellulose .
  • the yellowing reagent for yellowing is preferably CS 2 ; the mass ratio of the alkali cellulose to the yellowing reagent is preferably 1:0.25-0.32 (based on the dosage at 20°C), more preferably The ratio is 1:0.3; the initial temperature of yellowing is preferably 20-30°C, more preferably 25°C; the time of yellowing is preferably 30-60min, more preferably 40-50min.
  • the acid coagulation regeneration bath preferably includes dilute sulfuric acid or dilute sulfuric acid-sodium sulfate mixed solution; the concentration of the dilute sulfuric acid is preferably 10 to 18 wt%, more preferably 12 to 15 wt%, and the dilute sulfuric acid- In the sodium sulfate mixed solution, the concentration of dilute sulfuric acid (i.e. H 2 SO 4 /H 2 O) is preferably 10 to 18 wt%, more preferably 12 to 15 wt%, and the concentration of sodium sulfate is preferably 230 to 260 g/L, more preferably 245 ⁇ 255g/L.
  • the fibrous viscose liquid preferably enters an acid coagulation regeneration bath through a spray slot former for acid coagulation regeneration.
  • the present invention sequentially performs pretreatment and softening and anti-adhesive treatment on the regenerated cellulose film to obtain a regenerated cellulose base film.
  • the pretreatment preferably includes: sequentially subjecting the regenerated cellulose membrane to a first water wash, Desulfurization, second washing, bleaching, dechlorination and third washing.
  • the number of the first water washing, the second water washing and the third water washing is preferably 1 to 6 times independently, and more preferably 2 to 4 times.
  • the desulfurization is preferably performed using an alkali solution, and the concentration of the alkali solution is preferably 1.5 to 3.5 g/L, more preferably 2 to 3 g/L; the alkali solution preferably includes an aqueous sodium hydroxide solution.
  • the bleaching agent preferably includes sodium hypochlorite, hydrogen peroxide or ozone, more preferably sodium hypochlorite, and the concentration is preferably 1 to 4 g/L, more preferably 1.5 to 2.5 g/L.
  • the dechlorination preferably includes demineralized water washing.
  • the softener-anti-sticking agent aqueous dispersion used in the softening and anti-sticking treatment includes a softener, an anti-sticking agent and water; the softener preferably includes polyol, and more preferably includes triethylene glycol or glycerin;
  • the anti-adhesive agent preferably includes nano-silica; the particle size of the anti-adhesive agent is preferably 5 to 600 nm, more preferably 80 to 100 nm.
  • the mass ratio of the softener to the anti-adhesive agent is preferably 30-50:1.5-5, more preferably 35-45:2-4.5, further preferably 40-45:3-4.
  • the water is preferably demineralized water.
  • the concentration of the softener in the softener-anti-sticking agent aqueous dispersion is preferably 30 to 50 g/L, more preferably 35 to 45 g/L, and even more preferably 40 to 45 g/L.
  • the present invention has no special limitation on the amount of the softener-anti-sticking agent aqueous dispersion, as long as the wet regenerated cellulose film can be immersed.
  • the temperature of the softening and anti-adhesive treatment is preferably 30-70°C, more preferably 45-55°C; the time of the softening and anti-adhesive treatment is preferably 10-20 s, more preferably 12-16 s.
  • the present invention preferably further includes sequentially drying and winding the regenerated cellulose film after the softening and anti-sticking treatment to obtain a regenerated cellulose base film.
  • the drying temperature is preferably 100-150°C, more preferably 120-140°C; the drying time is preferably 20-80s, more preferably 40-50s.
  • the present invention has no special limitation on the winding, and the winding operation well known to those skilled in the art can be used.
  • the present invention uses barrier coating and adhesive coating to simultaneously double-side coat both sides of the regenerated cellulose base film to form a barrier layer and an adhesive layer respectively, thereby obtaining a barrier heat-sealing cellulose film.
  • the simultaneous double-sided coating preferably includes the following steps: using a pneumatic diaphragm pump to pump the barrier coating and the adhesive coating into the first coating tank and the second coating tank respectively, and using anilox roller coating
  • the regenerated cellulose base film is coated on both sides simultaneously.
  • the anilox roller coated The operating speed is preferably 70 to 95 m/min, more preferably 75 to 90 m/min, and even more preferably 80 to 85 m/min.
  • the mesh number of the anilox roller for the barrier coating is preferably 100 to 250 mesh, more preferably 150 to 200 mesh; the dry coating amount of the barrier coating is preferably 3 to 250 mesh.
  • the anilox roller mesh number of the anilox roller coating of the adhesive coating is preferably 100 to 180 mesh, more preferably 130 to 150 mesh; the dry coating amount of the adhesive coating is preferably 4 to 7 g/m 2 , more preferably 4.5 to 6.5 g/m 2 , even more preferably 5 to 6 g/m 2 .
  • the present invention preferably further includes drying the obtained wet barrier heat-sealing cellulose film and then cooling and rolling it to obtain a barrier heat-sealing cellulose film.
  • the drying preferably includes pre-drying and drying in sequence.
  • the pre-drying preferably includes infrared drying; the temperature of the pre-drying is preferably 60-80°C, more preferably 70°C, and the pre-drying time is preferably 1.2-1.8 s, more preferably 1.4 ⁇ 1.5s.
  • the drying temperature is preferably 60 to 120°C, and more preferably 85 to 120°C.
  • the drying preferably includes horizontal drying; the horizontal drying is divided into eight zones, which are sequentially designated as zone one to zone eight.
  • the temperature of the first zone is preferably 85-95°C, more preferably 90°C, and the drying time of the first zone is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the temperature of the second zone is preferably 95-105°C, more preferably 100°C, and the drying time of the second zone is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the temperature of the three zones is preferably 105-115°C, more preferably 110°C, and the drying time of the three zones is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the temperature of the four zones is preferably 105-120°C, more preferably 110-115°C, and the drying time of the four zones is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the temperature of the five zones is preferably 95-105°C, more preferably 100°C, and the drying time of the five zones is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the temperature of the six zones is preferably 85-100°C, more preferably 90-95°C, and the drying time of the six zones is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the temperature of the seven zones is preferably 80-98°C, more preferably 90-95°C, and the drying time of the seven zones is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the temperature of the eight zones is preferably 85-95°C, more preferably 88-93°C, and the drying time of the eight zones is preferably 2.7-3.2s, more preferably 2.8-3.0s.
  • the heat-barrier cover of the wet barrier heat-sealing cellulose film is on the bottom and the adhesive layer is on the top.
  • the regenerated cellulose base film will curl to one side, causing the coating process to fail to proceed normally.
  • the present invention adopts pre-drying and horizontal drying. By controlling the temperature and vehicle speed in eight zones, the double-sided stress of the regenerated cellulose base film is balanced and the winding is smooth.
  • the temperature of the cooling laminating roller of the cooling winding is preferably 20 to 25°C, and more preferably 22 to 23°C.
  • the present invention provides the application of the barrier heat-sealing cellulose film described in the above technical solution or the barrier heat-sealing cellulose film obtained by the preparation method described in the above technical solution in the field of packaging.
  • the barrier heat-sealing cellulose film provided by the present invention can be directly heat-pressed with paper products, meeting the bonding strength requirements of coated paper to a certain extent; at the same time, the barrier heat-sealing cellulose film provided by the present invention has moisture and oxygen barrier properties. It has high stability, good fragrance retention, freshness retention and moisture resistance; moreover, the barrier heat-sealing cellulose film provided by the invention can also be heat-pressed by itself, has high bag-making edge sealing strength, and has good application as a packaging material. prospect.
  • the regenerated cellulose is sequentially washed with water, desulfurized in an alkali solution with a concentration of 1.5g/L at 80°C, washed with water, bleached in a sodium hypochlorite solution with a pH value of 9, and dechlorinated in demineralized water at room temperature. Wash with water, then place it in a softening bath, soften it in triethylene glycol-nanoscale silica aqueous dispersion at 50°C for 8 seconds, then dry at 130°C, adjust humidity and wind up to obtain the moisture content.
  • Simultaneous double-sided coating use a pneumatic diaphragm pump to pump the barrier coating and adhesive coating into the first coating tank and the second coating tank respectively, and use anilox roller coating to coat the regenerated cellulose
  • the base film is coated on both sides at the same time to obtain a wet barrier heat-sealing cellulose film; the operating speed is 90m/min, the mesh number of the coating anilox roller used for coating the barrier coating is 250 mesh, and the dry coating amount is 2.5 g/m 2 ; the mesh number of the anilox roller used for coating the adhesive coating is 150 mesh, and the dry coating amount is 6 g/m 2 .
  • the performance test results of the barrier heat-sealing cellulose film basis weight is 40g/m 2 ; longitudinal tensile strength is 36.85N/15mm; longitudinal elongation is 18.36%; adhesive layer and paper
  • the adhesive strength of the product is 6.58N/15mm; the adhesive layer's own adhesive strength is 7.3N/15mm; the oxygen transmittance is 5mL/(m 2 ⁇ 24h); the water vapor permeability is 12g/(m 2 ⁇ 24h); the barrier layer
  • the surface tension is 42 dyne; the moisture content is 5.2wt%.
  • a barrier heat-sealing cellulose film was prepared according to the method of Example 1. The difference from Example 1 is:
  • step (1) the quantification of the regenerated cellulose base film is 40g/m 2 , the concentration of triethylene glycol is 40g/L, and the concentration of nanoscale silica is 3g/L;
  • step (2) the mass ratio of the acrylic emulsion to the wax anti-adhesive agent in the adhesive coating is 100:1, and the solid content of the adhesive coating is 42%;
  • step (3) the mass ratio of PVDC emulsion to wax anti-adhesive agent in the barrier coating is 100:1, and the solid content of the barrier coating is 40%;
  • step (4) the operating speed is 80m/min, the mesh number of the coating anilox roller used for coating the barrier coating is 200 mesh, and the dry coating amount is 3g/m 2 ; the anilox roller used for coating the adhesive coating The mesh number is 100 mesh, and the dry coating amount is 6.5g/m 2 ;
  • step (5) the infrared drying temperature is 70°C and the time is 1.5 s; the cooling laminating roller temperature is 23°C.
  • the performance test results of the barrier heat-sealing cellulose film basis weight is 50g/m 2 ; longitudinal tensile strength is 52.63N/15mm; longitudinal elongation is 22.34%; adhesive layer and paper
  • the adhesive strength of the product is 7.21N/15mm; the adhesive layer's own adhesive strength is 7.8N/15mm; the oxygen transmittance is 3.8mL/(m 2 ⁇ 24h); the water vapor permeability is 9g/(m 2 ⁇ 24h); barrier
  • the surface tension of the layer is 42 dynes; the moisture content is 5.5 wt%.
  • a barrier heat-sealing cellulose film was prepared according to the method of Example 1. The difference from Example 1 is:
  • step (1) the quantification of the regenerated cellulose base film is 50g/m 2 , the concentration of triethylene glycol is 50g/L, and the concentration of nanoscale silica is 5g/L;
  • step (2) the mass ratio of the acrylic emulsion to the wax anti-adhesive agent in the adhesive coating is 100:1.5, and the solid content of the adhesive coating is 42%;
  • step (3) the mass ratio of PVDC emulsion to wax anti-adhesive agent in the barrier coating is 100:2, and the solid content of the barrier coating is 40%;
  • step (4) the operating speed is 75m/min, the mesh number of the coating anilox roller used for coating the barrier coating is 150 mesh, and the dry coating amount is 4g/ m2 ; the anilox roller used for coating the adhesive coating The mesh number is 50 mesh, and the dry coating amount is 6g/m 2 ;
  • step (5) the infrared drying temperature is 70°C and the time is 1.6s; the cooling laminating roller temperature The temperature is 25°C; the conditions for horizontal drying are shown in Table 2:
  • the performance test results of the barrier heat-sealing cellulose film basis weight is 60g/m 2 ; longitudinal tensile strength is 73.26N/15mm; longitudinal elongation is 43.65%; adhesive layer and paper
  • the adhesive strength of the product is 7.83N/15mm; the adhesive layer's own adhesive strength is 8.31N/15mm; the oxygen transmittance is 2.8mL/(m 2 ⁇ 24h); the water vapor permeability is 7g/(m 2 ⁇ 24h); barrier
  • the surface tension of the layer is 42 dynes; the moisture content is 5.4 wt%.
  • a barrier heat-sealing cellulose film was prepared according to the method of Example 3. The difference from Example 1 is:
  • step (1) the quantification of the regenerated cellulose base film is 50g/m 2 , the concentration of triethylene glycol is 50g/L, and the concentration of nanoscale silica is 5g/L;
  • step (2) is replaced with the barrier coating in step (3);
  • step (4) the barrier coating is coated on both sides, the mesh number of the coating anilox roller used is 200 mesh, and the dry coating amount on both sides is 2.5g/m 2 ;
  • step (5) the temperature of infrared drying is 80°C and the time is 1.6 seconds.
  • the performance test results of the barrier heat-sealing cellulose film basis weight is 60g/m 2 ; longitudinal tensile strength is 70.26N/15mm; longitudinal elongation is 41.65%; adhesive layer and paper
  • the adhesive strength of the product is 0N/15mm; the adhesive strength of the barrier layer itself is 1.9N/15mm; the oxygen transmittance is 6mL/(m 2 ⁇ 24h); the water vapor permeability is 25g/(m 2 ⁇ 24h); two layers of barrier layers
  • the surface tension is 42 dyne; the moisture content is 5.4wt%.
  • Example 3 By comparing Example 3 and Comparative Example 1, it can be seen that compared with the technology of the present invention, the bonding strength of the barrier heat-sealing cellulose film prepared in Comparative Example 1 to paper products and its own bonding strength do not meet the requirements of coated paper composite products, and are not suitable for special Application scenarios.

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Abstract

本发明提供了一种阻隔热封纤维素膜及其制备方法和应用，涉及功能纤维素膜技术领域。本发明提供的阻隔热封纤维素膜，包括依次层叠的阻隔层、再生纤维素基膜和粘合层，阻隔层由阻隔涂料(聚偏二氯乙烯乳液、第一抗粘剂和水)形成，粘合层由粘合涂料(乳液(丙烯酸酯乳液和/或聚氨酯乳液)、第二抗粘剂和水)形成。本发明提供的阻隔热封纤维素膜具有高粘合力和阻隔性，可直接与纸制品热压合，且与纸制品的粘贴强度高，达到淋膜纸的粘结强度使用要求；本发明提供的阻隔热封纤维素膜的阻湿性高、阻氧性高，具有优异的保香、保鲜性和防潮性；本发明提供的阻隔热封纤维素膜的自身热封强度高，能够自身热压合制成包装袋，且包装袋的封边强度高。

Description

一种阻隔热封纤维素膜及其制备方法和应用
本申请要求于2022年06月08日提交中国专利局、申请号为CN202210642715.1、发明名称为“一种阻隔热封纤维素膜及其制备方法和应用”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明涉及功能纤维素膜技术领域，具体涉及一种阻隔热封纤维素膜及其制备方法和应用。
背景技术
以天然纤维素为原料制得的再生纤维素膜，具有可生物降解、绿色环保的特点，是一种理想的环保材料。
以再生纤维素膜为基膜，通过浸涂或刮涂溶剂型涂料等方式进行涂布，制得具备热封、阻隔性能的纤维素膜，能满足非承重、热封强度要求不高于350g/37mm的应用场景。
随着禁塑令在全球范围内的不断推出，跨领域应用的再生纤维素功能膜，成为包装行业需求热点，但原有热封强度使其在很多用途上受限，如不能满足承重包装袋制作、不能替代淋膜热熔胶塑料膜完成纸膜复合包装产品的需求等类似高粘合力的应用。
发明内容
有鉴于此，本发明的目的在于提供一种阻隔热封纤维素膜及其制备方法和应用，本发明提供的阻隔热封纤维素膜与纸的粘合强度以及阻隔热封纤维素膜自身粘合强度高，满足使用要求；应用水性乳液涂层，生产过程环境友好。
为了实现上述发明目的，本发明提供以下技术方案：
本发明提供了一种阻隔热封纤维素膜，包括依次层叠的阻隔层、再生纤维素基膜和粘合层；
所述阻隔层由阻隔涂料形成，所述阻隔涂料包括聚偏二氯乙烯乳液、第一抗粘剂和水；
所述粘合层由粘合涂料形成，所述粘合涂料包括乳液、第二抗粘剂和水；所述乳液包括丙烯酸酯乳液和/或聚氨酯乳液；。
优选的，所述再生纤维素基膜、阻隔层和粘合层的质量比为77～87：4～8：9～15。
优选的，所述阻隔热封纤维素膜的含水率为5～6％。
优选的，所述阻隔涂料中聚偏二氯乙烯乳液和第一抗粘剂的质量比为100：1～3。
优选的，所述粘合涂料中丙烯酸酯乳液和第二抗粘剂的质量比为100：0.5～1.5。
优选的，所述再生纤维素基膜的定量为30～60g/m2。
本发明提供了上述技术方案所述阻隔热封纤维素膜的制备方法，包括以下步骤：
利用阻隔涂料和粘合涂料在再生纤维素基膜的两对面进行同时双面涂布，分别形成阻隔层和粘合层，得到阻隔热封纤维素膜。
优选的，所述同时双面涂布包括以下步骤：利用气动隔膜泵将阻隔涂料和粘合涂料分别泵至第一涂布槽和第二涂布槽内，采用网纹辊涂布对再生纤维素基膜进行同时双面涂布。
优选的，所述网纹辊涂布的运行车速为70～95m/min；
所述阻隔涂料的网纹辊涂布的网纹辊目数为100～250目；所述阻隔涂料的干态涂布量为3～5g/m2；
所述粘合乳的网纹辊涂布的网纹辊目数为100～180目；所述粘合涂料的干态涂布量为4～7g/m2。
本发明提供了上述技术方案所述阻隔热封纤维素膜或上述技术方案所述制备方法得到的阻隔热封纤维素膜在包装领域的应用。
本发明提供了一种阻隔热封纤维素膜，包括依次层叠的阻隔层、再生纤维素基膜和粘合层；所述阻隔层由阻隔涂料形成，所述阻隔涂料包括聚偏二氯乙烯乳液、第一抗粘剂和水；所述粘合层由粘合涂料形成，所述粘合涂料包括乳液、第二抗粘剂和水；所述乳液包括丙烯酸酯乳液和/或聚氨酯乳液。阻隔热封纤维素膜同时具有高粘合力和阻隔性，可以直接与纸制品热压合， 且与纸制品的粘贴强度以及力学强度高，在一定程度上满足淋膜纸的粘结强度使用要求；阻湿性高、阻氧性高，具有优异的保香、保鲜性和防潮性；本发明提供的阻隔热封纤维素膜的自身粘贴高，能够自身热压合制包装袋，且包装袋的封边强度高，作为包装材料具有很好的应用前景。如实施例测试结果所示，本发明提供的阻隔热封纤维素膜的定量为40～60g/m2，纵向抗张强度＞36N/15mm，纵向伸长率＞18％，粘合层跟纸制品粘贴强度＞6N/15mm，粘合层的自身粘贴强度＞7N/15mm，氧气透过率≤5mL/(m2·24h)，水汽渗透性≤12g/(m2·24h)；阻隔层的表面张力≥42达因，含水率≤5.5wt％。
本发明提供了上述技术方案所述阻隔热封纤维素膜的制备方法。本发明提供的制备方法，操作简单，制备原料来源广且成本低，适宜工业化生产。
具体实施方式
本发明提供了一种阻隔热封纤维素膜，包括依次层叠的阻隔层、再生纤维素基膜和粘合层。
在本发明中，所述阻隔层由阻隔涂料形成，所述阻隔涂料包括聚偏二氯乙烯乳液、第一抗粘剂和水。在本发明的具体实施例中，所述聚偏二氯乙烯(PVDC)乳液优选购买于美国苏威。在本发明中，所述聚偏二氯乙烯乳液的固含量优选为30～45％，更优选为35～40％。在本发明中，所述第一抗粘剂优选包括蜡抗粘剂和二氧化硅粉状抗粘剂中的一种或两种；所述蜡抗粘剂优选为Poligen WE-1(巴斯夫蜡乳液)；所述第一抗粘剂的粒径优选为100～300nm，更优选为150～200nm。在本发明中，所述水优选包括软化水。在本发明中，所述阻隔涂料中聚偏二氯乙烯乳液和第一抗粘剂的质量比优选为100：1～3，更优选为100：1.5～2.5，进一步优选为100：2。
在本发明中，所述阻隔涂料的制备方法优选包括以下步骤：将聚偏二氯乙烯乳液、第一抗粘剂和水混合，得到阻隔涂料。在本发明中，所述混合的顺序优选为将第一抗粘剂与水预混合，将所得第一抗粘剂液与PVDC乳液混合；所述预混合的温度优选为室温，所述预混合的速度优选为500～1000r/min，更优选为700～800r/min，所述预混合的时间优选为5～15min，更优选为10min，所述预混合的温度优选为室温；所述混合的速度优选为60～120r/min，更优选为80～100r/min，所述混合的时间优选为15～25min，更 优选为20min；所述混合的温度优选为室温。在本发明中，所述阻隔层的厚度优选为2～7μm，更优选为3～6μm，进一步优选为4～5μm。
在本发明中，所述粘合层由粘合涂料形成，所述粘合涂料包括乳液、第二抗粘剂和水；所述乳液包括丙烯酸酯乳液和/或聚氨酯乳液。在本发明中，所述第二抗粘剂的可选种类和粒径优选与所述第一抗粘剂相同，在此不再赘述。在本发明的具体实施例中，所述丙烯酸酯乳液优选为帝斯曼水性丙烯酸乳液。在本发明中，所述丙烯酸酯乳液的固含量优选为30～45％，更优选为35～40％。在本发明中，所述水优选包括软化水。在本发明中，所述粘合涂料中丙烯酸酯乳液和第二抗粘剂的质量比优选为100：0.5～1.5，更优选为100：0.8～1.2，进一步优选为100：1。在本发明中，所述粘合涂料的制备方法优选包括以下步骤：将丙烯酸酯乳液、第二抗粘剂和水混合，得到粘合涂料。在本发明中，所述混合的顺序优选为将第二抗粘剂与水预混合，将所得第二抗粘剂液与丙烯酸酯乳液混合；所述预混合的温度优选为室温，所述预混合的速度速度优选为500～1000r/min，更优选为700～800r/min，所述预混合的时间优选为5～15min，更优选为10min，所述预混合的温度优选为室温；所述混合的速度优选为60～120r/min，更优选为80～100r/min，所述混合的时间优选为15～25min，更优选为20min；所述混合的温度优选为室温。在本发明中，所述粘合层的厚度优选为4～7μm，更优选为4.5～6.5μm，进一步优选为5～6μm。
在本发明中，所述再生纤维素基膜的定量优选为30～60g/m2，更优选为35～55g/m2，进一步优选为40～50g/m2；所述再生纤维素基膜的厚度优选为20～40μm，更优选为27～35μm。
在本发明中，所述阻隔热封纤维素膜中再生纤维素基膜、阻隔层和粘合层的质量比优选为77～87：4～8：9～15，更优选为80～85：5～7：10～14，进一步优选为82～83：6～6.5：12～13。在本发明中，所述阻隔热封纤维素膜的含水率优选为5～6％，更优选为5.2～5.8％，进一步优选为5.4～5.5％。
本发明提供了上述技术方案所述阻隔热封纤维素膜的制备方法，包括以下步骤：
利用阻隔涂料和粘合涂料在再生纤维素基膜的两对面进行同时双面涂 布，分别形成阻隔层和粘合层，得到阻隔热封纤维素膜。
在本发明中，若无特殊说明，所有的原料组分均为本领域技术人员熟知的市售商品。
本发明对于所述再生纤维素基膜的制备方法没有特殊限定，采用本领域技术人员熟知的制备方法即可，具体如二硫化碳粘胶法、文献(贾向娟.NMMO/H2O溶液法制备高吸附再生纤维素材料的研究[D].陕西科技大学.)中公开的再生纤维素膜制备方法或已经实现产业化生产的中国科学院与山东恒联新材料有限公司联合开发的通过离子液体直接溶解纤维素并进行再生纤维素膜生产方法。
在本发明的具体实施例中，所述再生纤维素基膜优选采用二硫化碳粘胶法生产，具体步骤如下：将纤维素原料进行碱化后黄化，得到纤维素黄酸酯即粘胶原液；将所述粘胶原液进行喷膜，然后置于酸凝固再生浴中进行酸凝固再生，得到再生纤维素膜。在本发明中，所述纤维原料优选包括棉浆粕、针叶或阔叶木浆粕。在本发明中，所述碱化用碱液，所述碱液优选包括氢氧化钠溶液；所述碱液的浓度优选为17.5～18.5wt％，更优选为18wt％；所述碱化的温度优选为45～65℃，更优选为50～60℃，所述碱化的时间优选为10～30min，更优选为15～25min；所述碱化过程中纤维素与氢氧化钠生成碱纤维素。在本发明中，所述黄化用黄化试剂优选为CS2；所述碱纤维素与黄化试剂的质量比优选为1：0.25～0.32(以20℃下的用量为准)，更优选为1:0.3；所述黄化的初始温度优选为20～30℃，更优选为25℃；所述黄化的时间优选30～60min，更优选为40～50min。在本发明中，所述酸凝固再生浴优选包括稀硫酸或稀硫酸-硫酸钠混合溶液；所述稀硫酸的浓度优选为10～18wt％，更优选为12～15wt％，所述稀硫酸-硫酸钠混合溶液中，稀硫酸的浓度(即H2SO4/H2O)优选为10～18wt％，更优选为12～15wt％，硫酸钠的浓度优选230～260g/L，更优选为245～255g/L。在本发明中，所述纤维粘胶原液优选通过喷缝式成型器进入酸凝固再生浴中进行酸凝固再生。
得到再生纤维素膜后，本发明将所述再生纤维素膜依次进行预处理和软化抗粘处理，得到再生纤维素基膜。
在本发明中，所述预处理优选包括：将再生纤维素膜依次进行第一水洗、 脱硫、第二水洗、漂白、脱氯和第三水洗。在本发明中，所述第一水洗、第二水洗和第三水洗的次数独立地优选为1～6次，更优选为2～4次。在本发明中，所述脱硫优选利用碱液进行，所述碱液的浓度优选为1.5～3.5g/L，更优选为2～3g/L；所述碱液优选包括氢氧化钠水溶液。在本发明中，所述漂白用漂白剂优选包括次氯酸钠、过氧化氢或臭氧，更优选为次氯酸钠，浓度优选为1～4g/L，更优选为1.5～2.5g/L。在本发明中，所述脱氯优选包括软化水洗涤。
在本发明中，所述软化抗粘处理采用的软化剂-抗粘剂水分散液包括软化剂、抗粘剂和水；所述软化剂优选包括多元醇，更优选包括三甘醇或甘油；所述抗粘剂优选包括纳米二氧化硅；所述抗粘剂的粒径优选为5～600nm，更优选为80～100nm。在本发明中，所述软化剂与抗粘剂的质量比优选为30～50：1.5～5，更优选为35～45：2～4.5，进一步优选为40～45：3～4。在本发明中，所述水优选为软化水。在本发明中，所述软化剂-抗粘剂水分散液中软化剂的浓度优选为30～50g/L，更优选为35～45g/L，进一步优选为40～45g/L。本发明对于所述软化剂-抗粘剂水分散液的用量没有特殊限定，能够将所述湿再生纤维素膜浸没即可。在本发明中，所述软化抗粘处理的温度优选为30～70℃，更优选为45～55℃；所述软化抗粘处理的时间优选为10～20s，更优选为12～16s。
所述软化抗粘处理后，本发明优选还包括将所述软化抗粘处理后的再生纤维素膜依次进行干燥和收卷，得到再生纤维素基膜。在本发明中，所述干燥的温度优选为100～150℃，更优选为120～140℃；所述干燥的时间优选为20～80s，更优选为40～50s。本发明对于所述收卷没有特殊限定，采用本领域技术人员熟知的收卷操作即可。
得到再生纤维素基膜后，本发明利用阻隔涂料和粘合涂料在再生纤维素基膜的两对面进行同时双面涂布，分别形成阻隔层和粘合层，得到阻隔热封纤维素膜。
在本发明中，所述同时双面涂布优选包括以下步骤：利用气动隔膜泵将阻隔涂料和粘合涂料分别泵至第一涂布槽和第二涂布槽内，采用网纹辊涂布对所述再生纤维素基膜进行同时双面涂布。在本发明中，所述网纹辊涂布的 运行车速优选为70～95m/min，更优选为75～90m/min，进一步优选为80～85m/min。在本发明中，所述阻隔涂料的网纹辊涂布的网纹辊目数优选为100～250目，更优选为150～200目；所述阻隔涂料的干态涂布量优选为3～5g/m2，更优选为3.5～4.5g/m2，进一步优选为4g/m2。在本发明中，所述粘合涂料的网纹辊涂布的网纹辊目数优选为100～180目，更优选为130～150目；所述粘合涂料的干态涂布量优选为4～7g/m2，更优选为4.5～6.5g/m2，进一步优选为5～6g/m2。
所述同时双面涂布完成后，本发明优选还包括将所得湿阻隔热封纤维素膜进行干燥后冷却收卷，得到阻隔热封纤维素膜。在本发明中，所述干燥优选包括依次进行预干燥和干燥。在本发明中，所述预干燥优选包括红外线干燥；所述预干燥的温度优选为60～80℃，更优选为70℃，所述预干燥的时间优选为1.2～1.8s，更优选为1.4～1.5s。在本发明中，所述干燥的温度优选为60～120℃，更优选为85～120℃。在本发明中，所述干燥优选包括卧式干燥；所述卧式干燥分为八区，依次记为一区～八区。在本发明中，所述一区的温度优选为85～95℃，更优选为90℃，所述一区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述二区的的温度优选为95～105℃，更优选为100℃，所述二区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述三区的的温度优选为105～115℃，更优选为110℃，所述三区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述四区的的温度优选为105～120℃，更优选为110～115℃，所述四区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述五区的的温度优选为95～105℃，更优选为100℃，所述五区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述六区的温度优选为85～100℃，更优选为90～95℃，所述六区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述七区的温度优选为80～98℃，更优选为90～95℃，所述七区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述八区的温度优选为85～95℃，更优选为88～93℃，所述八区的干燥时间优选为2.7～3.2s，更优选为2.8～3.0s。在本发明中，所述干燥过程中，湿阻隔热封纤维素膜的阻隔热封面在下，所述粘合层面在上。在本发明中，所述干燥过程中，由于 再生纤维素基膜的两面涂布的乳液性质及干态涂布量不同，再生纤维素基膜干燥过程中会向一面卷曲，导致涂布过程无法正常进行，本发明采用预干燥和卧式干燥方式，通过控制八区的温度及车速，使得再生纤维素基膜的双面应力达到平衡，收卷平整。在本发明中，所述冷却收卷的冷却贴合辊温度优选20～25℃，更优选为22～23℃。
本发明提供了上述技术方案所述阻隔热封纤维素膜或上述技术方案所述制备方法得到的阻隔热封纤维素膜在包装领域的应用。本发明提供的阻隔热封纤维素膜可以直接与纸制品热压合，在一定程度上达到淋膜纸粘合强度使用要求；同时，本发明提供的阻隔热封纤维素膜的阻湿阻氧性高，具有良好的的保香、保鲜性和防潮性；而且，本发明提供的阻隔热封纤维素膜还可以自身热压合，制袋封边强度高，作为包装材料具有很好的应用前景。
下面将结合本发明中的实施例，对本发明中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
(1)将质量比为1：3的棉浆泊和木浆粕混合均匀，将所得混合浆泊与浓度为17.5wt％氢氧化钠溶液按照体积比为1：28的比例混合均匀，在45℃条件下碱化30min，将所得成碱纤维素与CS2按照质量比为1：0.28的比例混合均匀，在20℃条件下黄化60min，得到纤维粘胶原液；将所述纤维粘胶原液通过喷缝式成型器进入稀硫酸(浓度为12wt％)中，在50℃条件下进行酸凝固，得到再生纤维素。将所述再生纤维素依次进行水洗、在80℃、浓度为1.5g/L的碱液中脱硫，水洗，在pH值为9的次氯酸钠溶液中漂白，在室温条件下置于软化水中脱氯，水洗，然后置于浸入软化浴槽子中，在三甘醇-纳米级二氧化硅水分散液中50℃条件下软化处理8s，然后在130℃条件下干燥，调湿收卷，得到含水率为6.0％、定量为30g/m2的再生纤维素基膜；其中，三甘醇-纳米级二氧化硅水分散液中三甘醇的浓度为30g/L，纳米级二氧化硅的粒径为80nm，浓度为1.5g/L。
(2)将软化水与蜡抗粘剂(巴斯夫蜡乳液，PoligenWE-1)按质量比为 1：0.3的比例在1000r/min条件下搅拌10min，将所得蜡抗粘剂液与帝斯曼水性丙烯酸酯乳液在200r/min条件下搅拌10min，得到粘合涂料，在200r/min条件下储存备用；其中，粘合涂料中丙烯酸酯乳液与蜡抗粘剂的质量比为100:0.5，粘合涂料的固含量为42％，搅拌均匀后按照200r/min速度搅拌储存、备用。
(3)将软化水与蜡抗粘剂(巴斯夫蜡乳液，PoligenWE-1)按质量比为1：0.3的比例在在1000r/min条件下搅拌10min，将所得蜡抗粘剂液与PVDC乳液(购买于美国苏威)与抗粘剂在200r/min条件下搅拌10min，得到阻隔涂料，在200r/min条件下储存备用，其中，阻隔涂料中PVDC乳液与蜡抗粘剂的质量比为100:1.5，阻隔涂料的固含量为40％。
(4)同时双面涂布：利用气动隔膜泵将所述阻隔涂料和粘合涂料分别泵至第一涂布槽和第二涂布槽内，采用网纹辊涂布对所述再生纤维素基膜进行同时双面涂布，得到湿阻隔热封纤维素膜；其中，运行车速为90m/min，阻隔涂料的涂布所用涂布网纹辊目数为250目，干态涂布量2.5g/m2；粘合涂料的涂布所用网纹辊目数为150目，干态涂布量6g/m2。
(5)将所述湿阻隔热封纤维素膜在60℃条件下红外线干燥1.3s，然后置于烘道中，采用热风加热的卧式干燥方式进行干燥，在冷却贴合辊温度为20℃条件下进行冷却收卷，得到阻隔热封纤维素膜；
其中，卧式干燥条件如表1所示：
表1干燥条件
根据GB/T24695-2009测试方法，阻隔热封纤维素膜的性能测试结果：定量为40g/m2；纵向抗张强度为36.85N/15mm；纵向伸长率为18.36％；粘合层跟纸制品粘贴强度为6.58N/15mm；粘合层自身粘贴强度为7.3N/15mm；氧气透过率为5mL/(m2·24h)；水汽渗透性为12g/(m2·24h)；阻隔层的表面张力为42达因；含水率为5.2wt％。
实施例2
按照实施例1的方法制备阻隔热封纤维素膜，与实施例1的区别在于：
步骤(1)中，再生纤维素基膜的定量为40g/m2，三甘醇的浓度为40g/L，纳米级二氧化硅的浓度为3g/L；
步骤(2)中，粘合涂料中丙烯酸酯乳液与蜡抗粘剂的质量比为100:1，粘合涂料的固含量为42％；
步骤(3)中，阻隔涂料中PVDC乳液与蜡抗粘剂的质量比为100:1，阻隔涂料的固含量为40％；
步骤(4)中，运行车速为80m/min，阻隔涂料的涂布所用涂布网纹辊目数为200目，干态涂布量3g/m2；粘合涂料的涂布所用网纹辊目数为100目，干态涂布量6.5g/m2；
步骤(5)中，红外线干燥的温度为70℃，时间为1.5s；冷却贴合辊温度为23℃。
根据GB/T24695-2009测试方法，阻隔热封纤维素膜的性能测试结果：定量为50g/m2；纵向抗张强度为52.63N/15mm；纵向伸长率为22.34％；粘合层跟纸制品粘贴强度为7.21N/15mm；粘合层自身粘贴强度为7.8N/15mm；氧气透过率为3.8mL/(m2·24h)；水汽渗透性为9g/(m2·24h)；阻隔层的表面张力为42达因；含水率为5.5wt％。
实施例3
按照实施例1的方法制备阻隔热封纤维素膜，与实施例1的区别在于：
步骤(1)中，再生纤维素基膜的定量为50g/m2，三甘醇的浓度为50g/L，纳米级二氧化硅的浓度为5g/L；
步骤(2)中，粘合涂料中丙烯酸酯乳液与蜡抗粘剂的质量比为100:1.5，粘合涂料的固含量为42％；
步骤(3)中，阻隔涂料中PVDC乳液与蜡抗粘剂的质量比为100:2，阻隔涂料的固含量为40％；
步骤(4)中，运行车速为75m/min，阻隔涂料的涂布所用涂布网纹辊目数为150目，干态涂布量4g/m2；粘合涂料的涂布所用网纹辊目数为50目，干态涂布量6g/m2；
步骤(5)中，红外线干燥的温度为70℃，时间为1.6s；冷却贴合辊温 度为25℃；卧式干燥的条件如表2所示：
表2卧式干燥条件
根据GB/T24695-2009测试方法，阻隔热封纤维素膜的性能测试结果：定量为60g/m2；纵向抗张强度为73.26N/15mm；纵向伸长率为43.65％；粘合层跟纸制品粘贴强度为7.83N/15mm；粘合层自身粘贴强度为8.31N/15mm；氧气透过率为2.8mL/(m2·24h)；水汽渗透性为7g/(m2·24h)；阻隔层的表面张力为42达因；含水率为5.4wt％。
对比例1
按照实施例3的方法制备阻隔热封纤维素膜，与实施例1的区别在于：
步骤(1)中，再生纤维素基膜的定量为50g/m2，三甘醇的浓度为50g/L，纳米级二氧化硅的浓度为5g/L；
步骤(2)中粘合涂料替换为步骤(3)中的阻隔涂料；
步骤(4)中，双面涂布阻隔涂料，所用涂布网纹辊目数为200目，两面的干态涂布量均为2.5g/m2；
步骤(5)中，红外线干燥的温度为80℃，时间为1.6s。
根据GB/T24695-2009测试方法，阻隔热封纤维素膜的性能测试结果：定量为60g/m2；纵向抗张强度为70.26N/15mm；纵向伸长率为41.65％；粘合层跟纸制品粘贴强度为0N/15mm；阻隔层自身粘贴强度为1.9N/15mm；氧气透过率为6mL/(m2·24h)；水汽渗透性为25g/(m2·24h)；两层阻隔层的表面张力均42达因；含水率为5.4wt％。
通过比较实施例3和对比例1可知，对比本发明技术，对比例1制备的阻隔热封纤维素膜与纸制品粘贴强度以及自身粘贴强度都没有达到淋膜纸复合制品的要求，不适合特殊应用场景使用。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (20)

  1. 一种阻隔热封纤维素膜，包括依次层叠的阻隔层、再生纤维素基膜和粘合层；
    所述阻隔层由阻隔涂料形成，所述阻隔涂料包括聚偏二氯乙烯乳液、第一抗粘剂和水；
    所述粘合层由粘合涂料形成，所述粘合涂料包括乳液、第二抗粘剂和水；所述乳液包括丙烯酸酯乳液和/或聚氨酯乳液；
  2. 根据权利要求1所述的阻隔热封纤维素膜，其特征在于，所述再生纤维素基膜、阻隔层和粘合层的质量比为77～87：4～8：9～15。
  3. 根据权利要求1或2所述的阻隔热封纤维素膜，其特征在于，所述阻隔热封纤维素膜的含水率为5～6％。
  4. 根据权利要求1或2所述的阻隔热封纤维素膜，其特征在于，所述阻隔涂料中聚偏二氯乙烯乳液和第一抗粘剂的质量比为100：1～3。
  5. 根据权利要求4所述的阻隔热封纤维素膜，其特征在于，所述聚偏二氯乙烯乳液的固含量为30～45％。
  6. 根据权利要求4所述的阻隔热封纤维素膜，其特征在于，所述第一抗粘剂包括蜡抗粘剂和二氧化硅粉状抗粘剂中的一种或两种；所述第一抗粘剂的粒径为100～300nm。
  7. 根据权利要求1、2、5或6所述的阻隔热封纤维素膜，其特征在于，所述阻隔层的厚度为2～7μm。
  8. 根据权利要求1或2所述的阻隔热封纤维素膜，其特征在于，所述粘合涂料中丙烯酸酯乳液和第二抗粘剂的质量比为100：0.5～1.5。
  9. 根据权利要求8所述的阻隔热封纤维素膜，其特征在于，所述丙烯酸酯乳液的固含量为30～45％。
  10. 根据权利要求8所述的阻隔热封纤维素膜，其特征在于，所述第一抗粘剂包括蜡抗粘剂和二氧化硅粉状抗粘剂中的一种或两种；所述第二抗粘剂的粒径为100～300nm。
  11. 根据权利要求1、2、9或10所述的阻隔热封纤维素膜，其特征在于，所述粘合层的厚度为4～7μm。
  12. 根据权利要求1或2所述的阻隔热封纤维素膜，其特征在于，所述 再生纤维素基膜的定量为30～60g/m2。
  13. 根据权利要求12所述的阻隔热封纤维素膜，其特征在于，所述再生纤维素基膜的厚度为20～40μm。
  14. 权利要求1～13任一项所述阻隔热封纤维素膜的制备方法，其特征在于，包括以下步骤：
    利用阻隔涂料和粘合涂料在再生纤维素基膜的两对面进行同时双面涂布，分别形成阻隔层和粘合层，得到阻隔热封纤维素膜。
  15. 根据权利要求14所述的制备方法，其特征在于，所述同时双面涂布包括以下步骤：利用气动隔膜泵将阻隔涂料和粘合涂料分别泵至第一涂布槽和第二涂布槽内，采用网纹辊对再生纤维素基膜进行同时双面涂布。
  16. 根据权利要求15所述的制备方法，其特征在于，所述网纹辊涂布的运行车速为70～95m/min；
    所述阻隔涂料的网纹辊涂布的网纹辊目数为100～250目；所述阻隔涂料的干态涂布量为3～5g/m2；
    所述粘合乳的网纹辊涂布的网纹辊目数为100～180目；所述粘合涂料的干态涂布量为4～7g/m2。
  17. 根据权利要求14、15或16所述的制备方法，其特征在于，所述同时双面涂布后还包括：将所得湿阻隔热封纤维素膜进行干燥后冷却收卷。
  18. 根据权利要求17所述的制备方法，其特征在于，所述干燥包括依次进行预干燥和干燥；所述预干燥包括红外线干燥；所述预干燥的温度为60～80℃，时间为1.2～1.8s；所述干燥的温度为60～120℃。
  19. 根据权利要求18所述的制备方法，其特征在于，所述干燥为卧式干燥；所述卧式干燥分为八区，依次记为一区～八区，所述一区的温度为85～95℃，所述二区的的温度为95～105℃，所述三区的的温度为105～115℃，所述四区的的温度为105～120℃，所述五区的的温度为95～105℃，所述六区的温度为85～100℃，所述七区的温度为80～98℃，所述八区的温度为85～95℃。
  20. 权利要求1～13任一项所述阻隔热封纤维素膜或权利要求14～19任一项所述制备方法得到的阻隔热封纤维素膜在包装领域的应用。
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