CN107012737A - A kind of preparation method of release liners - Google Patents

A kind of preparation method of release liners Download PDF

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Publication number
CN107012737A
CN107012737A CN201710260568.0A CN201710260568A CN107012737A CN 107012737 A CN107012737 A CN 107012737A CN 201710260568 A CN201710260568 A CN 201710260568A CN 107012737 A CN107012737 A CN 107012737A
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CN
China
Prior art keywords
preparation
mass ratio
release liners
adhesive
body paper
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Granted
Application number
CN201710260568.0A
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Chinese (zh)
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CN107012737B (en
Inventor
王明
陈家锵
邓家军
陈彦友
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JIANGSU JINDA PACKAGING MATERIAL TECHNOLOGY Co.,Ltd.
Original Assignee
JINDA PLASTIC CO Ltd SHANGHAI
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Priority to CN201710260568.0A priority Critical patent/CN107012737B/en
Publication of CN107012737A publication Critical patent/CN107012737A/en
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/001—Release paper
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C08G18/3206—Polyhydroxy compounds aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
    • C08G18/4269—Lactones
    • C08G18/4277—Caprolactone and/or substituted caprolactone
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67—Unsaturated compounds having active hydrogen
    • C08G18/671—Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • 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
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/10—Organic non-cellulose fibres
    • D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H13/26—Polyamides; Polyimides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H15/00—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
    • D21H15/02—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H15/00—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
    • D21H15/02—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
    • D21H15/10—Composite fibres
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/53—Polyethers; Polyesters
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/80—Paper comprising more than one coating
    • D21H19/82—Paper comprising more than one coating superposed
    • D21H19/824—Paper comprising more than one coating superposed two superposed coatings, both being non-pigmented
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/80—Paper comprising more than one coating
    • D21H19/84—Paper comprising more than one coating on both sides of the substrate
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
    • D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
    • D21H23/22—Addition to the formed paper
    • D21H23/52—Addition to the formed paper by contacting paper with a device carrying the material
    • D21H23/64—Addition to the formed paper by contacting paper with a device carrying the material the material being non-fluent at the moment of transfer, e.g. in form of preformed, at least partially hardened coating
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3415—Five-membered rings
    • C08K5/3417—Five-membered rings condensed with carbocyclic rings

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

A kind of preparation method of release liners, it is characterised in that the preparation including body paper, body paper surface coating, the preparation of adhesive is coated with adhesive, and the preparation of film layer, the preparation of release liners, preparation technology of the present invention is novel, can realize industrialized preparation.

Description

A kind of preparation method of release liners
Technical field
The present invention relates to a kind of preparation method of release liners.
Background technology
Adhesive material is seen everywhere in daily life, mostly with self-adhesive label, posting in time, Sticky Note, pressure-sensitive label Occur etc. form, be that, using paper, film or special material as fabric, the back side scribbles adhesive, to apply silicon base stock as protection sheet A kind of composite, and it is processed into finished product label through printing, cross cutting etc..Using when, it is only necessary to base stock is peeled off, gently one Press, you can be attached to the surface of various affixed objects, labelling machine automatic labeling on a production line can also be used.Adhesive sticker extensive use On extensive stock, such as medicine label, food labelling, wine label, battery label, outer container label, daily chemical products label.
With continuing to develop for society, requirement more and more higher of some clients to label will be used in multiple production processes When identical product information, the structure of this kind of label is usually two layers or multilayer labels, and the requirement to ground is also very harsh, from The quality of type power determines the quality of label, and the present invention had both prepared a kind of preparation technology novelty, and can realize industrialized preparation Method.
The content of the invention
The present invention is adopted the following technical scheme that：
1st, a kind of preparation method of release liners, its feature is being to comprise the following steps：
Step one, the preparation of body paper
According to mass ratio it is 2-4 by nanofiber material and chopped strand:3-8 is mixed, in high speed fluffer after mixing In discongest 2-6min, 0.5-1% polyethylene glycol oxide is added during discongesting, is manufactured paper with pulp quantification of 50g/ using handshcet former afterwards m2Fibrous web, be placed in after drying more than thermostatic chamber 24h carry out drying moisture, by dry moisture body paper carry out hot pressing at Reason, obtains body paper；
Step 2, body paper surface coating
Body paper is paved, PET, PP or PE particle are melted, afterwards using die head by PET, PP or PE after thawing Particle, which drenches, forms one layer of film plating layer after the one side in body paper, normal temperature cure 24h, the thickness of film layer is 20-100 microns；
Step 3, the preparation of adhesive
Step 4, is coated with adhesive
By the adhesive prepared by the another side application step three of the body paper of a face plated film in step 2, adhesive sticker is formed Layer, the coating weight of adhesive is 25 grams/m；
Step 5, the preparation of film layer
PET, PP or PE particle are melted, PET, PP or PE particle after thawing is drenched using die head do not done afterwards Thin film layer is formed on glue-line, after normal temperature cure 24h, the thickness of film layer is 20-100 microns；
Step 6, the preparation of release liners
The thin-film surface that step 5 is formed forms one layer of release layer using silicone oil mould release, and the coated weight of silicone oil is 20g/m2。
2nd, a kind of preparation method of release liners as claimed in claim 1, it is characterised in that nanofiber material in step one Preparation comprise the following steps：Pure water, eucalyptus pulp and calcium carbonate are using mass ratio as 10-15 first：50-60：3-8 is stirred Mixed slurry is mixed to prepare, NaBr, 2,2,6,6- tetramethyl piperidine oxides are added, stir obtained mixed liquor, wherein The mass ratio of NaBr, 2,2,6,6- tetramethyl piperidine oxides and mixed slurry is 5-10:1-2:80-120；Stir mixing After liquid, start that NaClO is added dropwise so that the pH value of mixed liquor is controlled in 9-10, and the reaction time is 1-3h, reaction is added after terminating and gone Ionized water carries out obtaining oxidation slurry after fully washing, by obtained oxidation slurry using nanometer homogenizer in 1000-3000bar Homogeneous obtains nanofiber slurry 3-8 times under pressure, will nanofiber slurry carry out drying dehydration processing after obtain nanofiber Material；Described chopped strand is selected from polyimides chopped strand；The temperature of described hot-pressing processing is 100-130 DEG C, hot pressing speed Spend for 1.2m/min, hot pressing pressure is 80-200N/mm.
3rd, a kind of preparation method of release liners as claimed in claim 1, it is characterised in that adhesive in step 3 Preparation comprises the following steps：
(a) base polyurethane prepolymer for use as
The ratio of 2,4- toluene di-isocyanate(TDI)s and the first solution using NCO/OH is mixed as 0.7-1.5 first, 60-80min is stirred under the conditions of 65 DEG C, 75 DEG C are warming up to, insulation reaction 30-60min obtains the solution of water white transparency, stops adding Base polyurethane prepolymer for use as is obtained after heat；
(b) preparation of modified polyurethane emulsion
By obtained base polyurethane prepolymer for use as and IPDI, polycaprolactone glycol, constant temperature is anti-at 90 DEG C Answer 1h；It is cooled to after 70 DEG C and adds 1-METHYLPYRROLIDONE reaction 3h, keeps 70 DEG C of temperature, the hydroxy-ethyl acrylate reaction of addition 1h, is cooled to after 45 DEG C plus people's potassium hydroxide solution is neutralized, and the pH for controlling product is 7.0 1 8.1, is then delayed under high velocity agitation Slow add after BDO, 30min can obtain milky liquid, both be modified polyaminoester emulsion；
(c) preparation of the acrylate copolymer containing terminal hydroxy group
The preparation of acrylate copolymer containing terminal hydroxy group：First at 40 DEG C by PPG, methyl methacrylate, third Acrylic monomer carries out mixing 30-60min, is warming up to 50 DEG C, is stirred in the case of adding the second solution, inflated with nitrogen in 65 DEG C 45min, obtains brown liquid, is precipitated in ethanol, and the product obtained after drying is that the acrylic acid containing terminal hydroxy group gathers Compound；
(d) preparation of adhesive
By the polyaminoester emulsion of foregoing prepared modification and acrylate copolymer and methyl methacrylate containing terminal hydroxy group Ester, butyl acrylate are using mass ratio as 3-7:2-6:1-3:1-2 is mixed, and stirs 30min at 45 DEG C, is warming up at 60 DEG C and is stirred Carbazole compound is added in the case of mixing 30-45min, inflated with nitrogen, temperature control is between 60-75 DEG C, insulation reaction 30- 60min, is cooled to 50 DEG C of addition azodiisobutyronitriles, stirs 40min, 2h is reacted between being warming up to 60-75 DEG C afterwards, naturally cold But to 40 DEG C, adhesive is obtained, the mass ratio of the polyaminoester emulsion of the modification, carbazole compound and azodiisobutyronitrile is 5-10:1-2:0.5-1。
4th, a kind of preparation method of release liners as claimed in claim 3, it is characterised in that polyurethane prepolymer in step 3 First solution described in the preparation of body is polyethylene glycol, dimethyl sulfoxide and methyl iso-butyl ketone (MIBK) with mass ratio 5-7:2-5:1-4's Mixed solution)
5th, a kind of preparation method of release liners as claimed in claim 3, it is characterised in that modified polyurethane in step 3 Base polyurethane prepolymer for use as described in the preparation of emulsion, IPDI, polycaprolactone glycol, 1-METHYLPYRROLIDONE, The mass ratio of hydroxy-ethyl acrylate and BDO is:10-20:1-3:2-3:1-2:0.5-2:1-2)
6th, a kind of preparation method of release liners as claimed in claim 3, it is characterised in that containing terminal hydroxy group in step 3 PPG described in the preparation of acrylate copolymer, methyl methacrylate, the quality of acrylic monomers and the second solution Than for 1-5:2-4:3-7:1-3.
7th, a kind of preparation method of release liners as claimed in claim 6, it is characterised in that second solution is by 2,2- Azo dihydroxymethyl propionitrile, dimethylformamide and sodium dihydrogen phosphate are using mass ratio as 3-4:1-2:0.2-0.5 is constituted.
8th, a kind of preparation method of release liners as claimed in claim 3, it is characterised in that carbazoles described in step 3 Compound is using the general structure as described in formula (1)：
Wherein R1 is selected from hydrogen, the carbochain of C1-6 length, alkene, R2, selected from hydrogen, amino, halogen.
Beneficial effect：
(1) in step one body paper preparation：It usually can just be mixed to prepare in the prior art after fiber and carry out being beaten-hot pressing The method of fractional steps is employed in standby coating paper, the present invention and carries out preparation coating paper, and mixed slurry is prepared first, is simply mixed, after Phase adds NaBr, 2,2,6,6- tetramethyl piperidine oxides, and (addition of the oxide causes nano-fiber material made from the later stage Be not in agglomeration), and must be controlled by pH value, prepare nanofiber slurry, by with polyimides chopped strand Mixing hot pressing obtains coating paper；Found by numerous studies, because nanofiber has larger reference area, paper can be strengthened Zhang Qiangdu, and cause the consistency enhancing of paper, gap is fewer (compared to the reduction 60% for not using nanofiber), research It has also been found that being risen to the content of nanofiber after certain phase, the intensity and gap rate of paper do not produce grade several levels but and become Change becomes comparison steadily, intensity, porosity, gas permeability and the warp of resulting paper when nanofiber material content is 35% Ji performance reaches most preferably；For described, " hot pressing speed is 1.2m/min ", and the hot pressing speed is compared to existing hot pressing speed It is quick a lot, found according to research in fiber containing nanofiber and according to the fibre furnish of the present invention, quick hot pressing institute The paper performance that can be reached, does not decline such as consistency, and has saved the plenty of time；As a result of nanofiber material Material, therefore quantification of 50g/m can be obtained2Fibrous web, the consistency of body paper is high, and the length of nanofiber material is 30- 100nm。
(2) in step 3 in the preparation process of base polyurethane prepolymer for use as：(a) it with the addition of dimethyl sulfoxide in the present invention and methyl be different Butyl ketone, the addition of both materials can be effectively promoted the formation of base polyurethane prepolymer for use as and (add above two by studying Material than the time short 10-15% required for the performed polymer that is worth to only by effective control NCo/OH ratios), by research It was found that when NCo/OH is 0.95, motion and the diffusivity of polymer segment can be strengthened so that strand is able to fully increase It is long, and hydrophilic chain extender need not be added, effectively improve the peel strength and water resistance of adhesive sticker, with the addition of dimethyl sulfoxide and The peel strength of adhesive sticker obtained by methyl iso-butyl ketone (MIBK) can enhance 15% compared to un-added；
(3) in step 3 in the preparation process of base polyurethane prepolymer for use as：(c) acroleic acid polymerization containing terminal hydroxy group is prepared in Thing, and added during preparation, homemade second solution, the addition of second solution can effectively lift adhesive sticker Boiling resistance energy, by adhesive sticker as 10h in 100 DEG C of steam, peel strength reduces peel strength after 5%, 24h and subtracted after taking-up Few 10%, it can effectively strengthen its boiling resistance energy；
(4) external had been reported that is reacted using base polyurethane prepolymer for use as with acrylate copolymer in the prior art, but It is so not all right in the preparation for adhesive sticker to be, present invention research finds obtained by being modified to base polyurethane prepolymer for use as Polyaminoester emulsion and prepared acrylate copolymer containing terminal hydroxy group, which carry out reaction, can obtain that performance is very excellent not to be done Glue material, and by being added in the preparation of adhesive, carbazole compound, the addition of the compound can strengthen this and not do The cold tolerance of glue, this be present invention firstly discovers that, also have specific requirement for the addition reaction time of the compound in addition Optimum proportioning for " carbazole compound is added in the case of inflated with nitrogen, temperature control is between 70 DEG C, insulation reaction 40min ", Pass through the process step of the invention so that the adhesive sticker when using for -67 DEG C peel strength without significant change.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.
A kind of preparation method of release liners, its feature is being to comprise the following steps：
Step one, the preparation of body paper
Pure water, eucalyptus pulp and calcium carbonate are using mass ratio as 10-15 first：50-60：3-8 be stirred be mixed to prepare it is mixed Slurry is closed, NaBr, 2,2,6,6- tetramethyl piperidine oxides are added, stir obtained mixed liquor, wherein NaBr, 2,2,6,6- The mass ratio of tetramethyl piperidine oxides and mixed slurry is 5-10:1-2:80-120；Stir after mixed liquor, start to be added dropwise NaClO so that the pH value of mixed liquor is controlled in 9-10, and the reaction time is 1-3h, addition deionized water is filled after reaction terminates Oxidation slurry is obtained after dividing washing, obtained oxidation slurry is used into nanometer homogenizer homogeneous 3- under 1000-3000bar pressure Obtain nanofiber slurry 8 times, will nanofiber slurry carry out drying dehydration processing after obtain nanofiber material；By nanofiber Material and chopped strand are 2-4 according to mass ratio:3-8 is mixed, and is discongested 2-6min in high speed fluffer after mixing, is discongested During add 0.5-1% polyethylene glycol oxide, manufactured paper with pulp quantification of 50g/m using handshcet former afterwards2Fibrous web, after drying It is placed in more than thermostatic chamber 24h and carries out drying moisture, the body paper for drying moisture is subjected to hot-pressing processing, body paper is obtained；Described is short Cut fiber and be selected from polyimides chopped strand；The temperature of described hot-pressing processing is 100-130 DEG C, and hot pressing speed is 1.2m/ Min, hot pressing pressure is 80-200N/mm.
Step 2, body paper surface coating
Body paper is paved, PET, PP or PE particle are melted, afterwards using die head by PET, PP or PE after thawing Particle, which drenches, forms one layer of film plating layer after the one side in body paper, normal temperature cure 24h, the thickness of film layer is 20-100 microns；
Step 3, the preparation of adhesive
Step 4, is coated with adhesive
By the adhesive prepared by the another side application step three of the body paper of a face plated film in step 2, adhesive sticker is formed Layer, the coating weight of adhesive is 25 grams/m；
Step 5, the preparation of film layer
PET, PP or PE particle are melted, PET, PP or PE particle after thawing is drenched using die head do not done afterwards Thin film layer is formed on glue-line, after normal temperature cure 24h, the thickness of film layer is 20-100 microns；
Step 6, the preparation of release liners
The thin-film surface that step 5 is formed forms one layer of release layer using silicone oil mould release, and the coated weight of silicone oil is 20g/m2；
The preparation of adhesive in step 3 comprises the following steps：
(a) base polyurethane prepolymer for use as
The ratio of 2,4- toluene di-isocyanate(TDI)s and the first solution using NCO/OH is mixed as 0.7-1.5 first, 60-80min is stirred under the conditions of 65 DEG C, 75 DEG C are warming up to, insulation reaction 30-60min obtains the solution of water white transparency, stops adding Base polyurethane prepolymer for use as is obtained after heat；
(b) preparation of modified polyurethane emulsion
By obtained base polyurethane prepolymer for use as and IPDI, polycaprolactone glycol, constant temperature is anti-at 90 DEG C Answer 1h；It is cooled to after 70 DEG C and adds 1-METHYLPYRROLIDONE reaction 3h, keeps 70 DEG C of temperature, the hydroxy-ethyl acrylate reaction of addition 1h, is cooled to after 45 DEG C plus people's potassium hydroxide solution is neutralized, and the pH for controlling product is 7.0 1 8.1, is then delayed under high velocity agitation Slow add after BDO, 30min can obtain milky liquid, both be modified polyaminoester emulsion；
(c) preparation of the acrylate copolymer containing terminal hydroxy group
The preparation of acrylate copolymer containing terminal hydroxy group：First at 40 DEG C by PPG, methyl methacrylate, third Acrylic monomer carries out mixing 30-60min, is warming up to 50 DEG C, is stirred in the case of adding the second solution, inflated with nitrogen in 65 DEG C 45min, obtains brown liquid, is precipitated in ethanol, and the product obtained after drying is that the acrylic acid containing terminal hydroxy group gathers Compound；
(d) preparation of adhesive
By the polyaminoester emulsion of foregoing prepared modification and acrylate copolymer and methyl methacrylate containing terminal hydroxy group Ester, butyl acrylate are using mass ratio as 3-7:2-6:1-3:1-2 is mixed, and stirs 30min at 45 DEG C, is warming up at 60 DEG C and is stirred Carbazole compound is added in the case of mixing 30-45min, inflated with nitrogen, temperature control is between 60-75 DEG C, insulation reaction 30- 60min, is cooled to 50 DEG C of addition azodiisobutyronitriles, stirs 40min, 2h is reacted between being warming up to 60-75 DEG C afterwards, naturally cold But to 40 DEG C, adhesive is obtained, the mass ratio of the polyaminoester emulsion of the modification, carbazole compound and azodiisobutyronitrile is 5-10:1-2:0.5-1。
The first solution described in the preparation of base polyurethane prepolymer for use as is polyethylene glycol, dimethyl sulfoxide and methyl tert-butyl in step 3 Base ketone is with mass ratio 5-7:2-5:1-4 mixed solution, preferably 6:3.7:2.7.
It is base polyurethane prepolymer for use as described in the preparation of modified polyurethane emulsion in step 3, IPDI, poly- Caprolactone diol, 1-METHYLPYRROLIDONE, the mass ratio of hydroxy-ethyl acrylate and BDO are:10-20:1-3:2-3:1- 2:0.5-2:1-2；It is preferred that 15:2.3:2.4:1.7:0.9:1.6；
PPG described in the preparation of acrylate copolymer containing terminal hydroxy group in step 3, methyl methacrylate, The mass ratio of acrylic monomers and the second solution is 1-5:2-4:3-7:1-3；It is preferred that 3.7:2.8:5:2.4.
Second solution by 2,2- azo dihydroxymethyls propionitrile, dimethylformamide and sodium dihydrogen phosphate using mass ratio as 3-4:1-2:0.2-0.5 is constituted, and preferably 3.5:1.7:0.4.
Carbazole compound described in step 3 is using the general structure as described in formula (1)：
Wherein R1 is selected from hydrogen, the carbochain of C1-6 length, alkene, R2, selected from hydrogen, amino, halogen；It is preferred that carbazole, N- ethyls Carbazole, AEC, 3- bromines carbazole or N- vinyl carbazoles, and its their compositions.
It should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that After the content of the invention lectured has been read, those skilled in the art can make various changes or modifications to the present invention, these The equivalent form of value equally falls within the application appended claims limited range.

Claims (8)

1. a kind of preparation method of release liners, its feature is being to comprise the following steps：
Step one, the preparation of body paper
According to mass ratio it is 2-4 by nanofiber material and chopped strand:3-8 is mixed, and is dredged after mixing in high speed fluffer 2-6min is solved, 0.5-1% polyethylene glycol oxide is added during discongesting, is manufactured paper with pulp quantification of 50g/m using handshcet former afterwards2's More than thermostatic chamber 24h is placed in after fibrous web, drying and carries out drying moisture, the body paper for drying moisture is subjected to hot-pressing processing, obtained To body paper；
Step 2, body paper surface coating
Body paper is paved, PET, PP or PE particle are melted, afterwards using die head by PET, PP or PE particle after thawing Drench and one layer of film plating layer is formed after the one side in body paper, normal temperature cure 24h, the thickness of film layer is 20-100 microns；
Step 3, the preparation of adhesive
Step 4, is coated with adhesive
By the adhesive prepared by the another side application step three of the body paper of a face plated film in step 2, non-drying glue layer, glue are formed The coating weight of glutinous agent is 25 grams/m；
Step 5, the preparation of film layer
PET, PP or PE particle are melted, afterwards drenched PET, PP or PE particle after thawing in non-drying glue layer using die head On, thin film layer is formed after normal temperature cure 24h, the thickness of film layer is 20-100 microns；
Step 6, the preparation of release liners
The thin-film surface that step 5 is formed is using silicone oil mould release one layer of release layer of formation, and the coated weight of silicone oil is 20g/ m2。
2. a kind of preparation method of release liners as claimed in claim 1, it is characterised in that the system of nanofiber material in step one It is standby to comprise the following steps：Pure water, eucalyptus pulp and calcium carbonate are using mass ratio as 10-15 first：50-60：3-8 is stirred mixing Mixed slurry is made, NaBr, 2,2,6,6- tetramethyl piperidine oxides are added, stir obtained mixed liquor, wherein NaBr, 2, The mass ratio of 2,6,6- tetramethyl piperidine oxides and mixed slurry is 5-10:1-2:80-120；Stir after mixed liquor, open Begin that NaClO is added dropwise so that the pH value of mixed liquor is controlled in 9-10, and the reaction time is 1-3h, reaction adds deionized water after terminating Carry out obtaining oxidation slurry after fully washing, obtained oxidation slurry is used into nanometer homogenizer under 1000-3000bar pressure Homogeneous obtains nanofiber slurry 3-8 times, will nanofiber slurry carry out drying dehydration processing after obtain nanofiber material；It is described Chopped strand be selected from polyimides chopped strand；The temperature of described hot-pressing processing is 100-130 DEG C, and hot pressing speed is 1.2m/min, hot pressing pressure is 80-200N/mm.
3. a kind of preparation method of release liners as claimed in claim 1, it is characterised in that the preparation of the adhesive in step 3 Comprise the following steps：
(a) base polyurethane prepolymer for use as
The ratio of 2,4- toluene di-isocyanate(TDI)s and the first solution using NCO/OH is mixed as 0.7-1.5 first, at 65 DEG C Under the conditions of stir 60-80min, be warming up to 75 DEG C, insulation reaction 30-60min obtains the solution of water white transparency, stop after heating To base polyurethane prepolymer for use as；
(b) preparation of modified polyurethane emulsion
By obtained base polyurethane prepolymer for use as and IPDI, polycaprolactone glycol isothermal reaction at 90 DEG C 1h；It is cooled to after 70 DEG C and adds 1-METHYLPYRROLIDONE reaction 3h, keeps 70 DEG C of temperature, the hydroxy-ethyl acrylate reaction of addition 1h, is cooled to after 45 DEG C and adds potassium hydroxide solution neutralization, and the pH for controlling product is 7.0-8.1, is then delayed under high velocity agitation Slow add after BDO, 30min can obtain milky liquid, both be modified polyaminoester emulsion；
(c) preparation of the acrylate copolymer containing terminal hydroxy group
The preparation of acrylate copolymer containing terminal hydroxy group：First at 40 DEG C by PPG, methyl methacrylate, acrylic acid Monomer carries out mixing 30-60min, is warming up to 50 DEG C, is stirred in the case of adding the second solution, inflated with nitrogen in 65 DEG C 45min, obtains brown liquid, is precipitated in ethanol, and the product obtained after drying is that the acrylic acid containing terminal hydroxy group gathers Compound；
(d) preparation of adhesive
By the polyaminoester emulsion of foregoing prepared modification and the acrylate copolymer containing terminal hydroxy group and methyl methacrylate, third Olefin(e) acid butyl ester is using mass ratio as 3-7:2-6:1-3:1-2 is mixed, and stirs 30min at 45 DEG C, is warming up at 60 DEG C and is stirred 30- Carbazole compound is added in the case of 45min, inflated with nitrogen, temperature control is between 60-75 DEG C, insulation reaction 30-60min, 50 DEG C of addition azodiisobutyronitriles are cooled to, 40min is stirred, reacts 2h between being warming up to 60-75 DEG C afterwards, naturally cool to 40 DEG C, obtain adhesive, the mass ratio of the polyaminoester emulsion of the modification, carbazole compound and azodiisobutyronitrile is 5-10: 1-2:0.5-1。
4. a kind of preparation method of release liners as claimed in claim 3, it is characterised in that base polyurethane prepolymer for use as in step 3 First solution described in preparation is polyethylene glycol, dimethyl sulfoxide and methyl iso-butyl ketone (MIBK) with mass ratio 5-7:2-5:1-4 mixing Solution.
5. a kind of preparation method of release liners as claimed in claim 3, it is characterised in that modified polyurethane emulsion in step 3 Preparation described in base polyurethane prepolymer for use as, IPDI, polycaprolactone glycol, 1-METHYLPYRROLIDONE, propylene The mass ratio of sour hydroxyl ethyl ester and BDO is:10-20:1-3:2-3:1-2:0.5-2:1-2.
6. a kind of preparation method of release liners as claimed in claim 3, it is characterised in that the propylene containing terminal hydroxy group in step 3 PPG described in the preparation of acid polymer, methyl methacrylate, the mass ratio of acrylic monomers and the second solution are 1-5:2-4:3-7:1-3。
7. a kind of preparation method of release liners as claimed in claim 6, it is characterised in that second solution is by 2,2- azos Dihydroxymethyl propionitrile, dimethylformamide and sodium dihydrogen phosphate are using mass ratio as 3-4:1-2:0.2-0.5 is constituted.
8. a kind of preparation method of release liners as claimed in claim 3, it is characterised in that carbazoles chemical combination described in step 3 Thing is using the general structure as described in formula (1)：
Wherein R1 is selected from hydrogen, the carbochain of C1-6 length, alkene, R2, selected from hydrogen, amino, halogen.
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CN109997578A (en) * 2019-04-23 2019-07-12 杭州德问贸易有限公司 A kind of high viscous tree whitening agent of environmental protection
CN112663377A (en) * 2020-12-22 2021-04-16 阿尔诺维根斯(衢州)特种纸有限公司 Preparation method of natural flexible transparent paper
CN114808540A (en) * 2022-05-18 2022-07-29 仙鹤股份有限公司 Preparation method of high-cleanness release paper
CN114905737A (en) * 2022-05-27 2022-08-16 苏州博理新材料科技有限公司 3D printing method and high-speed photocuring 3D printing equipment

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CN102476483A (en) * 2010-11-27 2012-05-30 福建恒安集团有限公司 Release material and preparation method thereof
CN102797195A (en) * 2012-08-06 2012-11-28 滁州云林数码影像耗材有限公司 Method for reducing organosilicon transfer of release paper
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CN201140561Y (en) * 2007-12-18 2008-10-29 张丽平 PET silicone oil thin film applying type release paper
KR101031866B1 (en) * 2010-10-21 2011-05-02 진현정 Carbon sheet for thermal diffusion utilizing metal foil and method for making the sheet
CN102476483A (en) * 2010-11-27 2012-05-30 福建恒安集团有限公司 Release material and preparation method thereof
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CN109997578A (en) * 2019-04-23 2019-07-12 杭州德问贸易有限公司 A kind of high viscous tree whitening agent of environmental protection
CN112663377A (en) * 2020-12-22 2021-04-16 阿尔诺维根斯(衢州)特种纸有限公司 Preparation method of natural flexible transparent paper
CN114808540A (en) * 2022-05-18 2022-07-29 仙鹤股份有限公司 Preparation method of high-cleanness release paper
CN114905737A (en) * 2022-05-27 2022-08-16 苏州博理新材料科技有限公司 3D printing method and high-speed photocuring 3D printing equipment
CN114905737B (en) * 2022-05-27 2024-02-06 苏州博理新材料科技有限公司 3D printing method and high-speed photo-curing 3D printing equipment

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