CN109206904A - A kind of preparation method of synthetic wax - Google Patents
A kind of preparation method of synthetic wax Download PDFInfo
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- CN109206904A CN109206904A CN201810974837.4A CN201810974837A CN109206904A CN 109206904 A CN109206904 A CN 109206904A CN 201810974837 A CN201810974837 A CN 201810974837A CN 109206904 A CN109206904 A CN 109206904A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- 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
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- 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
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1035—Preparatory processes from tetracarboxylic acids or derivatives and diisocyanates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of preparation methods of synthetic wax.By addition polyimides and a variety of wax sources, a kind of complex wax is prepared, has the features such as high rigidity, high-melting-point, high wearability by product prepared by the preparation method of synthetic wax of the embodiment of the present invention, has broad application prospects in coating and field of printing and dyeing.
Description
Technical field
The present invention relates to a kind of preparation methods of synthetic wax, belong to the preparation technical field of macromolecule synthesising wax.
Background technique
Macromolecule wax, is a kind of chemical materials formed by Polymer Processing agent, and quality is the small microballon shape/piece of white
Shape has the characteristics that fusing point compared with high, hardness is big, glossiness is high, color is snow-white.The most common synthetic wax is polyethylene wax, poly- second
Alkene wax and polyethylene, polypropylene, poly- cerinic acid ethylene, EP rubbers, butyl rubber intermiscibility are good, can improve polyethylene, polypropylene,
The release property of the mobility and polymethyl methacrylate of ABS, polycarbonate.Polyethylene wax is widely used in the low molecule of coating
Weight northylen homopolymer or copolymer, as a kind of additive can be applied directly to polyolefin processing in, increase product gloss and
Processing performance;As lubricant, chemical property is stable, electrical property is good.Can be used for producing powdery paints, can lacquer,
UV solidification, metal finishing coating, high glaze solvent reducible coatings, water paint, cardboard moisture-proof coating, solvent borne base gravure ink, stone
Print/offset printing, ink, set print-polishing oil.
However the fusing point of general polyethylene wax is between 101 DEG C -110 DEG C, therefore the fusing point by polyethylene wax is limited,
The fusing point of micronized polyethylene wax micro mist is extremely difficult to 110 DEG C or more.And since the quality of material polyethylene wax is softer, cause ultra-fine
The wearability of polyethylene wax micro mist product is poor, is unable to satisfy in the field micronized polyethylene wax micro powder product for requiring wearability high
User demand.Needle penetration is to indicate one of important indicator of performance of hardness, if needle penetration is larger, then it represents that its hardness compared with
It is small, indicate that its hardness is larger if needle penetration is smaller, needle penetration, that is, material hardness of micronized polyethylene wax micro mist can not basis
Different application demands are adjusted flexibly.Such as upper optical arena requires the hardness of polyethylene wax larger to improve glazing agent
Wiping properties are then difficult to meet the requirement of user so if the hardness of polyethylene wax is smaller.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation method of synthetic wax, add polyimides and
A variety of wax sources, are prepared a kind of complex wax, have the features such as high rigidity, high-melting-point, high wearability, in coating and field of printing and dyeing
It has broad application prospects.
In order to achieve the above objectives, the invention adopts the following technical scheme:
The embodiment of the invention provides a kind of preparation methods of synthetic wax, comprising the following steps: 1) it is pre- to prepare polyimides
Aggressiveness: the dimethyl sulfoxide saturated solution of preparation aromatic dianhydride under room temperature, preparation aromatic diamine and isocyanates
Saturated solution stirs under oil bath heating to be reacted, and reaction temperature is 70-90 DEG C, is warming up to 140 after sustained response 30min
DEG C, then cool down after reacting 30min, is cooled to and is stored at room temperature 2~3h and obtains polyimide prepolymer;2) by polyimide prepolymer
Catalyst is mixed in a solvent and added with polyethylene wax, polypropylene wax and stearmide, heats and is stirred;3) it will stir evenly
Mixture afterwards is pulverized, and synthetic wax of the invention is obtained.
Further, the solvent is n,N-Dimethylformamide, n,N-dimethylacetamide, N- methyl -2- pyrroles
One of alkanone, N- ethyl-2-pyrrolidone are a variety of.
Further, the catalyst is one of p-methyl benzenesulfonic acid, methane sulfonic acid, 3- toluenesulfonic acid or more
Kind.
Further, the stearmide is that the amides such as ethylene bis stearamide, erucyl amide or oleamide have
Machine compound.
Further, the polyethylene wax and polypropylene wax molecular weight ranges are from 2000-20000.
Gained synthetic wax partial size is between 50-100 microns.
Advantageous effects of the invention: the present invention is double stearic by polyethylene wax and polyimides, polypropylene wax, ethylene
The mixing of the wax materials such as amide, then Superfines Polymeric Wax Powder is produced using crushing, screening technology.
Polyacrylamide has the characteristics that high-melting-point, high intensity, addition polyacrylamide performed polymer make polyacrylamide
It is preferably merged with various wax sources in the course of the polymerization process, improves the overall mechanical properties of synthetic wax, extend its application field.
The softening point of polypropylene wax is apparently higher than polyethylene wax, have high rigidity, toughness lubricity is good, moisture-proof is good and
The wide equal excellent performances of melt viscosity range of choice, high-crystallinity is with brilliant brightness and glossiness.Polypropylene wax can be with
For paraffin modification agent, the pigment dispersing agent of Masterbatch, plastic additive, hot melt adhesive, easer, paper conversion auxiliary agent, rubber
Glue processing aid etc..
Ethylene bis stearamide and erucyl amide of the present invention, oleamide are common lubricants, are had both excellent
Internal lubrication and external lubrication effect.Above-mentioned substance is added in wax, can improve the property of wax layer;In addition, being answered in synthetic wax
Resistance to salt water, water resistance can be improved for addition above-mentioned substance in coating and paint and improve Baking Paint smoothness of the surface.
Product hardness height, the softening point height, good luster, partial size prepared by the preparation method of synthetic wax of the embodiment of the present invention
Small, at low cost, treating capacity is big, simple process.
Specific embodiment
The invention will be further described combined with specific embodiments below.Following embodiment is only used for clearly illustrating
Technical solution of the present invention, and not intended to limit the protection scope of the present invention.
" part " mentioned in following embodiment is calculated with weight fraction.
Embodiment 1
Polyimide prepolymer is prepared first: weighing 1 part 3 under room temperature, 3 ' 4,4 '-benzophenone tetracarboxylic dianhydrides,
Preparing in dimethyl sulfoxide solvent becomes saturated solution.10 parts of polyisocyanates are weighed, is configured to saturated solution with o-phenylenediamine
It is added in oil bath magnetic stirring apparatus and is reacted simultaneously, reaction temperature is 70 DEG C, reaction time 30min, and revolving speed is
Then 1500r/min raises the temperature to 140 DEG C, reaction time 30min, carries out under conditions of nitrogen protection, revolving speed is
1000r/min is cooled to and is stored at room temperature 3h and obtains polyimide prepolymer.According to relevant criterion to the knot of polyimide prepolymer
Structure is characterized.Polyimide prepolymer and polyethylene wax, polypropylene wax and ethylene bis stearamide are blended in N, N- diformazan
In base formamide and p-methyl benzenesulfonic acid is added, heat and is stirred.Mixture after mixing evenly is pulverized, is obtained
The synthetic wax that partial size is 50 microns.
Embodiment 2
Polyimide prepolymer is prepared first: weighing 1 part 3 under room temperature, 3 ' 4,4 '-benzophenone tetracarboxylic dianhydrides,
Preparing in dimethyl sulfoxide solvent becomes saturated solution.10 parts of polyisocyanates are weighed, is configured to saturated solution with o-phenylenediamine
It is added in oil bath magnetic stirring apparatus and is reacted simultaneously, reaction temperature is 70 DEG C, reaction time 30min, and revolving speed is
Then 1500r/min raises the temperature to 140 DEG C, reaction time 30min, carries out under conditions of nitrogen protection, revolving speed is
1000r/min is cooled to and is stored at room temperature 3h and obtains polyimide prepolymer.According to relevant criterion to the knot of polyimide prepolymer
Structure is characterized.Polyimide prepolymer and polyethylene wax, polypropylene wax and erucyl amide are blended in N, N- dimethylacetamide
In amine and methane sulfonic acid is added, heat and is stirred.Mixture after mixing evenly is pulverized, obtaining partial size is 100
The synthetic wax of micron.
Embodiment 3
Polyimide prepolymer is prepared first: weighing 1 part 3 under room temperature, 3 ' 4,4 '-benzophenone tetracarboxylic dianhydrides,
Preparing in dimethyl sulfoxide solvent becomes saturated solution.10 parts of polyisocyanates are weighed, is configured to saturated solution with o-phenylenediamine
It is added in oil bath magnetic stirring apparatus and is reacted simultaneously, reaction temperature is 70 DEG C, reaction time 30min, and revolving speed is
Then 1500r/min raises the temperature to 140 DEG C, reaction time 30min, carries out under conditions of nitrogen protection, revolving speed is
1000r/min is cooled to and is stored at room temperature 3h and obtains polyimide prepolymer.According to relevant criterion to the knot of polyimide prepolymer
Structure is characterized.Polyimide prepolymer and polyethylene wax, polypropylene wax and erucyl amide are blended in N, N- dimethylacetamide
In amine and methane sulfonic acid is added, heat and is stirred.Mixture after mixing evenly is pulverized, obtaining partial size is 100
The synthetic wax of micron.
Embodiment 4
Polyimide prepolymer is prepared first: weighing 1 part 3 under room temperature, 3 ' 4,4 '-benzophenone tetracarboxylic dianhydrides,
Preparing in dimethyl sulfoxide solvent becomes saturated solution.10 parts of polyisocyanates are weighed, is configured to saturated solution with o-phenylenediamine
It is added in oil bath magnetic stirring apparatus and is reacted simultaneously, reaction temperature is 70 DEG C, reaction time 30min, and revolving speed is
Then 1500r/min raises the temperature to 140 DEG C, reaction time 30min, carries out under conditions of nitrogen protection, revolving speed is
1000r/min is cooled to and is stored at room temperature 3h and obtains polyimide prepolymer.According to relevant criterion to the knot of polyimide prepolymer
Structure is characterized.Polyimide prepolymer and polyethylene wax, polypropylene wax and oleamide are blended in N, N- dimethylacetamide
In amine and methane sulfonic acid is added, heat and is stirred.Mixture after mixing evenly is pulverized, obtaining partial size is 100
The synthetic wax of micron.
Embodiment 5
Polyimide prepolymer is prepared first: weighing 1 part 3 under room temperature, 3 ' 4,4 '-benzophenone tetracarboxylic dianhydrides,
Preparing in dimethyl sulfoxide solvent becomes saturated solution.10 parts of polyisocyanates are weighed, is configured to saturated solution with o-phenylenediamine
It is added in oil bath magnetic stirring apparatus and is reacted simultaneously, reaction temperature is 70 DEG C, reaction time 30min, and revolving speed is
Then 1500r/min raises the temperature to 140 DEG C, reaction time 30min, carries out under conditions of nitrogen protection, revolving speed is
1000r/min is cooled to and is stored at room temperature 3h and obtains polyimide prepolymer.According to relevant criterion to the knot of polyimide prepolymer
Structure is characterized.Polyimide prepolymer and polyethylene wax, polypropylene wax and erucyl amide are blended in N- methyl -2- pyrrolidines
In ketone and 3- toluenesulfonic acid is added, heats and stirs.Mixture after mixing evenly is pulverized, obtaining partial size is
50 microns of synthetic wax.
Embodiment 6
Polyimide prepolymer is prepared first: weighing 1 part 3 under room temperature, 3 ' 4,4 '-benzophenone tetracarboxylic dianhydrides,
Preparing in dimethyl sulfoxide solvent becomes saturated solution.10 parts of polyisocyanates are weighed, is configured to saturated solution with o-phenylenediamine
It is added in oil bath magnetic stirring apparatus and is reacted simultaneously, reaction temperature is 70 DEG C, reaction time 30min, and revolving speed is
Then 1500r/min raises the temperature to 140 DEG C, reaction time 30min, carries out under conditions of nitrogen protection, revolving speed is
1000r/min is cooled to and is stored at room temperature 3h and obtains polyimide prepolymer.According to relevant criterion to the knot of polyimide prepolymer
Structure is characterized.Polyimide prepolymer and polyethylene wax, polypropylene wax and oleamide are blended in N- ethyl -2- pyrrolidines
In ketone and toluenesulfonic acid is added, heat and is stirred.Mixture after mixing evenly is pulverized, obtaining partial size is 75
The synthetic wax of micron.
Comparative example 1
Polyimide prepolymer and catalyst are not added, remaining condition is same as Example 1.
Comparative example 2
Stearoyl aminated compounds is not added, remaining condition is same as Example 1.
Comparative example 3
Polypropylene wax is not added, remaining condition is same as Example 1.
The mechanical property of test product by taking embodiment 1 as an example, with comparative example comparing result such as the following table 1
Needle penetration (25 DEG C, 100g) | Softening point (DEG C) | |
Embodiment 1 | 0.05 | 187 |
Comparative example 1 | 0.5 | 130 |
Comparative example 2 | 0.2 | 163 |
Comparative example 3 | 0.1 | 172 |
It can be seen that the product that preparation method of the present invention is prepared has the advantages that hardness is high, softening point is high, partial size is small.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations
Also it should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of synthetic wax, which is characterized in that 1) prepare polyimide prepolymer: preparing fragrance under room temperature
The dimethyl sulfoxide saturated solution of race's dianhydride, the saturated solution for preparing aromatic diamine and isocyanates stir under oil bath heating
It is reacted, reaction temperature is 70-90 DEG C, is warming up to 140 DEG C after sustained response 30min, then cool down after reacting 30min, cooling
Polyimide prepolymer is obtained to 2~3h is stored at room temperature;2) by polyimide prepolymer and polyethylene wax, polypropylene wax and tristearin
Amide mixes in a solvent and adds catalyst, heat and stir;3) mixture after mixing evenly is pulverized, is obtained
To synthetic wax of the invention.
2. a kind of preparation method according to claim 1, which is characterized in that the solvent is N, N- dimethyl formyl
One of amine, n,N-dimethylacetamide, n-methyl-2-pyrrolidone or N- ethyl-2-pyrrolidone are a variety of.
3. a kind of preparation method according to claim 1, the catalyst is p-methyl benzenesulfonic acid, methane sulfonic acid or 3-
One of toluenesulfonic acid is a variety of.
4. a kind of preparation method according to claim 1, which is characterized in that the stearmide is ethylene stearic bicine diester
The amides organic compound such as amine, erucyl amide or oleamide.
5. a kind of preparation method according to claim 1, which is characterized in that the polyethylene wax and polypropylene wax molecule
Range is measured from 2000-20000.
6. a kind of preparation method according to claim 1, which is characterized in that gained synthetic wax partial size is in 50-100 micron
Between.
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CN109206904B CN109206904B (en) | 2020-10-16 |
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Cited By (1)
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CN116135936A (en) * | 2021-11-18 | 2023-05-19 | 关西涂料株式会社 | Water-based coating composition for cans |
Citations (3)
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CN101082000A (en) * | 2007-06-07 | 2007-12-05 | 上海焦耳蜡业有限公司 | Polyethylene wax polypropylene wax and petroleum wax co-oxidation method |
KR20110014699A (en) * | 2011-01-05 | 2011-02-11 | 주식회사 케이씨앤지 | Wax manufacturing method using un-reacted material in polymerization process |
CN107523053A (en) * | 2017-08-15 | 2017-12-29 | 六安市杜尔邦绝缘材料有限公司 | A kind of resistant to elevated temperatures Kapton and its manufacturing process |
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2018
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CN101082000A (en) * | 2007-06-07 | 2007-12-05 | 上海焦耳蜡业有限公司 | Polyethylene wax polypropylene wax and petroleum wax co-oxidation method |
KR20110014699A (en) * | 2011-01-05 | 2011-02-11 | 주식회사 케이씨앤지 | Wax manufacturing method using un-reacted material in polymerization process |
CN107523053A (en) * | 2017-08-15 | 2017-12-29 | 六安市杜尔邦绝缘材料有限公司 | A kind of resistant to elevated temperatures Kapton and its manufacturing process |
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CN116135936A (en) * | 2021-11-18 | 2023-05-19 | 关西涂料株式会社 | Water-based coating composition for cans |
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