CN106280311A - A kind of preparation method of protecting film PET composite material - Google Patents
A kind of preparation method of protecting film PET composite material Download PDFInfo
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- CN106280311A CN106280311A CN201610664783.2A CN201610664783A CN106280311A CN 106280311 A CN106280311 A CN 106280311A CN 201610664783 A CN201610664783 A CN 201610664783A CN 106280311 A CN106280311 A CN 106280311A
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
- C08B15/05—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur
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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
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- C08L2203/16—Applications used for films
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The present invention provides the preparation method of a kind of protecting film PET composite material, the steps include: that Cortex Luffae is tanned by the sun, stripping and slicing, decocting in water, rinses, dries, pulverizes by (1), obtains luffa pericarp powder；(2) luffa pericarp powder is used sodium hydroxide solution soda boiling, obtain Cortex Luffae fiber；(3) Cortex Luffae fiber sulfuric acid solution is hydrolyzed, obtain Cortex Luffae cellulose；(4) by Cortex Luffae cellulose ion liquid dissolving, cellulose solution is obtained；(5) compound cellulose is synthesized for part with ruthenium ion with Cortex Luffae cellulose；(6) extruding pelletization after PET and other components being mixed, obtains protecting film PET composite material.The PET composite material that the present invention prepares has stronger weatherability and preferable fluorescence property.
Description
Technical field
The present invention relates to a kind of PET composite material, particularly relate to the preparation side of a kind of protecting film PET composite material
Method.
Background technology
PET full name is polyethylene terephthalate, it be to be reacted by p-phthalic acid and ethylene glycol condensation polymerization and
The advantages such as preparing, PET material has lightweight, and intensity is high, and the transparency and gas barrier property are good, nontoxic, tasteless, therefore PET obtains
Rapid development.Along with the development of the articles for daily use, the production of plastic package material and application are as emerge rapidly in large numbersBamboo shoots after a spring rain
Growing up, then along with the maturation of touch technology, what PET material also just followed a well mapped-out plan has used in various LCDs,
The most present PET protection film.PET protection film clear, colorless, surface have passed through cure process, according to its table of difference in the place of production
The hardening value in face is typically between 3H-4H, and Surface hardened layer is the best, and its wearability is the strongest.Light transmittance is also the main of PET protection film
Character, general light transmittance is more than 90%, and light transmittance is higher not only makes us have good regarding when using relevant instrument
Feel effective, and eyes are had a kind of well protective effect.
Such as, Publication No. CN105346174A, publication date are 2016.02.24, apply for that telecommunications is held up in sky, artificial Suzhou
The Chinese patent application of company limited discloses " a kind of antibiotic property PET protection film ", and described antibiotic property PET protection film includes going up most
Antibiotic layer, the radiation protective layer in intermediate layer and the undermost pet layer of layer combine, and described pet layer is that poly terephthalic acid is moulded
Material, described antibiotic layer accounts for the 27%-32% of the overall component of antibiotic property PET protection film, and described radiation protective layer accounts for antibiotic property PET
The 11%-14% of the overall component of protecting film, described pet layer accounts for the 50%-60% of the overall component of antibiotic property PET protection film, should
The antibiotic property PET protection film that invention provides has the features such as good dimensional stability, heat stability, chemical stability.But, should
The weatherability of antibiotic property PET protection film is the best, additionally, along with the raising of people's living standard, in some amusements or outdoor occasion
In the fluorescence property of PET protection film be it is also proposed requirement, PET protection film that this invention provides and existing PET protection film one
Sample does not possess fluorescence property.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of protecting film PET composite material, prepares
PET composite material there is stronger weatherability and preferable fluorescence property.
For solving above-mentioned technical problem, the technical scheme is that
The preparation method of a kind of protecting film PET composite material, the steps include:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put
Enter in water, after being heated to 100 DEG C, be incubated 30 minutes, be colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, powder after drying
Broken, obtain luffa pericarp powder；
(2) step (1) gained luffa pericarp powder is added in sodium hydroxide solution, be incubated 2 hours after being heated to 165 DEG C, take
With the deionized water wash 10 minutes of 50 DEG C after going out, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae
Fiber；
(3) step (2) gained Cortex Luffae fiber is added in sulfuric acid solution, stir 1 hour after being heated to 65 DEG C, add 5
DEG C distilled water after stand 1 hour, behind under reactant liquor 8000rpm speed centrifugal 20 minutes, be precipitated thing, by precipitate weight
After backwashing is washed, centrifugation step presents muddiness to supernatant, dialyses 2 days, obtain Cortex Luffae cellulose after being taken out by supernatant；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, open after being heated to 100 DEG C
Magnetic agitation, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) yttrium chloride solution is added in step (4) gained cellulose solution under agitation, regulate with sodium hydroxide
Ph value is 7, and after being heated to 65 DEG C, stirring reaction 20 minutes, proceed to reactant liquor, in bag filter, repeatedly soak with deionized water
Analysis bag, until detecting to without white precipitate with silver nitrate solution, is pulverized after being dried by product, is obtained compound cellulose；
(6) PET, compatilizer, toughener are added in blender, stir 30 minutes under room temperature, after taking-up, stand 20 hours
Obtain stirring material, stirring material, catalyst, antistatic additive, step (5) gained compound cellulose are added in blender, under room temperature
Stir and obtain compound in 30 minutes, add mixture into extruding pelletization in double screw extruder, obtain protecting film grade polyester composite wood
Material.
Preferably, in step of the present invention (2), the mass fraction of sodium hydroxide solution is 18%, luffa pericarp powder and hydrogen
The weight ratio of sodium hydroxide solution is 1:20.
Preferably, in step of the present invention (3), the mass fraction of sulfuric acid solution is 60%, Cortex Luffae fiber and sulphuric acid
The weight ratio of solution is 1:15.
Preferably, in step of the present invention (4), Yttrium chloride(Y2Cl6) is 1:10 with the weight ratio of Cortex Luffae cellulose.
Preferably, in step of the present invention (6), by weight, PET 81-86 part, compatilizer 2-3 part, toughener
3-4 part, catalyst 0.5-1 part, antistatic additive 1-2 part, compound cellulose 7-10 part.
Preferably, in step of the present invention (6), compatilizer is POE.
Preferably, in step of the present invention (6), toughener is SEBS.
Preferably, in step of the present invention (6), catalyst is antimony-based catalyst.
Preferably, in step of the present invention (6), antistatic additive is disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate.
Preferably, in step of the present invention (6), the extrusion temperature of double screw extruder is 160-190 DEG C, screw speed
130-150rpm。
Compared with prior art, the method have the advantages that
(1) Cortex Luffae is the skin portion of Fructus Luffae, can discard Cortex Luffae when people eat Fructus Luffae meat, and the present invention is by Fructus Luffae
Skin is reclaimed, and first passes through and tans by the sun, stripping and slicing, decocting in water, rinses, dries, pulverizes the impurity eliminating in Cortex Luffae and obtain Fructus Luffae
Corium farinosum, then effectively eliminates lignin, hemicellulose and pectin by luffa pericarp powder sodium hydroxide solution soda boiling and obtains Fructus Luffae
Hide fiber, then the hydrolysis of Cortex Luffae fiber sulfuric acid solution is obtained finely disseminated Cortex Luffae cellulose, Cortex Luffae cellulose has
Having good oxidation resistance and UV absorbing properties, therefore weatherability is relatively strong, then by Cortex Luffae cellulose ionic liquid
Body dissolves and obtains cellulose solution, then is reacted with yttrium chloride solution by cellulose solution, with Cortex Luffae cellulose as part
Synthesizing compound cellulose with ruthenium ion, yttrium is a kind of rare earth element with excellent fluorescence property, ruthenium ion and Cortex Luffae fiber
The composite fibre that element obtains after forming salt is also provided with after the components such as good fluorescence property, compound cellulose and PET are blended big
Improve greatly weatherability and the fluorescence property of PET composite material.
(2) surface of Cortex Luffae cellulose is that the compatibility between hydrophilic, and PET matrix is the best, uses in the present invention
Ionic liquid the hydrophilic of Cortex Luffae fiber surface can be become lipophile, effectively improve the phase between its with PET matrix
Capacitive and bond strength, thus improve weatherability and the fluorescence property of PET composite material further.
Detailed description of the invention
The present invention is described in detail, in illustrative examples and the explanation of this present invention below in conjunction with specific embodiment
It is used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1
Prepare protecting film PET composite material as steps described below:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put
Enter in water, after being heated to 100 DEG C, be incubated 30 minutes, be colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, powder after drying
Broken, obtain luffa pericarp powder；
(2) by step (1) gained luffa pericarp powder addition mass fraction be 18% sodium hydroxide solution in, luffa pericarp powder with
The weight ratio of sodium hydroxide solution is 1:20, is incubated 2 hours, with the deionized water wash of 50 DEG C after taking-up after being heated to 165 DEG C
10 minutes, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae fiber；
(3) by step (2) gained Cortex Luffae fiber addition mass fraction be 60% sulfuric acid solution in, Cortex Luffae fiber with
The weight ratio of sulfuric acid solution is 1:15, stirs 1 hour after being heated to 65 DEG C, stands 1 hour after adding the distilled water of 5 DEG C, will be anti-
Answer and be precipitated thing after centrifugal 20 minutes under liquid 8000rpm speed, precipitate repeated washing, centrifugation step are presented to supernatant
Muddiness, dialyses 2 days after being taken out by supernatant, obtains Cortex Luffae cellulose；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, open after being heated to 100 DEG C
Magnetic agitation, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) under agitation yttrium chloride solution is added in step (4) gained cellulose solution, Yttrium chloride(Y2Cl6) and Cortex Luffae
The weight ratio of cellulose is 1:10, is 7 by sodium hydroxide regulation ph value, and stirring reaction 20 minutes after being heated to 65 DEG C will reaction
Liquid proceeds in bag filter, repeatedly soak with deionized water bag filter until with silver nitrate solution detect to without white precipitate,
Pulverize after product is dried, obtain compound cellulose；
(6) 82 weight portion PET, 2.1 weight portion POE, 4 weight portion SEBS are added in blender, under room temperature, stir 30 points
Clock, stands after taking-up and within 20 hours, obtains stirring material, by stirring material, 0.5 weight portion antimony-based catalyst, 1.4 weight portion dodecyls
Diphenyl oxide disulfonate, 7.5 weight portion step (5) gained compound celluloses add in blender, stir 30 minutes under room temperature
To compound, adding mixture into extruding pelletization in double screw extruder, the extrusion temperature of double screw extruder is 160-190
DEG C, screw speed 130-150rpm, obtain protecting film PET composite material.
Embodiment 2
Prepare protecting film PET composite material as steps described below:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put
Enter in water, after being heated to 100 DEG C, be incubated 30 minutes, be colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, powder after drying
Broken, obtain luffa pericarp powder；
(2) by step (1) gained luffa pericarp powder addition mass fraction be 18% sodium hydroxide solution in, luffa pericarp powder with
The weight ratio of sodium hydroxide solution is 1:20, is incubated 2 hours, with the deionized water wash of 50 DEG C after taking-up after being heated to 165 DEG C
10 minutes, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae fiber；
(3) by step (2) gained Cortex Luffae fiber addition mass fraction be 60% sulfuric acid solution in, Cortex Luffae fiber with
The weight ratio of sulfuric acid solution is 1:15, stirs 1 hour after being heated to 65 DEG C, stands 1 hour after adding the distilled water of 5 DEG C, will be anti-
Answer and be precipitated thing after centrifugal 20 minutes under liquid 8000rpm speed, precipitate repeated washing, centrifugation step are presented to supernatant
Muddiness, dialyses 2 days after being taken out by supernatant, obtains Cortex Luffae cellulose；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, open after being heated to 100 DEG C
Magnetic agitation, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) under agitation yttrium chloride solution is added in step (4) gained cellulose solution, Yttrium chloride(Y2Cl6) and Cortex Luffae
The weight ratio of cellulose is 1:10, is 7 by sodium hydroxide regulation ph value, and stirring reaction 20 minutes after being heated to 65 DEG C will reaction
Liquid proceeds in bag filter, repeatedly soak with deionized water bag filter until with silver nitrate solution detect to without white precipitate,
Pulverize after product is dried, obtain compound cellulose；
(6) 84 weight portion PET, 2.5 weight portion POE, 3.2 weight portion SEBS are added in blender, under room temperature, stir 30
Minute, stand after taking-up and within 20 hours, obtain stirring material, by stirring material, 0.7 weight portion antimony-based catalyst, 1 weight portion dodecyl
Diphenyl oxide disulfonate, 10 weight portion step (5) gained compound celluloses add in blender, and under room temperature, stirring obtains for 30 minutes
Compound, adds mixture into extruding pelletization in double screw extruder, and the extrusion temperature of double screw extruder is 160-190 DEG C,
Screw speed 130-150rpm, obtains protecting film PET composite material.
Embodiment 3
Prepare protecting film PET composite material as steps described below:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put
Enter in water, after being heated to 100 DEG C, be incubated 30 minutes, be colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, powder after drying
Broken, obtain luffa pericarp powder；
(2) by step (1) gained luffa pericarp powder addition mass fraction be 18% sodium hydroxide solution in, luffa pericarp powder with
The weight ratio of sodium hydroxide solution is 1:20, is incubated 2 hours, with the deionized water wash of 50 DEG C after taking-up after being heated to 165 DEG C
10 minutes, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae fiber；
(3) by step (2) gained Cortex Luffae fiber addition mass fraction be 60% sulfuric acid solution in, Cortex Luffae fiber with
The weight ratio of sulfuric acid solution is 1:15, stirs 1 hour after being heated to 65 DEG C, stands 1 hour after adding the distilled water of 5 DEG C, will be anti-
Answer and be precipitated thing after centrifugal 20 minutes under liquid 8000rpm speed, precipitate repeated washing, centrifugation step are presented to supernatant
Muddiness, dialyses 2 days after being taken out by supernatant, obtains Cortex Luffae cellulose；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, open after being heated to 100 DEG C
Magnetic agitation, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) under agitation yttrium chloride solution is added in step (4) gained cellulose solution, Yttrium chloride(Y2Cl6) and Cortex Luffae
The weight ratio of cellulose is 1:10, is 7 by sodium hydroxide regulation ph value, and stirring reaction 20 minutes after being heated to 65 DEG C will reaction
Liquid proceeds in bag filter, repeatedly soak with deionized water bag filter until with silver nitrate solution detect to without white precipitate,
Pulverize after product is dried, obtain compound cellulose；
(6) 86 weight portion PET, 2 weight portion POE, 3.5 weight portion SEBS are added in blender, under room temperature, stir 30 points
Clock, stands after taking-up and within 20 hours, obtains stirring material, by stirring material, 0.9 weight portion antimony-based catalyst, 1.6 weight portion dodecyls
Diphenyl oxide disulfonate, 8 weight portion step (5) gained compound celluloses add in blender, and under room temperature, stirring obtains for 30 minutes
Compound, adds mixture into extruding pelletization in double screw extruder, and the extrusion temperature of double screw extruder is 160-190 DEG C,
Screw speed 130-150rpm, obtains protecting film PET composite material.
Embodiment 4
Prepare protecting film PET composite material as steps described below:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put
Enter in water, after being heated to 100 DEG C, be incubated 30 minutes, be colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, powder after drying
Broken, obtain luffa pericarp powder；
(2) by step (1) gained luffa pericarp powder addition mass fraction be 18% sodium hydroxide solution in, luffa pericarp powder with
The weight ratio of sodium hydroxide solution is 1:20, is incubated 2 hours, with the deionized water wash of 50 DEG C after taking-up after being heated to 165 DEG C
10 minutes, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae fiber；
(3) by step (2) gained Cortex Luffae fiber addition mass fraction be 60% sulfuric acid solution in, Cortex Luffae fiber with
The weight ratio of sulfuric acid solution is 1:15, stirs 1 hour after being heated to 65 DEG C, stands 1 hour after adding the distilled water of 5 DEG C, will be anti-
Answer and be precipitated thing after centrifugal 20 minutes under liquid 8000rpm speed, precipitate repeated washing, centrifugation step are presented to supernatant
Muddiness, dialyses 2 days after being taken out by supernatant, obtains Cortex Luffae cellulose；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, open after being heated to 100 DEG C
Magnetic agitation, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) under agitation yttrium chloride solution is added in step (4) gained cellulose solution, Yttrium chloride(Y2Cl6) and Cortex Luffae
The weight ratio of cellulose is 1:10, is 7 by sodium hydroxide regulation ph value, and stirring reaction 20 minutes after being heated to 65 DEG C will reaction
Liquid proceeds in bag filter, repeatedly soak with deionized water bag filter until with silver nitrate solution detect to without white precipitate,
Pulverize after product is dried, obtain compound cellulose；
(6) 85 weight portion PET, 2.7 weight portion POE, 3 weight portion SEBS are added in blender, under room temperature, stir 30 points
Clock, stands after taking-up and within 20 hours, obtains stirring material, by stirring material, 1 weight portion antimony-based catalyst, 1.2 weight portion dodecyls two
Phenylate sodium disulfonate, 8.5 weight portion step (5) gained compound celluloses add in blender, and under room temperature, stirring obtains for 30 minutes
Compound, adds mixture into extruding pelletization in double screw extruder, and the extrusion temperature of double screw extruder is 160-190 DEG C,
Screw speed 130-150rpm, obtains protecting film PET composite material.
Embodiment 5
Prepare protecting film PET composite material as steps described below:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put
Enter in water, after being heated to 100 DEG C, be incubated 30 minutes, be colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, powder after drying
Broken, obtain luffa pericarp powder；
(2) by step (1) gained luffa pericarp powder addition mass fraction be 18% sodium hydroxide solution in, luffa pericarp powder with
The weight ratio of sodium hydroxide solution is 1:20, is incubated 2 hours, with the deionized water wash of 50 DEG C after taking-up after being heated to 165 DEG C
10 minutes, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae fiber；
(3) by step (2) gained Cortex Luffae fiber addition mass fraction be 60% sulfuric acid solution in, Cortex Luffae fiber with
The weight ratio of sulfuric acid solution is 1:15, stirs 1 hour after being heated to 65 DEG C, stands 1 hour after adding the distilled water of 5 DEG C, will be anti-
Answer and be precipitated thing after centrifugal 20 minutes under liquid 8000rpm speed, precipitate repeated washing, centrifugation step are presented to supernatant
Muddiness, dialyses 2 days after being taken out by supernatant, obtains Cortex Luffae cellulose；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, open after being heated to 100 DEG C
Magnetic agitation, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) under agitation yttrium chloride solution is added in step (4) gained cellulose solution, Yttrium chloride(Y2Cl6) and Cortex Luffae
The weight ratio of cellulose is 1:10, is 7 by sodium hydroxide regulation ph value, and stirring reaction 20 minutes after being heated to 65 DEG C will reaction
Liquid proceeds in bag filter, repeatedly soak with deionized water bag filter until with silver nitrate solution detect to without white precipitate,
Pulverize after product is dried, obtain compound cellulose；
(6) 83 weight portion PET, 2.4 weight portion POE, 3.6 weight portion SEBS are added in blender, under room temperature, stir 30
Minute, stand after taking-up and within 20 hours, obtain stirring material, by stirring material, 0.8 weight portion antimony-based catalyst, 2 weight portion dodecyls
Diphenyl oxide disulfonate, 7 weight portion step (5) gained compound celluloses add in blender, and under room temperature, stirring obtains for 30 minutes
Compound, adds mixture into extruding pelletization in double screw extruder, and the extrusion temperature of double screw extruder is 160-190 DEG C,
Screw speed 130-150rpm, obtains protecting film PET composite material.
Embodiment 6
Prepare protecting film PET composite material as steps described below:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put
Enter in water, after being heated to 100 DEG C, be incubated 30 minutes, be colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, powder after drying
Broken, obtain luffa pericarp powder；
(2) by step (1) gained luffa pericarp powder addition mass fraction be 18% sodium hydroxide solution in, luffa pericarp powder with
The weight ratio of sodium hydroxide solution is 1:20, is incubated 2 hours, with the deionized water wash of 50 DEG C after taking-up after being heated to 165 DEG C
10 minutes, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae fiber；
(3) by step (2) gained Cortex Luffae fiber addition mass fraction be 60% sulfuric acid solution in, Cortex Luffae fiber with
The weight ratio of sulfuric acid solution is 1:15, stirs 1 hour after being heated to 65 DEG C, stands 1 hour after adding the distilled water of 5 DEG C, will be anti-
Answer and be precipitated thing after centrifugal 20 minutes under liquid 8000rpm speed, precipitate repeated washing, centrifugation step are presented to supernatant
Muddiness, dialyses 2 days after being taken out by supernatant, obtains Cortex Luffae cellulose；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, open after being heated to 100 DEG C
Magnetic agitation, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) under agitation yttrium chloride solution is added in step (4) gained cellulose solution, Yttrium chloride(Y2Cl6) and Cortex Luffae
The weight ratio of cellulose is 1:10, is 7 by sodium hydroxide regulation ph value, and stirring reaction 20 minutes after being heated to 65 DEG C will reaction
Liquid proceeds in bag filter, repeatedly soak with deionized water bag filter until with silver nitrate solution detect to without white precipitate,
Pulverize after product is dried, obtain compound cellulose；
(6) 81 weight portion PET, 3 weight portion POE, 3.3 weight portion SEBS are added in blender, under room temperature, stir 30 points
Clock, stands after taking-up and within 20 hours, obtains stirring material, by stirring material, 0.6 weight portion antimony-based catalyst, 1.8 weight portion dodecyls
Diphenyl oxide disulfonate, 9 weight portion step (5) gained compound celluloses add in blender, and under room temperature, stirring obtains for 30 minutes
Compound, adds mixture into extruding pelletization in double screw extruder, and the extrusion temperature of double screw extruder is 160-190 DEG C,
Screw speed 130-150rpm, obtains protecting film PET composite material.
The PET composite material preparing embodiment 1-6 and the weatherability of comparative example and fluorescence property are tested respectively,
Wherein, comparative example is the Chinese patent application of Publication No. CN105346174A.
Weatherability method of testing is: be placed in comparative example after the PET composite material that embodiment 1-6 prepares is made protecting film
Roof, every 5 days by each protecting film doubling, to there is the time representation weatherability of embrittlement, this time, the longest weatherability was the strongest.
Fluorescence property aspect tests the fluorescence intensity of each protecting film by spectrofluorophotometer, the biggest fluorescence of fluorescence intensity
Performance is the best.
Test result see table:
As seen from the above table, the appearance embrittlement of the protecting film made by PET composite material that embodiment of the present invention 1-6 prepares
Time exceed well over comparative example, fluorescence intensity aspect is also significantly greater than comparative example, shows to have stronger weatherability and preferably
Fluorescence property.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any ripe
Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage knowing this technology.Cause
This, have usually intellectual such as complete with institute under technological thought without departing from disclosed spirit in art
All equivalences become are modified or change, and must be contained by the claim of the present invention.
Claims (10)
1. the preparation method of a protecting film PET composite material, it is characterised in that comprise the steps:
(1) Cortex Luffae is placed in atmospheric exposure 2 hours, is cut into the Fructus Luffae skin bit of 1cm × 1cm × 1cm, Fructus Luffae skin bit is put into water
In, it is incubated 30 minutes after being heated to 100 DEG C, is colourless with deionized water rinsing to Fructus Luffae skin bit after taking-up, pulverizes after drying,
To luffa pericarp powder；
(2) step (1) gained luffa pericarp powder is added in sodium hydroxide solution, be incubated 2 hours after being heated to 165 DEG C, after taking-up
With the deionized water wash 10 minutes of 50 DEG C, then with the deionized water wash 5 minutes of 5 DEG C, after drying, obtain Cortex Luffae fiber；
(3) step (2) gained Cortex Luffae fiber is added in sulfuric acid solution, stir 1 hour after being heated to 65 DEG C, add 5 DEG C
Stand 1 hour after distilled water, behind under reactant liquor 8000rpm speed centrifugal 20 minutes, be precipitated thing, repeat to wash by precipitate
Wash, centrifugation step presents muddiness to supernatant, dialyses 2 days, obtain Cortex Luffae cellulose after being taken out by supernatant；
(4) 1-methoxyethyl-3-ethyl imidazol(e) chloride ionic liquid is added in flask, after being heated to 100 DEG C, open magnetic force
Stirring, is subsequently adding step (3) gained Cortex Luffae cellulose, and stirring obtains cellulose solution after being completely dissolved；
(5) under agitation yttrium chloride solution is added in step (4) gained cellulose solution, regulate ph value with sodium hydroxide
Being 7, after being heated to 65 DEG C, stirring reaction 20 minutes, proceed to reactant liquor in bag filter, repeatedly soak bag filter with deionized water
Until detecting to without white precipitate with silver nitrate solution, pulverize after product is dried, obtain compound cellulose；
(6) PET, compatilizer, toughener are added in blender, stir 30 minutes under room temperature, stand after taking-up and obtain for 20 hours
Stirring material, adds in blender by stirring material, catalyst, antistatic additive, step (5) gained compound cellulose, stirs under room temperature
Within 30 minutes, obtain compound, add mixture into extruding pelletization in double screw extruder, obtain protecting film PET composite material.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly in (2), the mass fraction of sodium hydroxide solution is 18%, and luffa pericarp powder is 1:20 with the weight ratio of sodium hydroxide solution.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly in (3), the mass fraction of sulfuric acid solution is 60%, and Cortex Luffae fiber is 1:15 with the weight ratio of sulfuric acid solution.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly, in (4), Yttrium chloride(Y2Cl6) is 1:10 with the weight ratio of Cortex Luffae cellulose.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly in (6), by weight, PET 81-86 part, compatilizer 2-3 part, toughener 3-4 part, catalyst 0.5-1 part, antistatic additive
1-2 part, compound cellulose 7-10 part.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly, in (6), compatilizer is POE.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly, in (6), toughener is SEBS.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly, in (6), catalyst is antimony-based catalyst.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly, in (6), antistatic additive is disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate.
The preparation method of a kind of protecting film PET composite material the most according to claim 1, it is characterised in that: described step
Suddenly in (6), the extrusion temperature of double screw extruder is 160-190 DEG C, screw speed 130-150rpm.
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| CN108822547A (en) * | 2018-06-07 | 2018-11-16 | 江苏理工学院 | A kind of preparation method of luffa/ionic liquid modified synergic composite conducting polymer material |
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| CN104559083A (en) * | 2014-12-24 | 2015-04-29 | 江苏至柔高分子材料有限公司 | Oriented transparent nano natural fiber polyester film and preparation method thereof |
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| CN104559083A (en) * | 2014-12-24 | 2015-04-29 | 江苏至柔高分子材料有限公司 | Oriented transparent nano natural fiber polyester film and preparation method thereof |
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