CN108864875A - A kind of preparation method of high intensity high heat stability water-based gloss oil - Google Patents
A kind of preparation method of high intensity high heat stability water-based gloss oil Download PDFInfo
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to a kind of preparation methods of high-intensitive high heat stability water-based gloss oil, belong to synthetic resin preparation technical field.The present invention produces graphene oxide and is added in gloss oil, graphene has fine and close molecular structure, the mechanical strength that gloss oil can be made to have had, the hydrophilic epoxies group such as a large amount of hydroxyl and carboxyl is introduced in simultaneous oxidation graphene, the present invention is modified acrylate with organosilicon, make to combine silicone ingredients on acrylate molecule chain, organosilicon, which can generate Si-C key with polyurethane molecular chain combination, to be made to have connected bridge beam action between each layer of polyurethane molecular chain, also make every layer of strand molecular structure that intermeshes even closer, to make the thermal stability of gloss oil be improved, simultaneous oxidation graphene has good thermal conductivity, enhance the heat dissipation effect of gloss oil by the evaporation endothermic of Free water, to make the thermal stability of gloss oil be further enhanced, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of high-intensitive high heat stability water-based gloss oil, belong to synthetic resin technology of preparing neck
Domain.
Background technique
Gloss oil, a kind of synthetic resin now typically refer to surface clear varnish, have base-material and auxiliary agent etc. to be made into, and are not added any
Pigment, it is glossy shinny after film forming, it is commonly called as being varnish, there is UV gloss oil and PU gloss oil.Earliest gloss oil refers to tung oil.
Gloss oil is mainly used for printed matter surface processing, to increase its glossiness and water resistance；By being printed in paper etc.
Product surface roller coating or the upper one layer of colorless and transparent coating of spraying, form one layer of uniform transparent light after levelling, solidification, press polish
Layer, after paper product is by upper light processing, surface gloss, smoothness, water resistance and wear-resisting property are all obviously improved；Gloss oil can be with
Beautification protection printing image-text, and prolongs its service life, and is therefore widely used in packing and decorating, picture album, substantially decoration and wide
In the surface processing of the printed matters such as announcement.
Hardness and flexibility are most important to UV coating, directly affect the performance and user experience of glazing product, but pass
System UV gloss oil is difficult to realize have both high rigidity and good flexibility；Because if improving hardness, need to select high molecular weight
Performed polymer then needs to increase the content of reactive diluent to guarantee low viscosity, thus become fragile after solidifying UV gloss oil, it is flexible
Property reduce；On the contrary, reducing reactive diluent content can be improved the flexibility after gloss oil solidifies, but molecular weight need to be selected low
Performed polymer, hardness reduces after causing gloss oil to solidify.
Water-based UV gloss oil is using water as reactive diluent, even if the performed polymer of selection high molecular weight, can still guarantee well viscous
Property, after gloss oil solidification, not only there is very high hardness, but also have good flexibility, and had been widely used in the neck more demanding to glazing
The glazing of domain, especially children's book and food and medicine package printed matter, is with a wide range of applications, in recent years gradually at
For the research hotspot of people.Water-based gloss oil as a kind of emerging environmentally protective printing material, be widely used in food packaging,
The printing such as medical packaging, Yan Bao, books and periodicals, wall calendar, water-based gloss oil possesses outstanding surface gloss, because its solvent is mainly water,
Harmful escaping gas will not be discharged to atmosphere, it is more environmentally friendly, meet the current theory for advocating environment protection health.Therefore aqueous light
Oil will be having wide development space from now on.The thermal stability of gloss oil is poor at present, and intensity difference wearability is insufficient.Therefore, one is invented
Kind intensity is high, and the good water-based gloss oil of thermal stability has positive effect to synthesis resin making technique field.
Summary of the invention
The technical problems to be solved by the invention：Poor for the thermal stability of current gloss oil, intensity difference wearability is insufficient
Defect provides a kind of preparation method of high-intensitive high heat stability water-based gloss oil.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
A kind of preparation method of high intensity high heat stability water-based gloss oil, it is characterised in that specifically preparation step is：
（1）According to parts by weight, 10~14 parts of graphite are weighed, 6~8 parts of potassium permanganate powders and 20~24 parts of concentrated sulfuric acids are put into burning
In cup, beaker is put into water-bath, bath temperature is increased after being stirred with blender, 2.5~2.7h of isothermal reaction obtains suspension；
（2）By above-mentioned suspension and deionized water in mass ratio 1：Mixed liquor is obtained in 2 investment beakers, then places the beaker water-bath
In pot, then the dehydrated alcohol of addition mixed liquor quality 25~30% and stirring into beaker, add mixed liquor quality 10~13%
Acetic acid solution, and with the revolving speed of 400~450r/min be mixed 20~30min obtain solidliquid mixture；
（3）Filter residue is obtained by filtration in above-mentioned solidliquid mixture while hot, is put into drying box after washing filter residue 3~5 times with dilute hydrochloric acid
It is dried to obtain oxide powder, it is spare；
（4）By butyl acrylate and vinyltriethoxysilane in mass ratio 10：1 is put into beaker and mixes, and beaker is put into
In water-bath, and modified liquid is stirred to get with blender；
（5）According to parts by weight, 28~30 parts of above-mentioned modified liquids, 2~3 parts of acrylic acid, 1~3 part of sodium bicarbonate, 5~7 are weighed
The spare oxide powder of part, 1~3 part of dodecyl sodium sulfate are put into reaction kettle, are stirred, and are discharged up to high-intensitive high fever
Stabilized aqueous gloss oil.
Step（1）Described in the concentrated sulfuric acid mass fraction be 80~90%, bath temperature be 0~5 DEG C, agitator speed
For 300~350r/min, mixing time is 70~90min, and water-bath increases temperature to 30~33 DEG C.
Step（2）Described in bath temperature be 85~90 DEG C, speed of agitator is 400~450r/min, and mixing time is
20~30min, the mass fraction of acetic acid solution are 80~90%.
Step（3）Described in the mass fraction of dilute hydrochloric acid be 12~15%, oven temperature is 105~110 DEG C, when dry
Between be 30~40min.
Step（4）Described in bath temperature be 50~55 DEG C, agitator speed be 400~500r/min, mixing time
For 20~30min.
Step（5）Described in temperature of reaction kettle be 30~35 DEG C, speed of agitator be 700~800r/min, be stirred
Time is 30~40min.
The method have the benefit that：
（1）The present invention first aoxidizes graphite potassium permanganate and the concentrated sulfuric acid, is re-introduced into hydroxyl, carboxylic group, oxidation is prepared
Graphene, then butyl acrylate is subjected to silane coupled modification, finally by graphene oxide, modification butyl acrylate and other
Auxiliary agent is stirred up to high-intensitive high stable water-based gloss oil, and the present invention produces graphene oxide and is added in gloss oil, graphene
With fine and close molecular structure, the mechanical strength that gloss oil can be made to have had introduces a large amount of hydroxyl in simultaneous oxidation graphene
The hydrophilic epoxies group such as base and carboxyl, can be such that graphene is well soluble in water, and the epoxy group in resin combines
Covalent bond and other chemical bond energys are formed, enables graphene and the even closer combination of gloss oil, obtains the intensity of gloss oil entirety
It improves, while organosilicon is also introduced into modified propylene acid butyl ester in gloss oil, organosilicon can be with the group knot in graphene oxide
Symphysis is at Si-O key and Si-C key, to keep gloss oil internal structure more stable, improves the mechanical strength and thermal stability of gloss oil；
（2）The present invention is modified acrylate with organosilicon, makes to combine silicone ingredients on acrylate molecule chain, organic
Silicon, which can generate Si-C key with polyurethane molecular chain combination, to be made to have connected bridge beam action between each layer of polyurethane molecular chain, is also made
Every layer of strand molecular structure that intermeshes is even closer, so that it is improved the thermal stability of gloss oil, simultaneous oxidation graphite
Alkene has good thermal conductivity, and the heat dissipation effect that heat transmitting increases gloss oil can be improved, have hydrophilic oxygen-containing functional group can
To absorb the hydrone in air, enhance the heat dissipation effect of gloss oil by the evaporation endothermic of Free water, to keep the heat of gloss oil steady
It is qualitative to be further enhanced, it has broad application prospects.
Specific embodiment
According to parts by weight, 10~14 parts of graphite are weighed, 6~8 parts of potassium permanganate powders and 20~24 parts of mass fractions are
80~90% concentrated sulfuric acid is put into beaker, beaker is put into the water-bath that temperature is 0~5 DEG C, with blender with 300~350r/
The revolving speed of min increases bath temperature to 30~33 DEG C after stirring 70~90min, and 2.5~2.7h of isothermal reaction obtains suspension；It will
Above-mentioned suspension and deionized water in mass ratio 1：Mixed liquor is obtained in 2 investment beakers, then placing the beaker bath temperature is 85
In~90 DEG C of water-bath, then into beaker be added mixed liquor quality 25~30% dehydrated alcohol and with 400~450r/min's
After 20~30min is mixed in revolving speed, the acetic acid solution that the mass fraction of mixed liquor quality 10~13% is 80~90% is added,
And 20~30min is mixed with the revolving speed of 400~450r/min and obtains solidliquid mixture；By above-mentioned solidliquid mixture mistake while hot
Filter obtains filter residue, and it is 105~110 DEG C of bakings that temperature is put into after washing filter residue 3~5 times with the dilute hydrochloric acid that mass fraction is 12~15%
Dry 30~40min obtains oxide powder in dry case, spare；In mass ratio by butyl acrylate and vinyltriethoxysilane
10：1 is put into beaker and mixes, and beaker is put into the water-bath that bath temperature is 50~55 DEG C, and with blender with 400~
The revolving speed of 500r/min stirs 20~30min and obtains modified liquid；According to parts by weight, 28~30 parts of above-mentioned modification liquids are weighed
Body, 2~3 parts of acrylic acid, 1~3 part of sodium bicarbonate, 5~7 parts of spare oxide powders, 1~3 part of dodecyl sodium sulfate are put into
In reaction kettle, it is stirred 30~40min under conditions of temperature is 30~35 DEG C, revolving speed is 700~800r/min, discharging is
Obtain high-intensitive high heat stability water-based gloss oil.
According to parts by weight, 10 parts of graphite, 6 parts of potassium permanganate powders and 20 parts of mass fractions are weighed as 80% concentrated sulfuric acid
It is put into beaker, beaker is put into the water-bath that temperature is 0 DEG C, risen after stirring 70min with blender with the revolving speed of 300r/min
For high bath temperature to 30 DEG C, isothermal reaction 2.5h obtains suspension；By above-mentioned suspension and deionized water in mass ratio 1：2 investments
Mixed liquor is obtained in beaker, then is placed the beaker in the water-bath that bath temperature is 85 DEG C, then mixed liquor matter is added into beaker
After measuring 25% dehydrated alcohol and 20min being mixed with the revolving speed of 400r/min, the quality point of mixed liquor quality 10% is added
The acetic acid solution that number is 80%, and 20min is mixed with the revolving speed of 400r/min and obtains solidliquid mixture；Above-mentioned solid-liquid is mixed
It closes object and filter residue is obtained by filtration while hot, it is 105 DEG C of drying that temperature is put into after washing filter residue 3 times with the dilute hydrochloric acid that mass fraction is 12%
Dry 30min obtains oxide powder in case, spare；By butyl acrylate and vinyltriethoxysilane in mass ratio 10：1 puts
Enter in beaker and mix, beaker is put into the water-bath that bath temperature is 50 DEG C, and stirred with blender with the revolving speed of 400r/min
It mixes 20min and obtains modified liquid；According to parts by weight, 28 parts of above-mentioned modified liquids, 2 parts of acrylic acid, 1 part of sodium bicarbonate, 5 are weighed
Part spare oxide powder, 1 part of dodecyl sodium sulfate are put into reaction kettle, temperature is 30 DEG C, revolving speed is 700r/min's
Under the conditions of be stirred 30min, discharge up to high-intensitive high heat stability water-based gloss oil.
According to parts by weight, 12 parts of graphite, 7 parts of potassium permanganate powders and 22 parts of mass fractions are weighed as 85% concentrated sulfuric acid
It is put into beaker, beaker is put into the water-bath that temperature is 2 DEG C, risen after stirring 80min with blender with the revolving speed of 320r/min
For high bath temperature to 32 DEG C, isothermal reaction 2.6h obtains suspension；By above-mentioned suspension and deionized water in mass ratio 1：2 investments
Mixed liquor is obtained in beaker, then is placed the beaker in the water-bath that bath temperature is 87 DEG C, then mixed liquor matter is added into beaker
After measuring 27% dehydrated alcohol and 25min being mixed with the revolving speed of 420r/min, the quality point of mixed liquor quality 12% is added
The acetic acid solution that number is 85%, and 25min is mixed with the revolving speed of 420r/min and obtains solidliquid mixture；Above-mentioned solid-liquid is mixed
It closes object and filter residue is obtained by filtration while hot, it is 107 DEG C of drying that temperature is put into after washing filter residue 4 times with the dilute hydrochloric acid that mass fraction is 12%
Dry 35min obtains oxide powder in case, spare；By butyl acrylate and vinyltriethoxysilane in mass ratio 10：1 puts
Enter in beaker and mix, beaker is put into the water-bath that bath temperature is 52 DEG C, and stirred with blender with the revolving speed of 450r/min
It mixes 25min and obtains modified liquid；According to parts by weight, 29 parts of above-mentioned modified liquids, 2 parts of acrylic acid, 2 parts of sodium bicarbonates, 6 are weighed
Part spare oxide powder, 2 parts of dodecyl sodium sulfates are put into reaction kettle, temperature is 32 DEG C, revolving speed is 750r/min's
Under the conditions of be stirred 35min, discharge up to high-intensitive high heat stability water-based gloss oil.
According to parts by weight, 14 parts of graphite, 8 parts of potassium permanganate powders and 24 parts of mass fractions are weighed as 90% concentrated sulfuric acid
It is put into beaker, beaker is put into the water-bath that temperature is 5 DEG C, risen after stirring 90min with blender with the revolving speed of 350r/min
For high bath temperature to 33 DEG C, isothermal reaction 2.7h obtains suspension；By above-mentioned suspension and deionized water in mass ratio 1：2 investments
Mixed liquor is obtained in beaker, then is placed the beaker in the water-bath that bath temperature is 90 DEG C, then mixed liquor matter is added into beaker
After measuring 30% dehydrated alcohol and 30min being mixed with the revolving speed of 450r/min, the quality point of mixed liquor quality 13% is added
The acetic acid solution that number is 90%, and 30min is mixed with the revolving speed of 450r/min and obtains solidliquid mixture；Above-mentioned solid-liquid is mixed
It closes object and filter residue is obtained by filtration while hot, it is 110 DEG C of bakings that temperature is put into after washing filter residue 3~5 times with the dilute hydrochloric acid that mass fraction is 15%
Dry 40min obtains oxide powder in dry case, spare；By butyl acrylate and vinyltriethoxysilane in mass ratio 10：1
It is put into beaker and mixes, beaker is put into the water-bath that bath temperature is 55 DEG C, and with blender with the revolving speed of 500r/min
Stirring 30min obtains modified liquid；According to parts by weight, 30 parts of above-mentioned modified liquids, 3 parts of acrylic acid, 3 parts of bicarbonates are weighed
Sodium, 7 parts of spare oxide powders, 3 parts of dodecyl sodium sulfates are put into reaction kettle, temperature be 35 DEG C, revolving speed 800r/
It is stirred 40min under conditions of min, discharges up to high-intensitive high heat stability water-based gloss oil.
Comparative example is as a comparison case made the present invention with the high-intensitive high heat stability water-based gloss oil that Jinjiang company produces
High-intensitive high heat stability water-based gloss oil and comparative example in high-intensitive high heat stability water-based gloss oil carry out performance detection, detection knot
Fruit is as shown in table 1：
Test method：
Liquid gloss oil performance：Using the viscosity of UV gloss oil made from NDJ-79 type rotary viscosity design determining, it is as a result listed in table 1；With
Upper water-based UV gloss oil obtained, which is placed under high temperature light protected environment, to be saved, and judges its stability according to lamination.
UV gloss oil curing membrane performance：Water-based UV gloss oil produced above is applied on standard print A4 paper, UV photocuring
As a result machine film-forming is listed in table 1 using 60 ° of gloss of WGG-60 glossiness tester measurement UV light film.
Adhesive force actual measurement is detected according to GB9286-1998 method.
Hardness test is detected according to GB/T6739-1996 method.
Elongation at break test：The UV gloss oil cured film of preparation is made by the 5B batten standard of ISO527/2-1993 (E)
It is flexible to measure film layer with the rate tensile in 2 mm/min on WDW3020 type micro-control electronic universal tester for standard batten
Property, it is indicated with elongation at break.
Abrasion resistance test：The counterweight that definite quality is encased using the A4 copy paper of suitable dimension is pressed in coated example 1
~3 and comparative example water-based gloss oil product to be tested above, starting tester rubs back and forth, measures the how many number rear surfaces of friction and occurs
Situation that wiping is spent and blank sheet of paper fades.
1 gloss oil performance measurement result of table
Good according to the high-intensitive high heat stability water-based gloss oil thermal stability produced by the present invention of data among the above, adhesive force is good,
Hardness and elongation at break are high, and intensity is high, and abrasion resistance is good, reaches 990 times or more, has broad application prospects.
Claims (6)
1. a kind of preparation method of high intensity high heat stability water-based gloss oil, it is characterised in that specifically preparation step is：
（1）According to parts by weight, 10~14 parts of graphite are weighed, 6~8 parts of potassium permanganate powders and 20~24 parts of concentrated sulfuric acids are put into burning
In cup, beaker is put into water-bath, bath temperature is increased after being stirred with blender, 2.5~2.7h of isothermal reaction obtains suspension；
（2）By above-mentioned suspension and deionized water in mass ratio 1：Mixed liquor is obtained in 2 investment beakers, then places the beaker water-bath
In pot, then the dehydrated alcohol of addition mixed liquor quality 25~30% and stirring into beaker, add mixed liquor quality 10~13%
Acetic acid solution, and with the revolving speed of 400~450r/min be mixed 20~30min obtain solidliquid mixture；
（3）Filter residue is obtained by filtration in above-mentioned solidliquid mixture while hot, is put into drying box after washing filter residue 3~5 times with dilute hydrochloric acid
It is dried to obtain oxide powder, it is spare；
（4）By butyl acrylate and vinyltriethoxysilane in mass ratio 10：1 is put into beaker and mixes, and beaker is put into
In water-bath, and modified liquid is stirred to get with blender；
（5）According to parts by weight, 28~30 parts of above-mentioned modified liquids, 2~3 parts of acrylic acid, 1~3 part of sodium bicarbonate, 5~7 are weighed
The spare oxide powder of part, 1~3 part of dodecyl sodium sulfate are put into reaction kettle, are stirred, and are discharged up to high-intensitive high fever
Stabilized aqueous gloss oil.
2. a kind of preparation method of high-intensitive high heat stability water-based gloss oil according to claim 1, it is characterised in that：Step
（1）Described in the concentrated sulfuric acid mass fraction be 80~90%, bath temperature be 0~5 DEG C, agitator speed be 300~350r/
Min, mixing time are 70~90min, and water-bath increases temperature to 30~33 DEG C.
3. a kind of preparation method of high-intensitive high heat stability water-based gloss oil according to claim 1, it is characterised in that：Step
（2）Described in bath temperature be 85~90 DEG C, speed of agitator be 400~450r/min, mixing time be 20~30min, second
The mass fraction of acid solution is 80~90%.
4. a kind of preparation method of high-intensitive high heat stability water-based gloss oil according to claim 1, it is characterised in that：Step
（3）Described in dilute hydrochloric acid mass fraction be 12~15%, oven temperature be 105~110 DEG C, drying time be 30~
40min。
5. a kind of preparation method of high-intensitive high heat stability water-based gloss oil according to claim 1, it is characterised in that：Step
（4）Described in bath temperature be 50~55 DEG C, agitator speed be 400~500r/min, mixing time be 20~30min.
6. a kind of preparation method of high-intensitive high heat stability water-based gloss oil according to claim 1, it is characterised in that：Step
（5）Described in temperature of reaction kettle be 30~35 DEG C, speed of agitator be 700~800r/min, be stirred the time be 30~
40min。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111732873A (en) * | 2020-06-12 | 2020-10-02 | 广州亦盛环保科技有限公司 | UV ink-jet gloss oil and preparation method thereof |
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| CN106433098A (en) * | 2016-09-28 | 2017-02-22 | 安徽大学 | Preparation method of graphene/polyacrylic ester-silicon-containing hyperbranched waterborne polyurethane multi-element composite emulsion |
| CN107053788A (en) * | 2017-03-29 | 2017-08-18 | 江阴海美金属新材料有限公司 | A kind of notebook computer casing overlay film aluminium sheet |
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