CN108485316A - A kind of modified titanium and preparation method for plastic light reflecting film - Google Patents
A kind of modified titanium and preparation method for plastic light reflecting film Download PDFInfo
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C09C1/36—Compounds of titanium
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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Abstract
The present invention relates to filler modified fields, disclose a kind of modified titanium and preparation method for plastic light reflecting film.Including following preparation process：（1）Water and alcohol are configured to mixed solvent；（2）Titanate coupling agent, surfactant and polyurethane modified acrylic resin lotion is added in the mixed solvent, heating stirring obtains organically-modified agent solution；（3）According to following parts by weight dispersion liquid：20 ~ 40 parts by weight of titanium dioxide, 60 ~ 80 parts by weight of organically-modified agent solution stir, filtering, the dry titanium dioxide coated to get organically-modified film.Modified titanium produced by the present invention can form a film on plastic substrate, and reflective function and the quality for obtaining reflective membrane are good, and significantly improve the mechanical property and weather resistance of reflective membrane, not influence reflecting effect after cleaning repeatedly, service life is long.
Description
Technical field
The present invention relates to filler modified field, a kind of modified titanium for plastic light reflecting film and preparation side are disclosed
Method.
Background technology
Reflective membrane be it is a kind of be made film can direct applied reflecting material, and the one kind being most widely used is inverse
Reflecting material.Nineteen thirty-seven, first piece of reflective membrane is traffic sign large-scale application in the laboratory birth in the U.S. in the world
The starting point of reflective membrane history.Hereafter, with the development of chemical industry, particularly synthetic resin, each research and development institution is constantly studied
Innovation, using glass bead technology, synthetic resin technology, thin film technique and coating technology, it is inverse to develop a series of high quality in succession
Reflect product.
Reflectorized material is mainly used for making various reflecting sign labels, number plate of vehicle, safety devices etc., fresh with its on daytime
Gorgeous color plays apparent warning function, and in the case of night or insufficient light, bright reflecting effect can effectively increase
The recognition capability of strong man, sees target clearly, arouses vigilance, and to avoid accident, reduces casualties, reduces economic loss,
As the indispensable security guard of road traffic, there is apparent social benefit.Use scope relate generally to public security traffic,
The departments such as traffic superintendance, fire-fighting, railway, coal mine, civilian reflectorized material are mainly reflective fabric, reflective lattice piece, reflection picture spraying cloth
Deng.
The surface layer of reflective membrane is usually by being translucency and the good resin film of weather resistance, and reflecting layer is according to inhomogeneity
Its composition material of the reflective membrane of type is also different, and it is mostly to set to have tiny glass beads, microprism or metal reflective coating etc., base
Film made of fat organic compound, adhesive layer are usually epoxide-resin glue, and bottom is the protective layer that ground paper is done.In recent years, titanium
As a kind of white pigment with efficient light reflective properties, the development in reflective membrane field is increasingly taken seriously white powder.
Chinese invention patent application number 201610639556.4 disclose a kind of reflectorized material based on modified titanium and
Preparation method is made of protective layer, soot layer, reflecting layer, supporting layer and adherent layer, and the reflecting layer by weighing as follows
The raw material of amount part is prepared：Modified titanium, 20 ~ 30 parts；Pearl powder, 5 ~ 15 parts；Ten dihydroxystearic acids, 10 ~ 20 parts；First
Base hydroxypropyl acrylate, 10 ~ 20 parts；Tert-amyl hydroperoxide, 15 ~ 25 parts；Pentaerythritol stearate, 2 ~ 4 parts；Dioctyl hexichol
Amine, 1 ~ 3 part；Tributyl phosphate, 1 ~ 3 part.The reflectorized material reflective function that the invention provides is high, and does not influence it after rinsing repeatedly
Reflecting effect, hence it is evident that the deficiencies in the prior art are overcome, compared with prior art with substantive distinguishing features outstanding and significantly
Progress.The preparation method of modified titanium is：While nanometer titanium dioxide is stirred, while spraying into misty tripotassium phosphate to nanometer titanium dioxide
Phenolic ester acetone soln；It is dried 20 ~ 30 minutes prior to 50 ~ 60 DEG C after spray uniformly, 5 ~ 15 minutes is dried then at 250 ~ 350 DEG C to obtain the final product.
Chinese invention patent application number 201610987555.9 discloses a kind of liquid crystal display reflective membrane of being used to prepare
White master batch is prepared by each component of following mass percent：Polyethylene terephthalate 31.5 ~ 49.7%, titanium white
Powder 50 ~ 65%, hyper-dispersant 0.2 ~ 1%, antioxidant 0.1 ~ 0.5%, fluorescent whitening agent 0 ~ 2%；The invention solves in the prior art
Master batch pigment is difficult evenly dispersed, so as to cause curtain coating extruding dies network blocking, diaphragm broken hole, rough, and then is caused
It is difficult to the not high problems of finished product reflectivity for carrying out continuous production and producing.It is evenly dispersed to develop a kind of pigment
It is used to prepare the white master batch of liquid crystal display reflective membrane, the reflective membrane produced using the master batch of the invention has reflectivity height,
Good, the simple for process advantage of continuity of production process.
According to plastic light reflecting film that is above-mentioned, being prepared using titanium dioxide in existing scheme, will appear after cleaning repeatedly reflective
The phenomenon that degree declines, to influence reflecting effect, mechanical property and weatherability be not good enough, and service life is short, and the present invention proposes one
Modified titanium and preparation method of the kind for plastic light reflecting film, can effectively solve above-mentioned technical problem.
Invention content
Exist at present using wider titanium dioxide plastic light reflecting film after cleaning repeatedly and the phenomenon that reflectance decline occurs, it is reflective
Effect is poor, and the poor mechanical property of reflective membrane, and heat-resisting quantity is poor, and weatherability is not good enough, and service life is short, influences normal use.
To solve the above problems, the present invention uses following technical scheme：
A kind of preparation method of modified titanium for plastic light reflecting film, the detailed process of preparation are：
（1）Water and alcohol are configured to mixed solvent；Wherein：20 ~ 60 parts by weight of water, 40 ~ 80 parts by weight of alcohol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, polyurethane modified acrylic resin lotion is added, is warming up to 60 ~ 80 DEG C, continues 30 ~ 50min of stirring, obtains organic change
Property agent solution；Wherein：60 ~ 70 parts by weight of mixed solvent, 1 ~ 2 parts by weight of titanate coupling agent, 1 ~ 2 parts by weight of surfactant,
28 ~ 36 parts by weight of polyurethane modified acrylic resin lotion；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continue 15 ~ 30min of stirring, filter, does
It is dry, obtain the titanium dioxide of organically-modified film cladding；Wherein：20 ~ 40 parts by weight of titanium dioxide, 60 ~ 80 weight of organically-modified agent solution
Part.
Preferably, step（1）The alcohol be ethyl alcohol, normal propyl alcohol, n-butanol, n-hexyl alcohol, n-amyl alcohol, 2- propyl alcohol, 2- butanol,
At least one of 2- hexanols, cyclohexanol, the tert-butyl alcohol, 2- methyl -2- butanol.
Preferably, step（2）The titanate coupling agent is isopropyl three (isostearoyl base) titanate esters, isopropyl three
(dioctyl pyrophosphoryl base) titanate esters, two (dioctyl pyrophosphoryl bases) close fluoroacetic acid ester titanium, two (dioctyl pyrophosphoryl base) ethylenes
In titanate esters, isopropyl three (dioctyl phosphoryl) titanate esters, isopropyl three (positive ethylamino-ethylamino) titanate esters at least
It is a kind of.
Preferably,：Step（2）The surfactant is sulfated castor oil, sldium lauryl sulfate, dioctyl succinate acid
At least one of sodium sulfonate, neopelex, sodium glycocholate, odium stearate.
Preferably, step（2）The solid content of the polyurethane modified acrylic resin lotion is 30 ~ 40%.
Preferably, step（3）The average grain diameter of the titanium dioxide is 0.2 ~ 0.25 μm, and content of titanium dioxide is 97 ~ 99%.
Preferably, step（3）The drying be vacuum drying, temperature be 70 ~ 80 DEG C, the time be 20 ~ for 24 hours.
A kind of modified titanium for plastic light reflecting film being prepared by the above method, by organic modifiers
Add polyurethane modified acrylic resin, can be formed a film on plastic substrate using polyurethane modified acrylic resin and
It is bonded titanium dioxide, so that manufactured reflectorized material is had the function of retroreflecting under light irradiation, and there is preferable high temperature resistant
Property.By coating one layer of organically-modified film on titanium dioxide surface, titanium dioxide and matrix resin is set to form stabilising system, therefore apply
It is easy to form single layer closely equally distributed titanium white bisque after cloth, obviously be carried with the reflective function of the reflective membrane of its making and quality
Height, while the function functional group on coupling agent can react with matrix resin, by the bonding of coupling agent, improve reflective membrane
Mechanical property and weather resistance, service life it is long.
The present invention provides a kind of modified titaniums and preparation method for plastic light reflecting film, compared with prior art,
Its feature protruded and excellent effect are：
1, the method that divided titanium dioxide is scattered to the modified titanium that organically-modified agent solution is prepared for plastic light reflecting film is proposed.
2, it by the polyurethane modified acrylic resin in organic modifiers, can form a film on plastic substrate and viscous
Titanium dioxide is connect, makes manufactured reflectorized material that there is excellent reflecting effect under light irradiation, and durability is good.
3, by carrying out organically-modified processing to titanium dioxide surface, the reflective function and quality of the reflective membrane of making obviously carry
Height, while the function functional group on coupling agent can react with matrix resin, by the bonding of coupling agent, improve reflective membrane
Mechanical property and weather resistance, repeatedly clean after do not influence reflecting effect, service life is long.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）Water and alcohol are configured to mixed solvent；Wherein：30 parts by weight of water, 70 parts by weight of alcohol；Alcohol is ethyl alcohol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, polyurethane modified acrylic resin lotion is added, is warming up to 72 DEG C, continues to stir 40min, it is molten to obtain organic modifiers
Liquid；Wherein：66 parts by weight of mixed solvent, 1 parts by weight of titanate coupling agent, 2 parts by weight of surfactant, polyurethane-modified propylene
31 parts by weight of acid resin lotion；Titanate coupling agent is isopropyl three (isostearoyl base) titanate esters；Surfactant is sulfuric acid
Change castor oil；The solid content of polyurethane modified acrylic resin lotion is 36%；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continues to stir 23min, filter, it is dry, it obtains
The titanium dioxide coated to organically-modified film；Wherein：32 parts by weight of titanium dioxide, 68 parts by weight of organically-modified agent solution；Titanium dioxide
Average grain diameter is 0.23 μm, content of titanium dioxide 98%；Dry is vacuum drying, and temperature is 76 DEG C, time 23h.
Polyethylene reflective membrane made from modified titanium made from embodiment 1, shown in reflection coefficient, tensile strength table 1.
Embodiment 2
（1）Water and alcohol are configured to mixed solvent；Wherein：20 parts by weight of water, 80 parts by weight of alcohol；Alcohol is normal propyl alcohol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, polyurethane modified acrylic resin lotion is added, is warming up to 60 DEG C, continues to stir 50min, it is molten to obtain organic modifiers
Liquid；Wherein：60 parts by weight of mixed solvent, 2 parts by weight of titanate coupling agent, 2 parts by weight of surfactant, polyurethane-modified propylene
36 parts by weight of acid resin lotion；Titanate coupling agent is isopropyl three (dioctyl pyrophosphoryl base) titanate esters；Surfactant is
Sldium lauryl sulfate；The solid content of polyurethane modified acrylic resin lotion is 30%；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continues to stir 15min, filter, it is dry, it obtains
The titanium dioxide coated to organically-modified film；Wherein：20 parts by weight of titanium dioxide, 80 parts by weight of organically-modified agent solution；Titanium dioxide
Average grain diameter is 0.2 μm, content of titanium dioxide 97%；Dry to be dried in vacuo, temperature is 70 DEG C, and the time is for 24 hours.
Polyethylene reflective membrane made from modified titanium made from embodiment 2, reflection coefficient, tensile strength such as 1 institute of table
Show.
Embodiment 3
（1）Water and alcohol are configured to mixed solvent；Wherein：60 parts by weight of water, 40 parts by weight of alcohol；Alcohol is n-butanol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, polyurethane modified acrylic resin lotion is added, is warming up to 80 DEG C, continues to stir 30min, it is molten to obtain organic modifiers
Liquid；Wherein：70 parts by weight of mixed solvent, 1 parts by weight of titanate coupling agent, 1 parts by weight of surfactant, polyurethane-modified propylene
28 parts by weight of acid resin lotion；Titanate coupling agent is that two (dioctyl pyrophosphoryl bases) close fluoroacetic acid ester titanium；Surfactant is
Dioctyl succinate disulfonate acid；The solid content of polyurethane modified acrylic resin lotion is 40%；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continues to stir 30min, filter, it is dry, it obtains
The titanium dioxide coated to organically-modified film；Wherein：40 parts by weight of titanium dioxide, 60 parts by weight of organically-modified agent solution；Titanium dioxide
Average grain diameter is 0.25 μm, content of titanium dioxide 99%；Dry is vacuum drying, and temperature is 80 DEG C, time 20h.
Polyethylene reflective membrane made from modified titanium made from embodiment 3, reflection coefficient, tensile strength such as 1 institute of table
Show.
Embodiment 4
（1）Water and alcohol are configured to mixed solvent；Wherein：30 parts by weight of water, 70 parts by weight of alcohol；Alcohol is n-hexyl alcohol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, polyurethane modified acrylic resin lotion is added, is warming up to 65 DEG C, continues to stir 45min, it is molten to obtain organic modifiers
Liquid；Wherein：67 parts by weight of mixed solvent, 1 parts by weight of titanate coupling agent, 2 parts by weight of surfactant, polyurethane-modified propylene
30 parts by weight of acid resin lotion；Titanate coupling agent is two (dioctyl pyrophosphoryl base) ethylene titanate esters；Surfactant is ten
Dialkyl benzene sulfonic acids sodium；The solid content of polyurethane modified acrylic resin lotion is 32%；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continues to stir 18min, filter, it is dry, it obtains
The titanium dioxide coated to organically-modified film；Wherein：25 parts by weight of titanium dioxide, 75 parts by weight of organically-modified agent solution；Titanium dioxide
Average grain diameter is 0.22 μm, content of titanium dioxide 97%；Dry is vacuum drying, and temperature is 72 DEG C, time 23h.
Polyethylene reflective membrane made from modified titanium made from embodiment 4, reflection coefficient, tensile strength such as 1 institute of table
Show.
Embodiment 5
（1）Water and alcohol are configured to mixed solvent；Wherein：50 parts by weight of water, 50 parts by weight of alcohol；Alcohol is 2- propyl alcohol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, polyurethane modified acrylic resin lotion is added, is warming up to 75 DEG C, continues to stir 35min, it is molten to obtain organic modifiers
Liquid；Wherein：64 parts by weight of mixed solvent, 2 parts by weight of titanate coupling agent, 2 parts by weight of surfactant, polyurethane-modified propylene
32 parts by weight of acid resin lotion；Titanate coupling agent is isopropyl three (dioctyl phosphoryl) titanate esters ester；Surfactant is
Sodium glycocholate；The solid content of polyurethane modified acrylic resin lotion is 38%；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continues to stir 25min, filter, it is dry, it obtains
The titanium dioxide coated to organically-modified film；Wherein：35 parts by weight of titanium dioxide, 65 parts by weight of organically-modified agent solution；Titanium dioxide
Average grain diameter is 0.24 μm, content of titanium dioxide 99%；Dry is vacuum drying, and temperature is 77 DEG C, time 21h.
Polyethylene reflective membrane made from modified titanium made from embodiment 5, reflection coefficient, tensile strength such as 1 institute of table
Show.
Comparative example 1
（1）Water and alcohol are configured to mixed solvent；Wherein：40 parts by weight of water, 60 parts by weight of alcohol；Alcohol is 2- methyl -2- butanol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, 70 DEG C are warming up to, continues to stir 40min, obtains organically-modified agent solution；Wherein：98 parts by weight of mixed solvent, titanate esters
1 parts by weight of coupling agent, 1 parts by weight of surfactant；Titanate coupling agent is isopropyl three (positive ethylamino-ethylamino) metatitanic acid
Ester；Surfactant is odium stearate；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continues to stir 22min, filter, it is dry, it obtains
The titanium dioxide coated to organically-modified film；Wherein：30 parts by weight of titanium dioxide, 70 parts by weight of organically-modified agent solution；Titanium dioxide
Average grain diameter is 0.23 μm, content of titanium dioxide 98%；Dry is vacuum drying, and temperature is 75 DEG C, time 22h.
Polyurethane modified acrylic resin lotion, Modified Titanium obtained are added not in organically-modified agent solution for comparative example 1
Polyethylene reflective membrane made from white powder, reflection coefficient, tensile strength such as table 1.
The test method of above-mentioned performance indicator is：
Under equal conditions, polyethylene tree is added with mass fraction 40% in modified titanium embodiment 1-5, comparative example 1 obtained
Vinyon reflective membrane is made in fat, casting film-forming；Reflective membrane made of polyethylene is added with non-modified titanium dioxide to carry out
Compare.
A length of 150mm, width 100mm are intercepted, the polyethylene reflective membrane that average thickness is 0.5mm is used as sample
ZRP6030 intensity of light reflection testers measure white light reflection coefficient of the sample when viewing angle is 0.2 °, incidence angle is 15 °, and repeatedly 3
Secondary calculating average value；Then using commercially available faintly acid plastic cleaning agent carry out surface clean, measure respectively repeatedly clean 10 times,
100 times and 300 times intensities of light reflection.
It is 150mm that length, which is made, in vinyon reflective membrane, and width 50mm, average thickness is the batten of 0.5mm, is adopted
With Labthink Intelligent electronic tensil testing machines, tensile strength test is carried out with the test speed of 500mm/min, measures reflective modeling
Expect the tensile strength of film.
Table 1：
Claims (8)
1. a kind of preparation method of modified titanium for plastic light reflecting film, which is characterized in that the detailed process of preparation is：
（1）Water and alcohol are configured to mixed solvent；Wherein：20 ~ 60 parts by weight of water, 40 ~ 80 parts by weight of alcohol；
（2）It stirs on one side, on one side to step（1）In the mixed solvent titanate coupling agent and surfactant is added, mixing is equal
After even, polyurethane modified acrylic resin lotion is added, is warming up to 60 ~ 80 DEG C, continues 30 ~ 50min of stirring, obtains organic change
Property agent solution；Wherein：60 ~ 70 parts by weight of mixed solvent, 1 ~ 2 parts by weight of titanate coupling agent, 1 ~ 2 parts by weight of surfactant,
28 ~ 36 parts by weight of polyurethane modified acrylic resin lotion；
（3）Divided titanium dioxide is scattered to step（2）In organically-modified agent solution obtained, continue 15 ~ 30min of stirring, filter, does
It is dry, obtain the titanium dioxide of organically-modified film cladding；Wherein：20 ~ 40 parts by weight of titanium dioxide, 60 ~ 80 weight of organically-modified agent solution
Part.
2. the preparation method of a kind of modified titanium for plastic light reflecting film according to claim 1, it is characterised in that：Step
Suddenly（1）The alcohol is ethyl alcohol, normal propyl alcohol, n-butanol, n-hexyl alcohol, n-amyl alcohol, 2- propyl alcohol, 2- butanol, 2- hexanols, cyclohexanol, uncle
At least one of butanol, 2- methyl -2- butanol.
3. the preparation method of a kind of modified titanium for plastic light reflecting film according to claim 1, it is characterised in that：Step
Suddenly（2）The titanate coupling agent is isopropyl three (isostearoyl base) titanate esters, isopropyl three (dioctyl pyrophosphoryl base) titanium
Acid esters, two (dioctyl pyrophosphoryl bases) close fluoroacetic acid ester titanium, two (dioctyl pyrophosphoryl base) ethylene titanate esters, isopropyl three (two
Octyl phosphoryl) titanate esters, at least one of isopropyl three (positive ethylamino-ethylamino) titanate esters.
4. the preparation method of a kind of modified titanium for plastic light reflecting film according to claim 1, it is characterised in that：Step
Suddenly（2）The surfactant is sulfated castor oil, sldium lauryl sulfate, dioctyl succinate disulfonate acid, detergent alkylate
At least one of sodium sulfonate, sodium glycocholate, odium stearate.
5. the preparation method of a kind of modified titanium for plastic light reflecting film according to claim 1, it is characterised in that：Step
Suddenly（2）The solid content of the polyurethane modified acrylic resin lotion is 30 ~ 40%.
6. the preparation method of a kind of modified titanium for plastic light reflecting film according to claim 1, it is characterised in that：Step
Suddenly（3）The average grain diameter of the titanium dioxide is 0.2 ~ 0.25 μm, and content of titanium dioxide is 97 ~ 99%.
7. the preparation method of a kind of modified titanium for plastic light reflecting film according to claim 1, it is characterised in that：Step
Suddenly（3）The drying be vacuum drying, temperature be 70 ~ 80 DEG C, the time be 20 ~ for 24 hours.
8. a kind of modified titanium for plastic light reflecting film that any one of claim 1 ~ 7 the method is prepared.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607699A (en) * | 2019-08-26 | 2019-12-24 | 佛山佛塑科技集团股份有限公司 | Breathable light-reflecting grass-proof base fabric and preparation method thereof |
| CN111897040A (en) * | 2020-08-12 | 2020-11-06 | 常州市日月反光材料有限公司 | High-strength tear-resistant reflective film and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607699A (en) * | 2019-08-26 | 2019-12-24 | 佛山佛塑科技集团股份有限公司 | Breathable light-reflecting grass-proof base fabric and preparation method thereof |
| CN110607699B (en) * | 2019-08-26 | 2022-04-26 | 佛山佛塑科技集团股份有限公司 | Breathable light-reflecting grass-proof base fabric and preparation method thereof |
| CN111897040A (en) * | 2020-08-12 | 2020-11-06 | 常州市日月反光材料有限公司 | High-strength tear-resistant reflective film and preparation process thereof |
| CN111897040B (en) * | 2020-08-12 | 2022-04-15 | 常州市日月反光材料有限公司 | High-strength tear-resistant reflective film and preparation process thereof |
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