CN109233223B - Hydrophilic transparent polyester film and preparation method thereof - Google Patents
Hydrophilic transparent polyester film and preparation method thereof Download PDFInfo
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- CN109233223B CN109233223B CN201811113269.5A CN201811113269A CN109233223B CN 109233223 B CN109233223 B CN 109233223B CN 201811113269 A CN201811113269 A CN 201811113269A CN 109233223 B CN109233223 B CN 109233223B
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- 229920006267 polyester film Polymers 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims description 32
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 30
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 19
- 239000012046 mixed solvent Substances 0.000 claims description 16
- 238000005266 casting Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 claims description 5
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 14
- 229920002799 BoPET Polymers 0.000 description 10
- LQLQDKBJAIILIQ-UHFFFAOYSA-N Dibutyl terephthalate Chemical compound CCCCOC(=O)C1=CC=C(C(=O)OCCCC)C=C1 LQLQDKBJAIILIQ-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 239000000693 micelle Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical group C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- YHASWHZGWUONAO-UHFFFAOYSA-N butanoyl butanoate Chemical compound CCCC(=O)OC(=O)CCC YHASWHZGWUONAO-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/19—Quaternary ammonium compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
The invention belongs to the technical field of polyester film modification, and particularly relates to a hydrophilic transparent polyester film and a preparation method thereof.
Description
Technical Field
The invention belongs to the technical field of polyester film modification, and particularly relates to a hydrophilic transparent polyester film and a preparation method thereof.
Background
PET is a main variety in thermoplastic polyester, has good film forming property, good friction resistance, dimensional stability, electrical insulation, weather resistance and optical performance, and determines that PET films are widely applied in many fields.
When the PET film is used for protecting films on surfaces of vehicle windows and doors, the PET film is required to have high transparency and hydrophilic performance so as to be used in environments such as moist and high fog.
The surface active agent generally has a hydrophilic end and a lipophilic end, when the surface active agent is mixed with a PET matrix to prepare the film, the lipophilic end tends to extend into a PET solid phase, and the hydrophilic end tends to extend out of the PET and point to an air phase.
The quantity of the hydrophilic ends extending out of the PET film can be correspondingly increased by increasing the dosage of the surfactant, so that the hydrophilicity of the surface of the PET film is improved, but the proportion of the surfactant in the PET film for forming micelles is increased, so that the light transmittance of the film is reduced, and therefore, when the hydrophilicity of the PET film is improved by using the surfactant at present, the adding quantity of the surfactant is greatly limited, so that the hydrophilicity of the film is improved to a limited extent.
Disclosure of Invention
In order to solve the technical problems, the invention provides a hydrophilic transparent polyester film and a preparation method thereof, the hydrophilic transparent polyester film comprises PET, a surfactant and bisphenol A dibutyrate,
the polyester resin comprises, by weight, 100 parts of PET, 5-8 parts of a surfactant and 6-9.5 parts of bisphenol A dibutyl ester.
The invention also provides a preparation method of the hydrophilic transparent polyester film, which comprises the following steps:
(1) adding PET particles and bisphenol A dibutyrate into a mixed solvent of tetrachloroethane and phenol, heating, stirring and dissolving to obtain a uniform mixed solution,
in the mixed solvent, the mass ratio of tetrachloroethane to phenol is 1-2.5: 1,
the mass ratio of the PET particles to the mixed solvent is 0.8-1.2: 10;
(2) adding a surfactant into the mixed solution obtained in the step (1) and fully stirring to obtain a uniform membrane casting solution;
(3) flatly paving the casting solution obtained in the step (2) on the surface of a matrix, drying and curing to obtain a hydrophilic transparent polyester film,
the substrate is a glass sheet, the casting film liquid is flatly paved on the surface of the substrate by adopting a coating or spraying mode, the drying temperature is controlled to be 55-75 ℃, and the drying time is 45-80 minutes.
In the scheme of this application, through the effect of bisphenol A dibutyrate, when using surfactant to improve PET film hydrophilicity, can effectively improve surfactant's quantity, effectively improved the hydrophilicity on membrane surface promptly to the negative effect to PET film's light transmissivity after fully having avoided surfactant quantity to increase.
Detailed Description
Comparative example 1
(1) Tetrachloroethane and phenol were mixed as 1.8: 1, fully stirring at 60 ℃ to obtain a mixed solvent of tetrachloroethane and phenol,
taking 100g of the mixed solvent, adding 10g of PET particles into the mixed solvent, heating to 75 ℃, and stirring to dissolve the mixture to obtain uniform mixed solution;
(2) adding 0.45g of surfactant tetradecyltrimethyl ammonium chloride into the mixed solution obtained in the step (1) under the heat preservation state, and fully stirring to obtain uniform membrane casting solution;
(3) and (3) flatly paving the casting solution obtained in the step (2) on the surface of a glass substrate in a coating mode, and drying the glass substrate at 70 ℃ in vacuum to obtain the hydrophilic transparent polyester film, wherein the thickness of the film is 45 microns.
The film was tested to have a contact angle with water of 36.17 ° in air and a light transmission of 95%.
Comparative example 2
The amount of the surfactant was increased based on the comparative example 1:
(1) tetrachloroethane and phenol were mixed as 1.8: 1, fully stirring at 60 ℃ to obtain a mixed solvent of tetrachloroethane and phenol,
taking 100g of the mixed solvent, adding 10g of PET particles into the mixed solvent, heating to 75 ℃, and stirring to dissolve the mixture to obtain uniform mixed solution;
(2) adding 0.75g of surfactant tetradecyltrimethyl ammonium chloride into the mixed solution obtained in the step (1) under the heat preservation state, and fully stirring to obtain uniform membrane casting solution;
(3) and (3) flatly paving the casting solution obtained in the step (2) on the surface of a glass substrate in a coating mode, and drying the glass substrate in vacuum at 70 ℃ to obtain the hydrophilic transparent polyester film, wherein the thickness of the film is controlled to be 45 microns.
The film was tested to have a contact angle with water of 30.62 ° in air and a light transmission of 81%.
From comparative examples 1 and 2, the hydrophilicity of the PET film did increase when the amount of the surfactant was increased, but the transmittance was significantly decreased, as mentioned above, due to the formation of micelles with more surfactant.
Example 1
Bisphenol a dibutyrate was added on the basis of comparative example 2:
preparation of bisphenol a dibutyrate:
according to the mass ratio of bisphenol A to xylene of 1: and 80, sufficiently dispersing the bisphenol A in xylene, adding 2.3 mol times of n-butyric anhydride of the bisphenol A and 1.5 wt% of catalyst lithium acetate into the mixture, sufficiently stirring and mixing the mixture, heating the mixture to a reflux state, stirring the mixture for reaction for 12 hours, removing solvent xylene by rotary evaporation after the reaction is finished, sufficiently washing the residue after the rotary evaporation with a sodium hydroxide solution, and drying the residue at 60 ℃.
(1) Tetrachloroethane and phenol were mixed as 1.8: 1, fully stirring at 60 ℃ to obtain a mixed solvent of tetrachloroethane and phenol,
taking 100g of the mixed solvent, adding 10g of PET particles and 0.8g of the prepared bisphenol A dibutyrate into the mixed solvent, heating to 75 ℃, and stirring to dissolve to obtain uniform mixed solution;
(2) adding 0.75g of surfactant tetradecyltrimethyl ammonium chloride into the mixed solution obtained in the step (1) under the heat preservation state, and fully stirring to obtain uniform membrane casting solution;
(3) and (3) flatly paving the casting solution obtained in the step (2) on the surface of a glass substrate in a coating mode, and drying the glass substrate for 60 minutes in vacuum at 70 ℃ to obtain the hydrophilic transparent polyester film, wherein the thickness of the film is 45 microns.
The film was tested to have a contact angle with water of 23.45 ° in air and a light transmittance of 91%.
Compared with the comparative example 2, the reduction degree of the light transmittance of the film is obviously reduced under the premise of adding the same amount of the surfactant. The applicant believes that the reason is:
the PET structure is mainly long chains, certain space distance exists between the long chains which are arranged in parallel, surfactant molecules can move to a large extent in the space channels, and hydrophilic groups and lipophilic groups on the surfactant molecules are attracted and gathered together to form micelles based on the mutual attraction of the hydrophilic groups and the lipophilic groups on the surfactant molecules;
after the bisphenol A dibutyrate is added, two butyl groups on the structure of the bisphenol A dibutyrate are easy to form a tangling effect with PET long chains, when the two butyl groups of the same bisphenol A dibutyrate are respectively tangled on different PET long chains, a transverse interception barrier is similarly set up on a space channel between the two PET long chains, the moving range of surfactant molecules in the space channel is limited, so that a part of surfactants are inhibited from being gathered together to form micelles, and the descending amplitude of light transmittance after film forming is obviously reduced when the same amount of the surfactants are added.
On the other hand, compared to comparative example 2, the hydrophilicity of the film in example 1 is significantly higher than that of comparative example 2 based on the addition of the same amount of surfactant, which fully illustrates that in the embodiment of example 1, the amount of surfactant aggregated into micelles is smaller, so that more hydrophilic ends of the surfactant molecules can fully exert their own hydrophilic effect.
Comparative example 1
The "bisphenol a dibutyrate" in example 1 was replaced with equimolar dibutyl terephthalate:
(1) tetrachloroethane and phenol were mixed as 1.8: 1, fully stirring at 60 ℃ to obtain a mixed solvent of tetrachloroethane and phenol,
taking 100g of the mixed solvent, adding 10g of PET particles and 0.6g of dibutyl terephthalate, heating to 75 ℃, stirring and dissolving to obtain a uniform mixed solution;
(2) adding 0.75g of surfactant tetradecyltrimethyl ammonium chloride into the mixed solution obtained in the step (1) under the heat preservation state, and fully stirring to obtain uniform membrane casting solution;
(3) and (3) flatly paving the casting solution obtained in the step (2) on the surface of a glass substrate in a coating mode, and drying the glass substrate for 60 minutes in vacuum at 70 ℃ to obtain the hydrophilic transparent polyester film, wherein the thickness of the film is 45 microns.
The film was tested to have a contact angle with water of 32.21 ° in air and a light transmission of 80%.
The hydrophilicity and transmittance of the film obtained in this comparative example were very close to those of comparative example 2, and it was found that the effect similar to that of this example was not obtained when dibutyl terephthalate was used.
In this regard, the applicants believe that: although the dibutyl terephthalate is similar to bisphenol a dibutyrate in the length of the molecular chain and the end groups are the same as bisphenol a dibutyrate and are all alkyl chains, the structure of the dibutyl terephthalate only contains one benzene ring and does not contain a methyl side chain (in the scheme, the bisphenol a dibutyrate is connected with two methyl side chains on the carbon atom between the two benzene rings). Based on the structure, after the dibutyl terephthalate enters the PET matrix resin, the orientation of the dibutyl terephthalate is easily assimilated by the long chain orientation of PET, so that the molecular chain of the dibutyl terephthalate tends to approach the length trend of the PET chain in the length walking direction, and thus the dibutyl terephthalate cannot well tangle different PET molecular chains in a state of being transversely vertical to the length direction of the PET chain; on the bisphenol A dibutyrate in the scheme, the molecular structure distribution of two benzene rings and methyl side chains just can lead the bisphenol A dibutyrate not to be assimilated by the trend of the PET long chains easily, and the transverse blocking effect of the bisphenol A dibutyrate on a space channel between the two PET long chains can be fully exerted.
In addition, from experimental data, the hydrophilicity of comparative example 1 is slightly worse than that of comparative example 2, which also shows that the small amount of dibutyl terephthalate added in comparative example 1 should tend to be hydrophobic, while the structure of the bisphenol a dibutyrate in the present scheme is provided with one more benzene ring and two more methyl side groups, and the hydrophobicity should be more obvious, but the hydrophilic result of the present scheme example 1 is just the opposite, which further proves that the addition of the bisphenol a dibutyrate in the present scheme greatly reduces the amount of the surfactant aggregated into micelles, so that more hydrophilic ends of the surfactant molecules can fully exert their own hydrophilic effect.
Claims (1)
1. A preparation method of a hydrophilic transparent polyester film is characterized by comprising the following steps: the preparation method comprises the following steps of,
(1) tetrachloroethane and phenol were mixed as 1.8: 1, fully stirring at 60 ℃ to obtain a mixed solvent of tetrachloroethane and phenol,
taking 100g of the mixed solvent, adding 10g of PET particles and 0.8g of bisphenol A dibutyrate, heating to 75 ℃, and stirring to dissolve to obtain uniform mixed solution;
(2) adding 0.75g of surfactant tetradecyltrimethyl ammonium chloride into the mixed solution obtained in the step (1) under the heat preservation state, and fully stirring to obtain uniform membrane casting solution;
(3) and (3) flatly paving the casting solution obtained in the step (2) on the surface of a glass substrate in a coating mode, and drying the glass substrate at 70 ℃ for 60 minutes in vacuum to obtain the hydrophilic transparent polyester film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811113269.5A CN109233223B (en) | 2018-09-25 | 2018-09-25 | Hydrophilic transparent polyester film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811113269.5A CN109233223B (en) | 2018-09-25 | 2018-09-25 | Hydrophilic transparent polyester film and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN109233223A CN109233223A (en) | 2019-01-18 |
| CN109233223B true CN109233223B (en) | 2020-07-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811113269.5A Active CN109233223B (en) | 2018-09-25 | 2018-09-25 | Hydrophilic transparent polyester film and preparation method thereof |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111793986B (en) * | 2019-04-09 | 2022-10-18 | 广东炬盛新材料科技有限公司 | Nylon moisture-absorbing and sweat-releasing finishing agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513401A (en) * | 2014-11-03 | 2015-04-15 | 中国科学院宁波材料技术与工程研究所 | Polyethylene glycol terephthalate transparent film with strong hydrophilicity and preparation method thereof |
| CN105694089A (en) * | 2016-04-27 | 2016-06-22 | 山东科技大学 | Preparation method of super-hydrophilic PET membrane material |
-
2018
- 2018-09-25 CN CN201811113269.5A patent/CN109233223B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513401A (en) * | 2014-11-03 | 2015-04-15 | 中国科学院宁波材料技术与工程研究所 | Polyethylene glycol terephthalate transparent film with strong hydrophilicity and preparation method thereof |
| CN105694089A (en) * | 2016-04-27 | 2016-06-22 | 山东科技大学 | Preparation method of super-hydrophilic PET membrane material |
Non-Patent Citations (1)
| Title |
|---|
| Transesterifications of Poly(bisphenol Acarbonate) with Aromatic and Aliphatic Segments in Ethylene Terephthalate-Caprolactone Copolyester;ZHONGPING ZHANG et al.;《Journal of Applied Polymer Science》;20011231;第80卷;1558-1565 * |
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