CN111411415A - Graphene modified flexible polyester - Google Patents
Graphene modified flexible polyester Download PDFInfo
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- CN111411415A CN111411415A CN202010381874.1A CN202010381874A CN111411415A CN 111411415 A CN111411415 A CN 111411415A CN 202010381874 A CN202010381874 A CN 202010381874A CN 111411415 A CN111411415 A CN 111411415A
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- Prior art keywords
- graphene
- flexible polyester
- polyester
- modified
- terylene
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/91—Polymers modified by chemical after-treatment
- C08G63/914—Polymers modified by chemical after-treatment derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/916—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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
Abstract
The invention discloses graphene modified flexible polyester, which is characterized in that graphene and polyester are modified so as to be better combined together, the graphene is treated at first, and the graphene is oxidized to obtain oxidized graphene containing hydrophilic groups such as carboxyl, alkyl and the like, and the oxidized graphene has better dispersibility and adsorbability compared with the graphene; meanwhile, the polyester is subjected to amination modification by matching with ethylenediamine, so that polar groups on the surface of the novel polyester are increased, the adsorption capacity of groups such as carboxyl, alkyl, epoxy and the like is improved, and the high-conductivity flexible polyester is obtained; on one hand, the problems of yarn breakage and blockage of the existing terylene in the spinning process are solved, and on the other hand, the conductivity of the whole terylene is enhanced, so that a foundation is provided for the popularization and application of intelligent equipment.
Description
Technical Field
The invention relates to the field of conductive polyester, in particular to graphene modified flexible polyester.
Background
In the textile field, there is an increasing interest in developing high performance or functional fibers, such as: flame retardant, self-cleaning, temperature control, electrical conductivity, and catalytic properties, among which electrical conductivity is of particular concern. The conductive fabric can be used for the production of intelligent textiles with integrated sensors or various electronic devices, and at present, various methods for preparing the conductive fiber are available, for example, common fiber and metal filament are blended to obtain the conductive fiber, but the fabric feels hard, and the fiber is damaged due to continuous bending and stretching in the fiber.
Graphene is a planar film with a hexagonal honeycomb lattice composed of SP2 hybridized carbon atoms, is only one carbon atom thick, and is a two-dimensional material. The graphene is a carbon material with a layered structure, and the upper and lower adjacent layers form the layered structure after being overlapped in parallel. The graphene is a structural foundation of other carbon materials, can be agglomerated into zero-dimensional fullerene, is curled into a one-dimensional carbon nanotube, and is stacked layer by layer to form three-dimensional graphite. Graphene is paid much attention to due to good electronic conductivity, high specific surface area and strong mechanical properties, so how to combine graphene and terylene to obtain modified terylene with conductive property is a technical problem to be solved urgently.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides the graphene modified flexible polyester, so that the problems of yarn breakage and blockage in the spinning process of the existing polyester are solved, and the conductivity of the whole polyester is enhanced, thereby providing a foundation for popularization and application of intelligent equipment.
In order to achieve the purpose, the invention provides graphene modified flexible polyester, and the preparation method comprises the following steps:
s1: carrying out physical stripping to obtain graphene, grinding for multiple times to obtain graphene slurry with the particle size of about 1mm, washing for multiple times, dehydrating, drying, and carrying out vacuum purification to obtain graphene nanoplatelets with the particle size of 1 mm;
s2, oxidizing the graphene nanoplatelets;
s3, mixing and emulsifying the oxidized graphene, glycol, a coupling agent and an emulsifier to obtain finely dispersed slurry containing the graphene;
s4, purifying the terephthalic acid and then reacting with the fine dispersion slurry to obtain polyethylene glycol terephthalate, namely terylene;
s5, mixing ethylenediamine and sodium hydroxide to obtain a mixed solution, placing the terylene in the mixed solution for treatment to obtain a flexible terylene primary product after the treatment is finished;
s6: and (3) putting the modified polyester primary product into graphene oxide for dipping, then taking out, cleaning and drying to finally obtain the flexible polyester.
Preferably, in step S2, the method for oxidizing graphene is: adding graphite powder into concentrated sulfuric acid, then adding sodium carbonate and potassium permanganate, and then heating and stirring; and then adding deionized water and a hydrogen peroxide solution, stirring, cooling, centrifuging, selecting supernate, adding hydrochloric acid, centrifuging, adding deionized water, and continuing centrifuging to obtain an oxidized graphene suspension.
Preferably, in step S3, ethylene glycol is first put into a stirrer, 0.5 to 1% by mass of a coupling agent and an emulsifier are added, the mixture is stirred for a while, then, a graphene suspension with a mass ratio of 3.5 to 5.5% is added, the mixture is continuously stirred, and then, the mixture is put into a homogenizer for emulsification, so that a graphene-containing finely dispersed slurry is obtained.
Preferably, the coupling agent is a chelating titanate coupling agent; the emulsifier is a cationic emulsifier and comprises one of alkyl ammonium salt or quaternary ammonium salt.
Preferably, in step S5, the dacron is modified in an infrared high-temperature dyeing prototype, EDA (ethylenediamine) and sodium hydroxide solution are added into a dyeing cup, then the temperature is raised from room temperature to 60 ℃ at the speed of 2 ℃/min, the temperature is kept for 30min, then the temperature is lowered to room temperature at the speed of 3 ℃/min, and the dacron is washed to be neutral by distilled water after being taken out and dried.
Preferably, in step S5, when the polyester is placed in the dyeing cup, the ratio of the mass of the polyester to the volume of the modified liquid is 1: 20.
preferably, in step S6, firstly, PH adjustment is performed on the graphene suspension, then the flexible polyester primary product is immersed in the graphene suspension after PH adjustment, and is taken out and dried after a period of time, and is reduced by a reducing agent for 30 minutes after being cooled to 60 ℃, and is taken out and washed by distilled water to be neutral and dried, so as to obtain the flexible polyester product.
Preferably, the graphene suspension is adjusted with acetic acid or a sodium bicarbonate solution so that the PH of the entire suspension is about 6, and the entire suspension is weakly acidic.
Preferably, the flexible terylene primary product is taken out after being soaked for 60 to 80 minutes, baked for 20 minutes at 90 ℃, then cooled to 60 ℃, and one of sodium hydrosulfite (sodium hydrosulfite) or hydrazine hydrate is used as a reducing agent.
The invention has the beneficial effects that: according to the method, graphene is firstly treated, and is subjected to oxidation treatment to obtain graphene oxide containing hydrophilic groups such as carboxyl and alkyl, and the graphene oxide has better dispersibility and adsorbability compared with graphene; in addition, the existing terylene has strong hydrophobicity, and the surface lacks polar groups, so that a novel terylene needs to be prepared, and meanwhile, the novel terylene is matched with ethylenediamine for amination modification, so that the polar groups on the surface of the novel terylene are increased, the adsorption capacity to groups such as carboxyl, alkyl, epoxy and the like is improved, and the high-conductivity flexible terylene is obtained.
Drawings
FIG. 1 is a flow chart of the steps of the present invention;
FIG. 2 is a graph showing an experiment of the concentration of the reducing agent according to the present invention.
Detailed Description
In order to more clearly describe the present invention, the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, the application discloses a graphene modified flexible polyester, which is characterized in that,
mainly comprises the following steps: firstly, obtaining graphene, then processing the graphene to finally obtain graphene oxide; reacting the obtained graphene oxide with ethylene glycol and the like to obtain terylene, performing amination modification on the obtained terylene by adopting ethylenediamine, and reacting the obtained terylene with the graphene oxide again to finally obtain a final product: the flexible terylene is prepared by the following steps in more detail:
s1: carrying out physical stripping to obtain graphene, grinding for multiple times to obtain graphene slurry with the particle size of about 1mm, washing for multiple times, dehydrating, drying, and carrying out vacuum purification to obtain graphene nanoplatelets with the particle size of 1 mm;
s2, oxidizing the graphene nanoplatelets;
s3, mixing and emulsifying the oxidized graphene, glycol, a coupling agent and an emulsifier to obtain finely dispersed slurry containing the graphene;
s4, purifying the terephthalic acid and then reacting with the fine dispersion slurry to obtain polyethylene glycol terephthalate, namely terylene;
s5, mixing ethylenediamine and sodium hydroxide to obtain a mixed solution, placing the terylene in the mixed solution for treatment to obtain a flexible terylene primary product after the treatment is finished;
s6: and (3) putting the modified polyester primary product into graphene oxide for dipping, then taking out, cleaning and drying to finally obtain the flexible polyester.
More specifically, the graphene oxidation method comprises the steps of adding graphite powder into concentrated sulfuric acid, adding sodium carbonate and potassium permanganate, heating and stirring, adding deionized water and a hydrogen peroxide solution, stirring, cooling, centrifuging, selecting a supernatant, adding hydrochloric acid, centrifuging, adding deionized water, continuously centrifuging to obtain an oxidized graphene suspension, in the specific embodiment, weighing 2g of graphite powder, adding 50ml of concentrated sulfuric acid, slowly stirring by using a glass rod, adding 2g of sodium carbonate, stirring by placing on a magnetic stirrer, controlling the temperature to be about 15 ℃, slowly adding 6g of potassium permanganate into a middle plate, keeping stirring for one hour, heating to 35 ℃, continuously stirring for 20 hours, slowly adding 90ml of deionized water, heating to 85 ℃, continuously stirring for 1 hour, adding 30% of hydrogen peroxide solution, stirring until the solution is bright yellow, cooling, centrifuging, placing the prepared solution into a centrifuge, centrifuging at a speed of 5000 plus material 6000r/min for 5-10 minutes, adding 351.5 mol/5 mol of the supernatant, adding 355.5 mol/5 mol of the supernatant, and repeatedly adding the supernatant into a supernatant of the supernatant, and centrifuging the supernatant again, and taking the supernatant again the supernatant of graphene suspension, wherein the pH value of the supernatant is about 3-2.
The preparation of terylene: firstly, putting ethylene glycol into a stirrer, adding 0.5-1% of coupling agent and emulsifier according to the mass ratio, stirring for a period of time, adding 3.5-5.5% of graphene suspension liquid, continuously stirring, and then putting into a homogenizer for emulsification to obtain finely dispersed slurry containing graphene; the coupling agent is a chelating titanate coupling agent; the emulsifier is cationic emulsifier, and comprises one of alkyl ammonium salt or quaternary ammonium salt. More specifically, the emulsifier is designed as a cationic emulsifier, because the graphene suspension is weakly acidic in the whole reaction system, and the pH is about 6, the graphene suspension is just the optimal reaction pH value of the cationic emulsifier for emulsion polymerization, such as dodecyl ammonium chloride, so that the optimal reaction rate is achieved, and the emulsified fine dispersion slurry is obtained more quickly; in the specific operation, firstly putting ethylene glycol into a dispersion machine, then putting 0.5-1% of chelating titanate coupling agent and dodecyl ammonium chloride according to the mass ratio, stirring for 15-20 minutes, then putting 3.5-5.5% of graphene suspension liquid according to the mass ratio, continuously stirring at the speed of 800r/min for 20 minutes, then putting into a homogenizer for emulsification, then putting into a sand mill for grinding for 2-3 hours, sieving through a 800-plus-1000-mesh sieve to obtain fine dispersion slurry containing graphene, finally purifying benzene dimethanol, then carrying out esterification reaction with the fine dispersion slurry at 170 ℃ of 150-plus-170 ℃, then heating to 280 ℃ for polycondensation to obtain initial terylene; due to the action of the emulsifier, the surface of the terylene contains hydrophilic groups and other polar groups, which is beneficial to adsorbing and fixing the graphene oxide.
Modifying the terylene in an infrared high-temperature dyeing prototype, adding EDA (ethylenediamine) and sodium hydroxide solution into a dyeing cup, increasing the temperature from room temperature to 60 ℃ at the speed of 2 ℃/min, preserving the temperature for 30min, reducing the temperature to room temperature at the speed of 3 ℃/min, taking out, washing the terylene to be neutral by using distilled water, drying, and placing the terylene in the dyeing cup, wherein the ratio of the mass of the terylene to the volume of a modified solution is 1: 20, so as to modify the terylene, wherein the reaction equation is as follows:
the method comprises the steps of firstly adjusting the pH of a graphene suspension liquid, adopting an acetic acid or sodium bicarbonate solution to adjust the graphene suspension liquid to enable the pH of the whole suspension liquid to be about 6 and to be weakly acidic, then putting a flexible terylene primary product into the graphene suspension liquid after the pH adjustment to be soaked, taking out and drying the flexible terylene primary product after one end of the flexible terylene primary product is carried out for a while, then reducing the flexible terylene primary product to 60 ℃ for 30 minutes by using a reducing agent, taking out the flexible terylene primary product, washing the flexible terylene primary product to be neutral and drying the flexible terylene primary product by using distilled water, more specifically, taking out the flexible terylene primary product after being soaked for 60-80 minutes, drying the flexible terylene primary product for 20 minutes at 90 ℃, cooling the flexible terylene primary product to 60 ℃, adopting one of sodium hydrosulfite or hydrazine hydrate as a reducing agent, firstly adjusting the pH of the graphene suspension liquid by using the acetic acid or the sodium bicarbonate to enable the pH of the solution to be about 6, controlling the pH of the solution to be 6 because the graphene oxide is electronegative in the solution, and the terylene after the ethylenediamine amination is adsorbed in the solution, but when the pH is the alkaline, the graphene is the optimal graphene oxide, the graphene is finally obtained by using an ionized graphene surface ionization test for 352, and finally selecting the graphene is carried out.
The invention has the advantages that:
1) the optimal pH value is adopted, so that the reaction rate can be effectively accelerated, and other reaction conditions cannot be damaged;
2) the obtained flexible polyester has strong conductivity and can be effectively used in the technical fields of intelligent wearing and the like;
3) in the spinning process, graphene is attached, so that the fiber is smoother and not easy to break.
The above disclosure is only for a few specific embodiments of the present invention, but the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (9)
1. The graphene modified flexible polyester is characterized in that the preparation method comprises the following steps:
s1: carrying out physical stripping to obtain graphene, grinding for multiple times to obtain graphene slurry with the particle size of about 1mm, washing for multiple times, dehydrating, drying, and carrying out vacuum purification to obtain graphene nanoplatelets with the particle size of 1 mm;
s2, oxidizing the graphene nanoplatelets;
s3, mixing and emulsifying the oxidized graphene, glycol, a coupling agent and an emulsifier to obtain finely dispersed slurry containing the graphene;
s4, purifying the terephthalic acid and then reacting with the fine dispersion slurry to obtain polyethylene glycol terephthalate, namely terylene;
s5, mixing ethylenediamine and sodium hydroxide to obtain a mixed solution, placing the terylene in the mixed solution for treatment to obtain a flexible terylene primary product after the treatment is finished;
s6: and (3) putting the modified polyester primary product into graphene oxide for dipping, then taking out, cleaning and drying to finally obtain the flexible polyester.
2. The graphene-modified flexible polyester according to claim 1, wherein in step S2, the method for oxidizing graphene is as follows: adding graphite powder into concentrated sulfuric acid, then adding sodium carbonate and potassium permanganate, and then heating and stirring; and then adding deionized water and a hydrogen peroxide solution, stirring, cooling, centrifuging, selecting supernate, adding hydrochloric acid, centrifuging, adding deionized water, and continuing centrifuging to obtain an oxidized graphene suspension.
3. The graphene-modified flexible polyester according to claim 1, wherein in step S3, ethylene glycol is first put into a stirrer, 0.5 to 1% of a coupling agent and an emulsifier are added according to a mass ratio, after stirring for a period of time, a graphene suspension with a mass ratio of 3.5 to 5.5% is added, and stirring is continued, and then the graphene-modified flexible polyester is put into a homogenizer for emulsification, so as to obtain a finely dispersed slurry containing graphene.
4. The graphene-modified flexible polyester according to claim 3, wherein the coupling agent is a chelating titanate coupling agent; the emulsifier is a cationic emulsifier and comprises one of alkyl ammonium salt or quaternary ammonium salt.
5. The graphene modified flexible polyester fiber according to claim 1, wherein in step S5, the polyester fiber is modified in an infrared high temperature dyeing prototype, EDA (ethylenediamine) and sodium hydroxide solution are added into a dyeing cup, the temperature is raised from room temperature to 60 ℃ at a rate of 2 ℃/min, the temperature is maintained for 30min, the temperature is lowered to room temperature at a rate of 3 ℃/min, and the polyester fiber is taken out, washed to be neutral by distilled water and dried.
6. The graphene-modified flexible polyester according to claim 5, wherein in step S5, when the polyester is placed in a dyeing cup, the ratio of the mass of the polyester to the volume of the modified liquid is 1: 20.
7. the graphene-modified flexible polyester according to claim 1, wherein in step S6, the PH of the graphene suspension is adjusted, the flexible polyester primary product is immersed in the PH-adjusted graphene suspension, the flexible polyester primary product is taken out and dried after a period of time, the flexible polyester primary product is reduced by a reducing agent for 30 minutes after being cooled to 60 ℃, and the flexible polyester product is washed by distilled water to be neutral and dried after being taken out, so that the flexible polyester product is obtained.
8. The graphene-modified flexible polyester according to claim 7, wherein the graphene suspension is adjusted by using acetic acid or sodium bicarbonate solution, so that the whole suspension has a pH =6 and is weakly acidic.
9. The graphene-modified flexible polyester fiber as claimed in claim 7, wherein the flexible polyester primary product is taken out after being soaked for 60-80 minutes, baked for 20 minutes at 90 ℃, and then cooled to 60 ℃, and one of sodium hydrosulfite (sodium hydrosulfite) or hydrazine hydrate is used as a reducing agent.
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|---|---|---|---|
| CN202010381874.1A CN111411415A (en) | 2020-05-08 | 2020-05-08 | Graphene modified flexible polyester |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010381874.1A CN111411415A (en) | 2020-05-08 | 2020-05-08 | Graphene modified flexible polyester |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212416A (en) * | 2014-08-30 | 2014-12-17 | 海安南京大学高新技术研究院 | Preparation method for paraffin microcapsule phase-change material modified by graphene oxide |
| CN107829294A (en) * | 2017-11-16 | 2018-03-23 | 江阴市博帆化纺有限公司 | A kind of modified polyester fibre production method |
| CN107892742A (en) * | 2017-12-05 | 2018-04-10 | 桐乡守敬应用技术研究院有限公司 | The terylene that a kind of graphene is modified |
-
2020
- 2020-05-08 CN CN202010381874.1A patent/CN111411415A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212416A (en) * | 2014-08-30 | 2014-12-17 | 海安南京大学高新技术研究院 | Preparation method for paraffin microcapsule phase-change material modified by graphene oxide |
| CN107829294A (en) * | 2017-11-16 | 2018-03-23 | 江阴市博帆化纺有限公司 | A kind of modified polyester fibre production method |
| CN107892742A (en) * | 2017-12-05 | 2018-04-10 | 桐乡守敬应用技术研究院有限公司 | The terylene that a kind of graphene is modified |
Non-Patent Citations (2)
| Title |
|---|
| 刘圆圆 等: ""氧化石墨烯共聚改性PET纤维的制备及表征"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 曹机良 等: ""石墨烯柔性导电涤纶织物的制备与性能"", 《精细化工》 * |
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