CN109505022A - A kind of preparation method of the modified dispersion liquid of graphene for spinning - Google Patents
A kind of preparation method of the modified dispersion liquid of graphene for spinning Download PDFInfo
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- CN109505022A CN109505022A CN201811371734.5A CN201811371734A CN109505022A CN 109505022 A CN109505022 A CN 109505022A CN 201811371734 A CN201811371734 A CN 201811371734A CN 109505022 A CN109505022 A CN 109505022A
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- Prior art keywords
- graphene
- dispersion liquid
- preparation
- modified dispersion
- stoste
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Classifications
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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
-
- 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
- D01F1/10—Other agents for modifying properties
Abstract
Invention broadly provides a kind of preparation methods of the modified dispersion liquid of graphene for spinning.The dispersion liquid is mainly made by micro crystal graphite, ethylene glycol, hydrofluoric acid, phosphoric acid, sodium hydroxide, ethyl alcohol, resin reaction, its process is as follows: micro crystal graphite, ethylene glycol are blended in acid-resistant container, hydrofluoric acid and phosphoric acid are compounded, and it is added in above-mentioned slurry and carries out ultrasound, sodium hydroxide ultrasound is added after a period of time, mixed slurry is made.It is used as stoste 1 spare after the slurry is carried out forward and reverse energization.Resin and ethyl alcohol are blended, 60 DEG C of obtained stostes 2 are warming up to.Stoste 1 and stoste 2 are distinguished into ultrasonic atomizatio, leads in reaction kettle and is reacted, the modified dispersion liquid of the liquid after collecting reaction, as graphene.The dispersion liquid can be used as ethylene glycol, be exclusively used in the in-situ synthesized reaction of polyester.Plug-hole, not fracture of wire, the terylene thermal conductivity of spinning do not have good mechanical property to graphene modified poly ester made from this method in spinning technique.
Description
Technical field
The present invention relates to a kind of preparation method of graphene modified material, especially a kind of modification dispersion liquid for spinning
Preparation method.
Background technique
Graphene is referred to as the material of 21 century " change ", is strongest two-dimensional material in nature now according to it is tested,
It is ten times of common steel.Graphene has excellent room temperature thermal conductivity and translucency, while as known resistance in the world
The smallest material of rate, its electric conductivity also with super strength.Above many features cause graphene in new energy, space flight, electricity
The fields such as son, military project have great application prospect, and become international research hotspot.
Graphene is as two-dimensional material, thickness in monolayer only 0.34nm or so, but area is often larger, and market product is mostly
10~30 μm, this raw material easily blocks in spinning technique.Micro crystal graphite is called amorphous graphite powder, and amorphous graphite powder is black
Lead powder belongs to aphanitic graphite.Mainly contain in Hebei, Inner Mongol, northeast, Hunan, the ground such as Xinjiang.It is repeatedly surveyed through geology department
It visits, existing 2,000,000,000 tons of amorphous graphite of China is world saving first.The micro crystal graphite overwhelming majority is graphitic carbon, and color is just grey, has
Metallic luster, matter is soft, not color hardness 1-2, specific gravity 2-2.24, and chemical property is stablized, and is not influenced by strong acid-base, and objectionable impurities is few,
Iron, sulphur, phosphorus, nitrogen, molybdenum, hydrogen content is low, have the characteristics that high temperature resistant, heat transfer, conduction, lubrication and plasticity be widely used in casting,
Smearing, battery, carbon product, pencil, pigment, refractory material, smelting, carburant, casting covering slag etc..Specification: it is divided into
" WT " --- has iron requirement (being commonly called as " electrical carbon "), " W " --- iron-free to require (being commonly called as " casting ") two major classes, and major product has graphite
Ball, graphite powder, granular graphite, graphite sand, carburant.Its specification have 100 mesh, 200 mesh, 325 mesh, 800 mesh, 1200 mesh, 2000 mesh,
The various models such as 4000 mesh, 5000 mesh, 8000 mesh, 10000 mesh, 12000 mesh, anticorrosive paint is dedicated, rubber is dedicated, lubricating oil is special
With, glass reinforced plastic is dedicated, ink is dedicated, dry cell is dedicated, subtracting property battery is dedicated, slip coating, powder metallurgy is dedicated, aquadag is special
With etc., it can also be applied to textile industry.
In the preparation process of graphene, redox method is commonly used, wherein oxidant not only acts as oxidation
Effect, there are also the effects of intercalation.The compound oxidant that the present invention uses keeps two kinds of effects simultaneous instead of original single-oxidizer
Tool.The means that electrochemistry is combined during following process remove graphene further, obtained thinner thinner
Product is more advantageous to the use of downstream product.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the modified dispersion liquid of graphene for spinning, this method
Micro crystal graphite is prepared as modified graphene dispersion liquid, material particular diameter is small, can use in spinning technique, not influence Cheng Sipin
Matter.
A kind of modified dispersion liquid of graphene for spinning of the present invention is mainly by micro crystal graphite, ethylene glycol, hydrogen fluorine
Acid, phosphoric acid, sodium hydroxide, ethyl alcohol, resin reaction be made, process is as follows: by micro crystal graphite, ethylene glycol in acid-resistant container into
Row is blended, and hydrofluoric acid and phosphoric acid are compounded, and is added in above-mentioned slurry and carries out ultrasound, and sodium hydroxide is added after a period of time
Mixed slurry is made in ultrasound.It is used as stoste 1 spare after the slurry is carried out forward and reverse energization.Resin and ethyl alcohol are blended,
It is warming up to 60 DEG C of obtained stostes 2.Stoste 1 and stoste 2 are distinguished into ultrasonic atomizatio, leads in reaction kettle and is reacted, collects reaction
Liquid afterwards, as graphene are modified dispersion liquid.
The preparation method of the modified dispersion liquid of a kind of graphene for spinning, it is characterised in that micro crystal graphite makes
Dosage is 1~5g.
A kind of preparation method of the modified dispersion liquid of graphene for spinning, it is characterised in that the use of ethylene glycol
Amount is 80~100g.
A kind of preparation method of the modified dispersion liquid of graphene for spinning, it is characterised in that the use of hydrofluoric acid
Amount is 5~10g.
A kind of preparation method of the modified dispersion liquid of graphene for spinning, it is characterised in that the usage amount of phosphoric acid
For 5~10g.
The preparation method of the modified dispersion liquid of a kind of graphene for spinning, it is characterised in that sodium hydroxide makes
Dosage is 10~20g.
A kind of preparation method of the modified dispersion liquid of graphene for spinning, it is characterised in that the usage amount of ethyl alcohol
100~150g.
The preparation method of the modified dispersion liquid of described a kind of graphene for spinning, it is characterised in that resin used is
One of polyimides, polystyrene, polyvinyl chloride are a variety of, and usage amount is 2~8g.
A kind of preparation method of the modified dispersion liquid of described graphene for spinning, it is characterised in that by micro crystal graphite,
Ethylene glycol is blended in acid-resistant container, and hydrofluoric acid and phosphoric acid are compounded, and is added in above-mentioned slurry and is carried out ultrasound 30
~60 minutes, 30~60 minutes obtained mixed slurries of sodium hydroxide ultrasound are added, which is applied forward voltage 1~3 minute
Apply again afterwards backward voltage 1~3 minute, obtains stoste 1 after so recycling 10~50 times.Resin is taken to be added in ethyl alcohol, stirring is simultaneously
60 DEG C are warming up to, stoste 2 is obtained.Two kinds of stostes are passed through into ultrasonic atomizatio respectively, and is passed through in reaction kettle and is reacted, generation
Liquid is the modified dispersion liquid of graphene.
The present invention uses compound oxidant instead of the single-oxidizer of original system, while playing oxidation and intercalation two
Kind effect, is more advantageous to the removing of graphene.And the means in subsequent machining technology with electrochemistry combine, and can prepare more
Thin smaller graphene product.It is final to be combined using atomization reaction with resin, graphene dispersing solution can be made more uniform and
There is preferable combination with polyester.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph of the modified dispersion liquid of graphene in embodiment 2
Specific embodiment
The present invention is described in detail below by specific example, but protection scope of the present invention is not only restricted to these
Examples of implementation.
Embodiment 1: taking 1g micro crystal graphite, and blended under agitation in 80g ethylene glycol is added, and takes 5g hydrofluoric acid and 5g phosphoric acid to be blended multiple
Match, nitration mixture is added in micro crystal graphite blended liquid, be stirred by ultrasonic 30 minutes, 10g sodium hydroxide is added, is stirred by ultrasonic 30 minutes.
Apply backward voltage again 1 minute after applying forward voltage 1 minute to the slurry, so recycles 10 times and obtain stoste 1.Take polyamides sub-
Polyimide resin 2g is added in 100g ethyl alcohol, and stirring is warming up to 60 DEG C and is used as stoste 2.Two kinds of stostes are passed through into ultrasonic atomizatio respectively, and
It is passed through in reaction kettle and is reacted, the liquid of generation is the modified dispersion liquid of graphene.
Embodiment 2: taking 5g micro crystal graphite, and blended under agitation in 100g ethylene glycol is added, and takes 10g hydrofluoric acid and 10g phosphoric acid total
Mixed compounding, nitration mixture is added in micro crystal graphite blended liquid, is stirred by ultrasonic 60 minutes, and 20g sodium hydroxide is added, and is stirred by ultrasonic 60 points
Clock.Apply backward voltage again 3 minutes after applying forward voltage 3 minutes to the slurry, so recycles 50 times and obtain stoste 1.It takes poly-
Styrene resin 8g is added in 150g ethyl alcohol, and stirring is warming up to 60 DEG C and is used as stoste 2.Two kinds of stostes are passed through into ultrasonic mist respectively
Change, and be passed through in reaction kettle and reacted, the liquid of generation is the modified dispersion liquid of graphene.
Embodiment 3: taking 3g micro crystal graphite, and blended under agitation in 90g ethylene glycol is added, and takes 8g hydrofluoric acid and 8g phosphoric acid to be blended multiple
Match, nitration mixture is added in micro crystal graphite blended liquid, be stirred by ultrasonic 45 minutes, 15g sodium hydroxide is added, is stirred by ultrasonic 45 minutes.
Apply backward voltage again 2 minutes after applying forward voltage 2 minutes to the slurry, so recycles 30 times and obtain stoste 1.Take polychlorostyrene second
Olefine resin 2g is added in 125g ethyl alcohol, and stirring is warming up to 60 DEG C and is used as stoste 2.Two kinds of stostes are passed through into ultrasonic atomizatio respectively, and
It is passed through in reaction kettle and is reacted, the liquid of generation is the modified dispersion liquid of graphene.
Embodiment 4: terephthalic acid (TPA), catalyst is added in the modified dispersion liquid of graphene in Example 1, be esterified,
Graphene polyester master particle can be obtained in polycondensation, pelletizing.The master batch is mixed, melt spinning with blank polyester slice, be can be obtained
Graphene modified polyester fiber.
The mechanical strength of graphene fiber in 1 embodiment 4 of table
Claims (9)
1. a kind of preparation method of the modified dispersion liquid of graphene for spinning.The dispersion liquid is mainly by micro crystal graphite, second
Glycol, hydrofluoric acid, phosphoric acid, sodium hydroxide, ethyl alcohol, resin reaction are made, and process is as follows: by micro crystal graphite, ethylene glycol resistance to
It is blended in sour container, hydrofluoric acid and phosphoric acid is compounded, and be added in above-mentioned slurry and carry out ultrasound, added after a period of time
Enter sodium hydroxide ultrasound, mixed slurry is made.It is used as stoste 1 spare after the slurry is carried out forward and reverse energization.By resin and second
Alcohol is blended, and 60 DEG C of obtained stostes 2 are warming up to.Stoste 1 and stoste 2 are distinguished into ultrasonic atomizatio, leads in reaction kettle and carries out instead
It answers, the modified dispersion liquid of the liquid after collecting reaction, as graphene.
2. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
The usage amount of micro crystal graphite is 1~5g.
3. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
The usage amount of ethylene glycol is 80~100g.
4. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
The usage amount of hydrofluoric acid is 5~10g.
5. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
The usage amount of phosphoric acid is 5~10g.
6. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
The usage amount of sodium hydroxide is 10~20g.
7. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
100~150g of usage amount of ethyl alcohol.
8. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
Resin used is one of polyimides, polystyrene, polyvinyl chloride or a variety of, and usage amount is 2~8g.
9. a kind of preparation method of the modified dispersion liquid of graphene for spinning according to claim 1, it is characterised in that
Micro crystal graphite, ethylene glycol are blended in acid-resistant container, hydrofluoric acid and phosphoric acid are compounded, and is added in above-mentioned slurry
It carries out ultrasound 30~60 minutes, 30~60 minutes obtained mixed slurries of sodium hydroxide ultrasound is added, positive electricity is applied to the slurry
Pressure applied backward voltage 1~3 minute after 1~3 minute again, obtained stoste 1 after so recycling 10~50 times.Take resin that ethyl alcohol is added
In, it stirs and is warming up to 60 DEG C, obtain stoste 2.Two kinds of stostes are passed through into ultrasonic atomizatio respectively, and is passed through in reaction kettle and carries out instead
It answers, the liquid of generation is the modified dispersion liquid of graphene.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334807A (en) * | 2023-04-04 | 2023-06-27 | 德清申力索具有限公司 | Preparation method of high-strength polyester fiber lifting belt |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130272950A1 (en) * | 2012-04-16 | 2013-10-17 | Electronics And Telecommunications Research Institute | Method of manufacturing a graphene fiber |
| US20140061059A1 (en) * | 2011-03-10 | 2014-03-06 | The University Of Manchester | Production of graphene |
| WO2014032378A1 (en) * | 2012-08-25 | 2014-03-06 | 华南理工大学 | Methods for preparing functionalized graphene and the composite electroconductive glue thereof |
| CN105776187A (en) * | 2016-01-27 | 2016-07-20 | 复旦大学 | Method for green environmental-protection preparation of high-concentration ultra-clean graphene dispersion liquid |
-
2018
- 2018-11-12 CN CN201811371734.5A patent/CN109505022A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140061059A1 (en) * | 2011-03-10 | 2014-03-06 | The University Of Manchester | Production of graphene |
| US20130272950A1 (en) * | 2012-04-16 | 2013-10-17 | Electronics And Telecommunications Research Institute | Method of manufacturing a graphene fiber |
| WO2014032378A1 (en) * | 2012-08-25 | 2014-03-06 | 华南理工大学 | Methods for preparing functionalized graphene and the composite electroconductive glue thereof |
| CN105776187A (en) * | 2016-01-27 | 2016-07-20 | 复旦大学 | Method for green environmental-protection preparation of high-concentration ultra-clean graphene dispersion liquid |
Non-Patent Citations (3)
| Title |
|---|
| 强亮生等编著: "《新型功能材料制备技术与分析表征方法》", 30 June 2017, 哈尔滨工业大学出版社 * |
| 李垚等编著: "《新型功能材料制备原理与工艺》", 31 August 2017, 哈尔滨工业大学出版社 * |
| 李银峰等著: "《碳纳米材料制备及其应用研究》", 31 March 2019, 中国原子能出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334807A (en) * | 2023-04-04 | 2023-06-27 | 德清申力索具有限公司 | Preparation method of high-strength polyester fiber lifting belt |
| CN116334807B (en) * | 2023-04-04 | 2023-12-12 | 德清申力索具有限公司 | Preparation method of high-strength polyester fiber lifting belt |
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