CN111349186A - In-situ polymerization modified graphene polypropylene master batch and preparation method thereof - Google Patents
In-situ polymerization modified graphene polypropylene master batch and preparation method thereof Download PDFInfo
- Publication number
- CN111349186A CN111349186A CN202010332421.XA CN202010332421A CN111349186A CN 111349186 A CN111349186 A CN 111349186A CN 202010332421 A CN202010332421 A CN 202010332421A CN 111349186 A CN111349186 A CN 111349186A
- Authority
- CN
- China
- Prior art keywords
- modified graphene
- graphene oxide
- master batch
- polypropylene master
- situ polymerization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
- C08F110/06—Propene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- 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
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- 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
-
- 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
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
Abstract
The invention discloses an in-situ polymerization modified graphene polypropylene master batch and a preparation method thereof, wherein the master batch comprises the following raw materials in percentage by mass: 90-95% of propylene monomer, 0.1-9% of graphene oxide, 0.1-5% of modifier and 0.1-1% of catalyst. The invention also provides a preparation method of the fiber, which comprises the following steps: step 1, weighing raw materials in proportion; step 2, preparing modified graphene oxide slurry; step 3, preparing modified graphene oxide powder; step 4, preparing a propylene/modified graphene oxide mixed material; and 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction. According to the in-situ polymerization modified graphene polypropylene master batch and the preparation method thereof, the prepared composite master batch has the characteristics of antibiosis, far infrared and ultraviolet resistance, and graphene in the in-situ polymerization modified graphene polypropylene master batch is uniformly dispersed and is not easy to fall off, and the functionality has durability.
Description
Technical Field
The invention relates to a graphene polypropylene master batch and a preparation method thereof, and particularly relates to an in-situ polymerization modified graphene polypropylene master batch and a preparation method thereof.
Background
Graphene is a two-dimensional material with carbon atoms arranged in a hexagon, and graphene oxide has a carboxyl group, an epoxy group, a hydroxyl group and other group-containing modifications on the surface layer of graphene. The graphene oxide is simple in preparation process and low in raw material cost, and meanwhile, the graphene oxide is less prone to agglomeration compared with graphene in actual operation, so that the graphene oxide can be widely applied to large-scale industrial production.
The polypropylene master batch is a chemical master batch with low cost, good performance and extremely wide application, but the traditional polypropylene master batch does not have functionality, along with social development, the traditional polypropylene cannot meet the requirements of people on functional textiles, the graphene polypropylene master batch has good antibacterial property, far infrared, ultraviolet resistance and other functions, the original polymerized graphene polypropylene functionality is permanent, the condition that the functionality is weakened along with the increase of washing times is avoided, the application range of the traditional polypropylene is expanded, the added value of products is improved, and the requirements of people on healthy and environment-friendly functional textiles are well met.
Disclosure of Invention
The invention aims to provide a graphene polypropylene master batch and a preparation method thereof, and the modified graphene polypropylene master batch with the functions of antibiosis, mite prevention, ultraviolet resistance, far infrared and the like is prepared, so that the additional value of polypropylene is improved, and the application range of the polypropylene master batch is expanded.
In order to achieve the purpose, the invention provides an in-situ polymerization modified graphene polypropylene master batch, wherein the master batch comprises the following raw materials in percentage by mass: 90-95% of propylene monomer, 0.1-9% of graphene oxide, 0.1-5% of modifier and 0.1-1% of catalyst.
The in-situ polymerization modified graphene polypropylene master batch comprises one or more of polyvinyl alcohol, hydroxypropyl cellulose, polyethylene glycol, sodium lignosulfonate, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, cetyl trimethyl ammonium bromide, sodium deoxycholate, aminosiloxane, octadecylamine and silane coupling agents.
The in-situ polymerization modified graphene polypropylene master batch comprises a metallocene catalyst or a Z-N catalyst.
The in-situ polymerization modified graphene polypropylene master batch is prepared from graphene oxide by any one of a mechanical stripping method, a chemical vapor deposition method and an oxidation-reduction method.
The invention also provides a preparation method of the in-situ polymerization modified graphene polypropylene master batch, wherein the method comprises the following steps: step 1, weighing raw materials in proportion; step 2, preparing modified graphene oxide slurry; step 3, preparing modified graphene oxide powder; step 4, preparing a propylene/modified graphene oxide mixed material; and 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
In the step 2, the graphene oxide powder and the modifier are added into deionized water, stirred for 0.5-1 h, heated to 50-80 ℃, and subjected to ultrasonic dispersion treatment for 10-20 min to prepare the modified graphene oxide slurry.
The preparation method of the in-situ polymerization modified graphene polypropylene master batch comprises the step of preparing modified graphene oxide slurry, wherein the concentration of graphene oxide in the modified graphene oxide slurry is 1-5 mg/ml.
In the step 3, the obtained modified graphene oxide slurry is freeze-dried to obtain modified graphene oxide powder, and the obtained powder is sent into a container to be sealed and vacuumized, and then is filled with nitrogen to protect for later use.
In the step 4, the prepared modified graphene oxide powder is taken, the powdered propylene monomer is added in proportion, and the mixture is uniformly stirred.
In the step 5, the mixed propylene/modified graphene oxide material is placed into a polymerization kettle, a catalyst is added, the mixture is heated to 50-60 ℃, stirred for 10-20 min, the temperature is raised to 70-90 ℃, the polymerization reaction is carried out for 3-5 h, and the material is discharged, granulated and dried to obtain the in-situ polymerized graphene polypropylene master batch.
The in-situ polymerization modified graphene polypropylene master batch and the preparation method thereof provided by the invention have the following advantages:
the graphene oxide powder prepared by the formula is subjected to compound copolymerization with propylene to prepare the graphene polypropylene master batch. The graphene in the in-situ polymerization modified graphene polypropylene master batch is uniformly dispersed, is not easy to fall off, and has durability in functionality.
The in-situ polymerized graphene polypropylene master batch disclosed by the invention has excellent performances of antibiosis, mite prevention, far infrared, ultraviolet resistance and the like, wherein the bacteriostasis rate of escherichia coli, staphylococcus aureus and candida albicans reaches 99.9%, the mite inhibition rate is more than 90%, the far infrared temperature rise reaches 0.88, the UPF is more than 100, and the functionality is good.
The in-situ polymerized graphene polypropylene master batch prepared by the method has the advantages of simple process, easy operation, low cost and high economic benefit, and is suitable for large-scale industrial production.
Detailed Description
The following further describes embodiments of the present invention.
The in-situ polymerization modified graphene polypropylene master batch provided by the invention comprises the following raw materials in percentage by mass: 90-95% of propylene monomer, 0.1-9% of graphene oxide, 0.1-5% of modifier and 0.1-1% of catalyst.
Preferably, the modifier comprises any one or more of polyvinyl alcohol, hydroxypropyl cellulose, polyethylene glycol, sodium lignosulfonate, polyvinyl pyrrolidone (PVP), sodium dodecylbenzenesulfonate, sodium lauryl sulfate, cetyltrimethylammonium bromide, sodium deoxycholate, aminosilicone, octadecylamine, silane coupling agents, and the like.
The catalyst includes any one of a metallocene catalyst, a Z-N catalyst, and the like.
The graphene oxide is prepared by any one of a mechanical exfoliation method, a chemical vapor deposition method, a redox method, and the like.
The invention also provides a preparation method of the in-situ polymerization modified graphene polypropylene master batch, which comprises the following steps: step 1, weighing raw materials in proportion; step 2, preparing modified graphene oxide slurry; step 3, preparing modified graphene oxide powder; step 4, preparing a propylene/modified graphene oxide mixed material; and 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
Preferably, in the step 2, the graphene oxide powder and the modifier are added into deionized water, stirred for 0.5-1 h, and subjected to ultrasonic dispersion treatment for 10-20 min after the temperature is raised to 50-80 ℃ to prepare the modified graphene oxide slurry.
The concentration of the graphene oxide in the modified graphene oxide slurry is 1-5 mg/ml.
And 3, freeze-drying the obtained modified graphene oxide slurry to obtain modified graphene oxide powder, conveying the obtained powder into a container, sealing, vacuumizing, and filling nitrogen for protection for later use.
And 4, taking the prepared modified graphene oxide powder, adding the powdered propylene monomer according to a proportion, and uniformly stirring.
And 5, putting the mixed propylene/modified graphene oxide material into a polymerization kettle, adding a catalyst, heating to 50-60 ℃, stirring for 10-20 min, raising the temperature to 70-90 ℃, carrying out polymerization reaction for 3-5 h, discharging, granulating and drying to obtain the in-situ polymerized graphene polypropylene master batch.
The in-situ polymerization modified graphene polypropylene masterbatch and the preparation method thereof provided by the invention are further described below with reference to the examples.
Example 1
The in-situ polymerization modified graphene polypropylene master batch comprises the following raw materials in percentage by mass: 95% of propylene monomer, 0.1% of graphene oxide, 3.9% of modifier and 1% of catalyst.
Preferably, the modifying agent comprises polyvinyl alcohol or hydroxypropyl cellulose.
The catalyst comprises a metallocene catalyst.
The graphene oxide is prepared by a mechanical stripping method.
The embodiment also provides a preparation method of the in-situ polymerization modified graphene polypropylene master batch, which comprises the following steps:
step 1, weighing the raw materials in proportion.
And 2, preparing the modified graphene oxide slurry.
Adding the graphene oxide powder and the modifier into deionized water, stirring for 0.5-1 h, heating to 50-80 ℃, and performing ultrasonic dispersion treatment for 10-20 min to prepare modified graphene oxide slurry. The concentration of graphene oxide in the modified graphene oxide slurry is 1 mg/ml.
And 3, preparing modified graphene oxide powder.
And freeze-drying the obtained modified graphene oxide slurry to obtain modified graphene oxide powder, conveying the obtained powder into a container, sealing, vacuumizing, and then filling nitrogen for protection for later use.
And 4, preparing the propylene/modified graphene oxide mixed material.
And adding the prepared modified graphene oxide powder into the powdered propylene monomer according to a proportion, and uniformly stirring.
And 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
Putting the mixed propylene/modified graphene oxide material into a polymerization kettle, adding a catalyst, heating to 50-60 ℃, stirring for 10-20 min, raising the temperature to 70-90 ℃, carrying out polymerization reaction for 3-5 h, discharging, granulating and drying to obtain the in-situ polymerized graphene polypropylene master batch.
Example 2
The in-situ polymerization modified graphene polypropylene master batch comprises the following raw materials in percentage by mass: 91.8% of propylene monomer, 3% of graphene oxide, 5% of modifier and 0.2% of catalyst.
Preferably, the modifying agent comprises polyethylene glycol and sodium lignosulfonate.
The catalyst comprises a Z-N catalyst.
The graphene oxide is prepared by a chemical vapor deposition method.
The embodiment also provides a preparation method of the in-situ polymerization modified graphene polypropylene master batch, which comprises the following steps:
step 1, weighing the raw materials in proportion.
And 2, preparing the modified graphene oxide slurry.
Adding the graphene oxide powder and the modifier into deionized water, stirring for 0.5-1 h, heating to 50-80 ℃, and performing ultrasonic dispersion treatment for 10-20 min to prepare modified graphene oxide slurry. The concentration of graphene oxide in the modified graphene oxide slurry was 2 mg/ml.
And 3, preparing modified graphene oxide powder.
And freeze-drying the obtained modified graphene oxide slurry to obtain modified graphene oxide powder, conveying the obtained powder into a container, sealing, vacuumizing, and then filling nitrogen for protection for later use.
And 4, preparing the propylene/modified graphene oxide mixed material.
And adding the prepared modified graphene oxide powder into the powdered propylene monomer according to a proportion, and uniformly stirring.
And 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
Putting the mixed propylene/modified graphene oxide material into a polymerization kettle, adding a catalyst, heating to 50-60 ℃, stirring for 10-20 min, raising the temperature to 70-90 ℃, carrying out polymerization reaction for 3-5 h, discharging, granulating and drying to obtain the in-situ polymerized graphene polypropylene master batch.
Example 3
The in-situ polymerization modified graphene polypropylene master batch comprises the following raw materials in percentage by mass: 94.1% of propylene monomer, 5% of graphene oxide, 0.1% of modifier and 0.8% of catalyst.
Preferably, the modifier comprises polyvinylpyrrolidone.
The catalyst comprises a metallocene catalyst.
The graphene oxide is prepared by a redox method.
The embodiment also provides a preparation method of the in-situ polymerization modified graphene polypropylene master batch, which comprises the following steps:
step 1, weighing the raw materials in proportion.
And 2, preparing the modified graphene oxide slurry.
Adding the graphene oxide powder and the modifier into deionized water, stirring for 0.5-1 h, heating to 50-80 ℃, and performing ultrasonic dispersion treatment for 10-20 min to prepare modified graphene oxide slurry. The concentration of graphene oxide in the modified graphene oxide slurry was 3 mg/ml.
And 3, preparing modified graphene oxide powder.
And freeze-drying the obtained modified graphene oxide slurry to obtain modified graphene oxide powder, conveying the obtained powder into a container, sealing, vacuumizing, and then filling nitrogen for protection for later use.
And 4, preparing the propylene/modified graphene oxide mixed material.
And adding the prepared modified graphene oxide powder into the powdered propylene monomer according to a proportion, and uniformly stirring.
And 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
Putting the mixed propylene/modified graphene oxide material into a polymerization kettle, adding a catalyst, heating to 50-60 ℃, stirring for 10-20 min, raising the temperature to 70-90 ℃, carrying out polymerization reaction for 3-5 h, discharging, granulating and drying to obtain the in-situ polymerized graphene polypropylene master batch.
Example 4
The in-situ polymerization modified graphene polypropylene master batch comprises the following raw materials in percentage by mass: 91% of propylene monomer, 7% of graphene oxide, 1.5% of modifier and 0.5% of catalyst.
Preferably, the modifier comprises sodium dodecylbenzene sulfonate, sodium dodecyl sulfate.
The catalyst comprises a Z-N catalyst.
The graphene oxide is prepared by a mechanical stripping method or a chemical vapor deposition method.
The embodiment also provides a preparation method of the in-situ polymerization modified graphene polypropylene master batch, which comprises the following steps:
step 1, weighing the raw materials in proportion.
And 2, preparing the modified graphene oxide slurry.
Adding the graphene oxide powder and the modifier into deionized water, stirring for 0.5-1 h, heating to 50-80 ℃, and performing ultrasonic dispersion treatment for 10-20 min to prepare modified graphene oxide slurry. The concentration of graphene oxide in the modified graphene oxide slurry was 4 mg/ml.
And 3, preparing modified graphene oxide powder.
And freeze-drying the obtained modified graphene oxide slurry to obtain modified graphene oxide powder, conveying the obtained powder into a container, sealing, vacuumizing, and then filling nitrogen for protection for later use.
And 4, preparing the propylene/modified graphene oxide mixed material.
And adding the prepared modified graphene oxide powder into the powdered propylene monomer according to a proportion, and uniformly stirring.
And 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
Putting the mixed propylene/modified graphene oxide material into a polymerization kettle, adding a catalyst, heating to 50-60 ℃, stirring for 10-20 min, raising the temperature to 70-90 ℃, carrying out polymerization reaction for 3-5 h, discharging, granulating and drying to obtain the in-situ polymerized graphene polypropylene master batch.
Example 5
The in-situ polymerization modified graphene polypropylene master batch comprises the following raw materials in percentage by mass: 90% of propylene monomer, 9% of graphene oxide, 0.9% of modifier and 0.1% of catalyst.
Preferably, the modifier comprises any one or more of cetyltrimethylammonium bromide, sodium deoxycholate, aminosilicone, octadecylamine, silane coupling agents, and the like.
The catalyst includes any one of a metallocene catalyst, a Z-N catalyst, and the like.
The graphene oxide is prepared by any one of a mechanical exfoliation method, a chemical vapor deposition method, a redox method, and the like.
The embodiment also provides a preparation method of the in-situ polymerization modified graphene polypropylene master batch, which comprises the following steps:
step 1, weighing the raw materials in proportion.
And 2, preparing the modified graphene oxide slurry.
Adding the graphene oxide powder and the modifier into deionized water, stirring for 0.5-1 h, heating to 50-80 ℃, and performing ultrasonic dispersion treatment for 10-20 min to prepare modified graphene oxide slurry. The concentration of graphene oxide in the modified graphene oxide slurry was 5 mg/ml.
And 3, preparing modified graphene oxide powder.
And freeze-drying the obtained modified graphene oxide slurry to obtain modified graphene oxide powder, conveying the obtained powder into a container, sealing, vacuumizing, and then filling nitrogen for protection for later use.
And 4, preparing the propylene/modified graphene oxide mixed material.
And adding the prepared modified graphene oxide powder into the powdered propylene monomer according to a proportion, and uniformly stirring.
And 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
Putting the mixed propylene/modified graphene oxide material into a polymerization kettle, adding a catalyst, heating to 50-60 ℃, stirring for 10-20 min, raising the temperature to 70-90 ℃, carrying out polymerization reaction for 3-5 h, discharging, granulating and drying to obtain the in-situ polymerized graphene polypropylene master batch.
The in-situ polymerization modified graphene polypropylene master batch and the preparation method thereof are characterized in that the modified graphene oxide powder is prepared by using graphene oxide, then the modified graphene oxide powder is subjected to composite copolymerization with propylene, then the obtained product is placed into a reaction kettle for reaction, and finally the obtained product is discharged and granulated. The graphene-polypropylene master batch is prepared by utilizing a modified graphene oxide solution preparation and dispersion system and a polypropylene in-situ polymerization technology, the composite master batch has the characteristics of antibiosis, far infrared and ultraviolet resistance, graphene in the in-situ polymerization modified graphene-polypropylene master batch is uniformly dispersed and is not easy to fall off, and the functionality has durability.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (10)
1. The in-situ polymerization modified graphene polypropylene master batch is characterized by comprising the following raw materials in percentage by mass: 90-95% of propylene monomer, 0.1-9% of graphene oxide, 0.1-5% of modifier and 0.1-1% of catalyst.
2. The in-situ polymerization modified graphene polypropylene master batch of claim 1, wherein the modifier comprises any one or more of polyvinyl alcohol, hydroxypropyl cellulose, polyethylene glycol, sodium lignosulfonate, polyvinylpyrrolidone, sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, cetyltrimethylammonium bromide, sodium deoxycholate, aminosilicone, octadecylamine and silane coupling agent.
3. The in-situ polymerization modified graphene polypropylene masterbatch according to claim 1, wherein the catalyst comprises any one of a metallocene catalyst or a Z-N catalyst.
4. The in-situ polymerization modified graphene polypropylene master batch according to claim 1, wherein the graphene oxide is prepared by any one of a mechanical stripping method, a chemical vapor deposition method and a redox method.
5. The preparation method of the in-situ polymerization modified graphene polypropylene master batch as claimed in any one of claims 1 to 4, wherein the method comprises the following steps:
step 1, weighing raw materials in proportion;
step 2, preparing modified graphene oxide slurry;
step 3, preparing modified graphene oxide powder;
step 4, preparing a propylene/modified graphene oxide mixed material;
and 5, obtaining the in-situ polymerized graphene polypropylene master batch through polymerization reaction.
6. The preparation method of the in-situ polymerization modified graphene polypropylene master batch as claimed in claim 5, wherein in the step 2, the graphene oxide powder and the modifier are added into deionized water, the mixture is stirred for 0.5 to 1 hour, the temperature is increased to 50 to 80 ℃, and then ultrasonic dispersion treatment is carried out for 10 to 20min to prepare the modified graphene oxide slurry.
7. The preparation method of the in-situ polymerization modified graphene polypropylene master batch according to claim 6, wherein the concentration of graphene oxide in the modified graphene oxide slurry is 1-5 mg/ml.
8. The method for preparing in-situ polymerization modified graphene polypropylene master batch according to claim 5, wherein in the step 3, the obtained modified graphene oxide slurry is freeze-dried to obtain modified graphene oxide powder, the obtained powder is sent into a container to be sealed, vacuumized and then filled with nitrogen for protection for later use.
9. The method for preparing in-situ polymerization modified graphene polypropylene masterbatch according to claim 5, wherein in the step 4, the prepared modified graphene oxide powder is taken, the powdered propylene monomer is added according to a proportion, and the mixture is uniformly stirred.
10. The preparation method of the in-situ polymerization modified graphene polypropylene master batch as claimed in claim 5, wherein in the step 5, the mixed propylene/modified graphene oxide material is placed into a polymerization kettle, a catalyst is added, the mixture is heated to 50-60 ℃, stirred for 10-20 min, then the temperature is raised to 70-90 ℃, the polymerization reaction is carried out for 3-5 h, and the material is discharged, granulated and dried to obtain the in-situ polymerization graphene polypropylene master batch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010332421.XA CN111349186A (en) | 2020-04-24 | 2020-04-24 | In-situ polymerization modified graphene polypropylene master batch and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010332421.XA CN111349186A (en) | 2020-04-24 | 2020-04-24 | In-situ polymerization modified graphene polypropylene master batch and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111349186A true CN111349186A (en) | 2020-06-30 |
Family
ID=71191585
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010332421.XA Pending CN111349186A (en) | 2020-04-24 | 2020-04-24 | In-situ polymerization modified graphene polypropylene master batch and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111349186A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113174068A (en) * | 2021-04-26 | 2021-07-27 | 高碑店市隆泰丰博石墨烯有限公司 | Graphene-based functional master batch capable of absorbing moisture, releasing sweat and dissipating heat quickly and preparation method thereof |
| CN113235223A (en) * | 2021-03-12 | 2021-08-10 | 大连德力石墨烯材料有限公司 | Graphene modified melt-blown fabric and preparation method and application thereof |
| CN113715421A (en) * | 2021-10-12 | 2021-11-30 | 广州康滤净化科技有限公司 | Virus-killing aggregate, H12-grade melt-blown fabric and graphene non-woven fabric bonding material and preparation method thereof |
| CN113733694A (en) * | 2021-10-12 | 2021-12-03 | 广州康滤净化科技有限公司 | Virus-killing aggregate, H13-grade melt-blown fabric and graphene non-woven fabric bonding material and preparation method thereof |
| CN114575038A (en) * | 2022-03-11 | 2022-06-03 | 湖北瑞康医用耗材有限公司 | Preparation method of graphene non-woven fabric with microorganism inactivation performance |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108048936A (en) * | 2017-12-30 | 2018-05-18 | 杭州高烯科技有限公司 | A kind of preparation method of high-performance PP fibers |
| CN109731413A (en) * | 2019-02-22 | 2019-05-10 | 常州兴烯石墨烯科技有限公司 | A kind of functionality graphene airstrainer and preparation method thereof |
| CN109944080A (en) * | 2019-03-31 | 2019-06-28 | 任国峰 | A kind of anti-puncture fabric of graphene and preparation method thereof |
| CN110205706A (en) * | 2019-07-05 | 2019-09-06 | 常州兴烯石墨烯科技有限公司 | A kind of modified white graphite alkene polyamide fibre composite fibre and preparation method thereof |
| CN110205702A (en) * | 2019-07-05 | 2019-09-06 | 常州兴烯石墨烯科技有限公司 | A kind of modified white graphite alkene terylene composite fibre and preparation method thereof |
-
2020
- 2020-04-24 CN CN202010332421.XA patent/CN111349186A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108048936A (en) * | 2017-12-30 | 2018-05-18 | 杭州高烯科技有限公司 | A kind of preparation method of high-performance PP fibers |
| CN109731413A (en) * | 2019-02-22 | 2019-05-10 | 常州兴烯石墨烯科技有限公司 | A kind of functionality graphene airstrainer and preparation method thereof |
| CN109944080A (en) * | 2019-03-31 | 2019-06-28 | 任国峰 | A kind of anti-puncture fabric of graphene and preparation method thereof |
| CN110205706A (en) * | 2019-07-05 | 2019-09-06 | 常州兴烯石墨烯科技有限公司 | A kind of modified white graphite alkene polyamide fibre composite fibre and preparation method thereof |
| CN110205702A (en) * | 2019-07-05 | 2019-09-06 | 常州兴烯石墨烯科技有限公司 | A kind of modified white graphite alkene terylene composite fibre and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113235223A (en) * | 2021-03-12 | 2021-08-10 | 大连德力石墨烯材料有限公司 | Graphene modified melt-blown fabric and preparation method and application thereof |
| CN113174068A (en) * | 2021-04-26 | 2021-07-27 | 高碑店市隆泰丰博石墨烯有限公司 | Graphene-based functional master batch capable of absorbing moisture, releasing sweat and dissipating heat quickly and preparation method thereof |
| CN113174068B (en) * | 2021-04-26 | 2023-10-13 | 高碑店市隆泰丰博石墨烯有限公司 | Graphene-based moisture-absorbing sweat-releasing functional master batch capable of rapidly dissipating heat and preparation method thereof |
| CN113715421A (en) * | 2021-10-12 | 2021-11-30 | 广州康滤净化科技有限公司 | Virus-killing aggregate, H12-grade melt-blown fabric and graphene non-woven fabric bonding material and preparation method thereof |
| CN113733694A (en) * | 2021-10-12 | 2021-12-03 | 广州康滤净化科技有限公司 | Virus-killing aggregate, H13-grade melt-blown fabric and graphene non-woven fabric bonding material and preparation method thereof |
| CN114575038A (en) * | 2022-03-11 | 2022-06-03 | 湖北瑞康医用耗材有限公司 | Preparation method of graphene non-woven fabric with microorganism inactivation performance |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111349186A (en) | In-situ polymerization modified graphene polypropylene master batch and preparation method thereof | |
| CN111235671A (en) | Modified graphene anti-ultraviolet polyamide fiber and preparation method thereof | |
| CN102976660A (en) | Disposable disperse re-dispersible emulsion powder | |
| CN114149295B (en) | Coated molecular perovskite energetic material and preparation method thereof | |
| CN109485771A (en) | A kind of preparation method of crospovidone | |
| CN108102150B (en) | Method for constructing polyelectrolyte composite material based on chitosan | |
| CN101319060B (en) | Method for preparing dry heat denatured rice starch | |
| CN109880169B (en) | In-situ polymerization modified white graphene nylon composite slice and preparation method thereof | |
| CN108014754A (en) | A kind of preparation method of sulfhydryl modified active bentonite molecular sieve | |
| WO2017020237A1 (en) | Triple-response type starch-based microgel and preparation method therefor | |
| CN111636112A (en) | Graphene composite antibacterial and antiviral polypropylene filament and preparation method thereof | |
| CN105001493A (en) | Low-density polyethylene degradable mulching film which is modified by carrying cross-linked starch through nanometer sepiolite and is capable of adsorbing heavy metal and preparing method of low-density polyethylene degradable mulching film | |
| CN108976446A (en) | The preparation method of powder styrene butadiene rubber | |
| CN103865469A (en) | Method for preparing montmorillonite modified alcohol-soluble polyurethane (PU) adhesive | |
| KR101818650B1 (en) | Organic-inorganic composite particle material having water repellent and antibiotic, and preparation method thereof | |
| CN106800616A (en) | A kind of preparation method of high bulk density PVPP | |
| CN103130935A (en) | Simple method for preparing monodisperse anionic polystyrene microsphere | |
| JPS6351435A (en) | Manufacture of flowable silicic acid-filled rubber powder | |
| CN115044105A (en) | Silver-loaded mesoporous silica microsphere and preparation method and application thereof | |
| WO2018113496A1 (en) | Pbs resin composition and preparation method therefor | |
| CN108976351A (en) | The preparation method of graft powder butadiene-styrene rubber | |
| CN107082895A (en) | The preparation method of degradable nano antibacterial film | |
| CN107118551A (en) | Based on the pressure-sensitive high polymer material preparation method of bionical selfreparing | |
| CN109160766B (en) | Core-shell structure expanding agent for concrete and preparation method thereof | |
| CN106750745A (en) | One-step silane cross-linked polyethylene material special compounding solution of silane and its application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230721 Address after: 100176 701, Floor 7, Building 42, Yard 1, Jinghai 5th Road, Beijing Economic-Technological Development Area (Tongzhou), Daxing District, Beijing Applicant after: Beijing yingchuanglihe Electronic Technology Co.,Ltd. Address before: 063000 Room 401, 5 / F, deyuanli building, Xuzhuang community, Beixin Xidao, Lubei District, Tangshan City, Hebei Province Applicant before: Ren Guofeng |