CN115011039A - Graphene modified polypropylene resin and preparation method thereof - Google Patents

Graphene modified polypropylene resin and preparation method thereof Download PDF

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Publication number
CN115011039A
CN115011039A CN202210773888.7A CN202210773888A CN115011039A CN 115011039 A CN115011039 A CN 115011039A CN 202210773888 A CN202210773888 A CN 202210773888A CN 115011039 A CN115011039 A CN 115011039A
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Prior art keywords
graphene
polypropylene resin
modified polypropylene
parts
antioxidant
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CN202210773888.7A
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Inventor
修忠海
郝春波
李秉荣
付莹
薛浩
刘忠全
李春晖
肖大君
武天希
王楠
孙洪伟
殷志华
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North Huajin Chemical Industries Co Ltd
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North Huajin Chemical Industries Co Ltd
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Priority to CN202210773888.7A priority Critical patent/CN115011039A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/04—Antistatic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

The invention relates to the field of high polymer materials, and discloses graphene modified polypropylene resin and a preparation method thereof. The polypropylene resin comprises the following components in parts by mass: 75-90 parts of polypropylene powder, 9.5-22 parts of graphene, 0.1-0.5 part of heat stabilizer, 0.1-0.5 part of antioxidant and 0.3-2 parts of compatilizer. The polypropylene resin is obtained by weighing the components, mixing, extruding and granulating. The obtained polypropylene resin has good conductivity, and the impact property and the tensile property are obviously improved.

Description

Graphene modified polypropylene resin and preparation method thereof
Technical Field
The invention relates to the technical field of high polymer materials, and discloses graphene modified polypropylene resin and a preparation method thereof.
Background
With the development of polymer materials, the requirements of people are no longer limited to basic performances such as rigidity, durability and the like, and the polymer materials are also required to have comprehensive properties such as safety, environmental protection, static resistance, conductivity and the like. Research and development of conductive polyolefin is a research topic in the technical field of high polymer materials. The conductive polyolefin is a polyolefin material prepared by methods of surface treatment, filler dispersion compounding, conductive filler lamination compounding and the like, and the product is widely applied to the fields of electronics and electric appliances, explosion-proof product shells and components, semiconductive shielding materials and electromagnetic shielding shells of electronic products, and is particularly widely applied to the field of military industry.
At present, the preparation of polypropylene resin with good conductivity is a difficult problem in engineering technology. The graphene has excellent mechanical property and conductivity, and is a good material for modifying polypropylene. CN108610559B discloses a graphene modified polypropylene composite material and a preparation method thereof, but it requires polypropylene fibers as a graphene adsorption carrier, and has high requirements on the diameter and length of the polypropylene fibers, and the preparation method is not simple and requires much inorganic filler.
Therefore, it is required to develop a graphene-modified polypropylene resin with a simpler production process, which can simplify the preparation procedure and the preparation raw materials, and simultaneously can maintain good conductivity and mechanical properties of the polypropylene resin to meet the market demand.
Disclosure of Invention
The invention has the conception that the graphene has excellent mechanical property and conductivity, and the polypropylene resin with good conductivity, impact resistance and tensile property is prepared by adding the graphene into polypropylene powder, matching with other heat stabilizers, antioxidants and compatilizers and adjusting a proper proportion.
In a first aspect, the present invention provides a graphene-modified polypropylene resin.
The graphene modified polypropylene resin comprises the following components in parts by mass: 75-90 parts of polypropylene powder, 9.5-22 parts of graphene, 0.1-0.5 part of heat stabilizer, 0.1-0.5 part of antioxidant and 0.3-2 parts of compatilizer; the melt flow rate of the polypropylene powder is 6-12 g/10min under the conditions of 230 ℃ and 2.16Kg of load.
Preferably, the heat stabilizer is heat stabilizer 1010.
Preferably, the antioxidant is antioxidant 168.
Preferably, the compatilizer is maleic anhydride grafted polypropylene, and the grafting rate of maleic anhydride is 0.2-5%.
Preferably, the graphene is prepared by the following method: adding 20mL of concentrated sulfuric acid (96 wt%) and 4g P into 1.0g of high-purity graphite at 80 deg.C 2 O 5 And 4g K 2 S 2 O 8 To the prepared mixed solution, magnetic stirring was performed for 4.5 hours, and then 4g of KMnO was slowly added under ice-water bath 4 (ii) a After the solution is cooled to room temperature, slowly adding 80mL of hydrogen peroxide solution (80 wt%), and standing for 24 h; centrifuging the solution after standing, separating out a yellow brown solid, and washing with deionized water for multiple times until the pH value of the supernatant is 7; and (3) carrying out vacuum freeze drying on the yellow brown solid for 24 hours to obtain the graphene.
In a second aspect, the present invention provides a method for preparing a graphene-modified polypropylene resin according to the first aspect, including the following steps:
s1: drying the polypropylene powder in a blast drying oven;
s2: weighing the components in corresponding parts by mass according to any one of claims 1 to 5, and fully stirring and mixing to obtain a mixture;
s3: and extruding and granulating the mixture to obtain the graphene modified polypropylene resin.
Preferably, in the step S1, the moisture content of the polypropylene powder material is dried to less than 100 ppm.
Preferably, in the step S2, a high-speed stirrer is used for mixing for 2-3 min.
Preferably, in the step S3, a twin-screw extruder is used for extrusion granulation, wherein the temperature of the extruder is 180 to 230 ℃, and the screw rotation speed is 350 to 400 r/min.
The invention has the following beneficial effects:
the modification method is simple and convenient, and the obtained material has excellent conductivity and antistatic property, wide application range and excellent toughness and processability.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples.
It should be noted that the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1
Example 1 the raw material composition comprises: 93% of polypropylene powder, 5% of graphene, 10100.2% of heat stabilizer, 1680.3% of antioxidant and 1.5% of maleic anhydride grafted polypropylene.
The preparation method comprises the following steps: (1) drying the polypropylene powder in a blast drying oven at 90 ℃ for 4h to ensure that the water content is less than 100 ppm;
(2) the components are respectively weighed according to the weight percentage, mixed in a high-speed mixer for 2-3 min to obtain a mixture, and then the mixture is extruded and granulated by a double-screw extruder to obtain a target product.
The temperature of the double-screw extruder is controlled to be 180-230 ℃, and the rotating speed of the screw is 350-400 r/min.
The graphene used above is prepared by the following method: adding 20mL of concentrated sulfuric acid (96 wt%) and 4g P into 1.0g of high-purity graphite at 80 deg.C 2 O 5 And 4g K 2 S 2 O 8 To the prepared mixed solution, magnetic stirring was performed for 4.5 hours, and then 4g of KMnO was slowly added under ice-water bath 4 (ii) a After the solution is cooled to room temperature, slowly adding 80mL of hydrogen peroxide solution (80 wt%), and standing for 24 h; centrifuging the solution after standing, separating out a yellow brown solid, and washing with deionized water for multiple times until the pH value of the supernatant is 7; and (3) carrying out vacuum freeze drying on the yellow brown solid for 24 hours to obtain the graphene.
Example 2
Example 2 the raw material composition comprises: 88% of polypropylene powder, 10% of graphene, 10100.2% of heat stabilizer, 1680.2% of antioxidant and 1.6% of maleic anhydride grafted polypropylene. The preparation method of the graphene used was the same as in example 1.
The preparation method comprises the following steps: (1) drying the polypropylene powder in a blast drying oven at 90 ℃ for 4h to ensure that the water content is less than 100 ppm;
(2) the components are respectively weighed according to the weight percentage, mixed in a high-speed mixer for 2-3 min to obtain a mixture, and then the mixture is extruded and granulated by a double-screw extruder to obtain a target product.
The temperature of the double-screw extruder is controlled to be 180-230 ℃, and the rotating speed of the screw is 350-400 r/min.
Example 3
Example 3 the raw material composition comprises: 83% of polypropylene powder, 15% of graphene, 10100.3% of heat stabilizer, 1680.3% of antioxidant and 1.4% of maleic anhydride grafted polypropylene. The preparation method of the graphene used was the same as in example 1.
The preparation method comprises the following steps: (1) drying the polypropylene powder in a blast drying oven at 90 ℃ for 4h to ensure that the water content is less than 100 ppm;
(2) the components are respectively weighed according to the weight percentage, mixed in a high-speed mixer for 2-3 min to obtain a mixture, and then the mixture is extruded and granulated by a double-screw extruder to obtain a target product.
The temperature of the double-screw extruder is controlled to be 180-230 ℃, and the rotating speed of the screw is 350-400 r/min.
Example 4
Example 4 the raw material composition comprises: 78% of polypropylene powder, 20% of graphene, 10100.2% of heat stabilizer, 1680.3% of antioxidant and 1.5% of maleic anhydride grafted polypropylene. The preparation method of the graphene used is the same as in example 1.
The preparation method comprises the following steps: (1) drying the polypropylene powder in a blast drying oven at 90 ℃ for 4h to ensure that the water content is less than 100 ppm;
(2) the components are respectively weighed according to the weight percentage, mixed in a high-speed mixer for 2-3 min to obtain a mixture, and then the mixture is extruded and granulated by a double-screw extruder to obtain a target product.
The temperature of the double-screw extruder is controlled to be 180-230 ℃, and the rotating speed of the screw is 350-400 r/min.
Comparative example
The raw materials of the comparative example comprise: 98% of polypropylene powder, 10100.2% of heat stabilizer, 1680.3% of antioxidant and 1.5% of maleic anhydride grafted polypropylene.
The preparation method comprises the following steps: (1) drying the polypropylene powder in a blast drying oven at 90 ℃ for 4h to ensure that the water content is less than 100 ppm;
(2) the components are respectively weighed according to the weight percentage, mixed in a high-speed mixer for 2-3 min to obtain a mixture, and then the mixture is extruded and granulated by a double-screw extruder to obtain a target product.
The temperature of the double-screw extruder is controlled to be 180-230 ℃, and the rotating speed of the screw is 350-400 r/min.
Effects of the implementation
According to the above examples and comparative examples, GB/T1410-2006 is adopted for measuring the volume resistivity, GB/T1043.1-2008 is adopted for measuring the notch impact performance of the simple beam, and GB/T1040.2-2006 standard is adopted for measuring the tensile performance. The results of the performance tests are shown in Table 1.
Table 1 results of performance testing
Figure BDA0003725691530000051
As can be seen from Table 1, compared with the comparative example, the volume resistivity of the polypropylene resin can be obviously reduced after the polypropylene resin is modified by the graphene, and the volume resistivity can be reduced to 10 when the addition amount of the graphene is 10 percent 5 Omega cm, the impact performance and tensile property of the modified polypropylene resin are also in an increasing trend due to the high rigidity of the graphene material, and the modified polypropylene resin has good processability.

Claims (9)

1. The graphene-modified polypropylene resin is characterized by comprising the following components in parts by mass: 75-90 parts of polypropylene powder, 9.5-22 parts of graphene, 0.1-0.5 part of heat stabilizer, 0.1-0.5 part of antioxidant and 0.3-2 parts of compatilizer; the melt flow rate of the polypropylene powder is 6-12 g/10min under the conditions of 230 ℃ and 2.16Kg of load.
2. The graphene-modified polypropylene resin according to claim 1, wherein the heat stabilizer is 1010.
3. The graphene-modified polypropylene resin according to claim 1, wherein the antioxidant is antioxidant 168.
4. The graphene-modified polypropylene resin according to claim 1, wherein the compatibilizer is maleic anhydride grafted polypropylene, and the maleic anhydride grafting ratio is 0.2 to 5%.
5. The graphene-modified polypropylene resin according to claim 1, wherein the graphene is prepared by a method comprising: adding 20mL of concentrated sulfur into every 1.0g of high-purity graphite at the temperature of 80 DEG CAcid (96 wt%), 4g P 2 O 5 And 4g K 2 S 2 O 8 To the prepared mixed solution, magnetic stirring was performed for 4.5 hours, and then 4g of KMnO was slowly added under ice-water bath 4 (ii) a After the solution is cooled to room temperature, slowly adding 80mL of hydrogen peroxide solution (80 wt%), and standing for 24 h; centrifuging the solution after standing, separating out a yellow brown solid, and washing with deionized water for multiple times until the pH value of the supernatant is 7; and (3) carrying out vacuum freeze drying on the yellow brown solid for 24 hours to obtain the graphene.
6. A preparation method of the graphene-modified polypropylene resin as claimed in any one of claims 1 to 5, comprising the following steps:
s1: drying the polypropylene powder in a blast drying oven;
s2: weighing the components in corresponding parts by mass according to any one of claims 1 to 5, and fully stirring and mixing to obtain a mixture;
s3: and extruding and granulating the mixture to obtain the graphene modified polypropylene resin.
7. The method of claim 6, wherein in step S1, the moisture content of the polypropylene powder is dried to less than 100 ppm.
8. The method according to claim 6, wherein in step S2, the mixture is mixed with a high-speed mixer for 2-3 min.
9. The method according to claim 6, wherein in step S3, the extrusion granulation is performed by using a twin-screw extruder, wherein the extruder temperature is 180-230 ℃ and the screw rotation speed is 350-400 r/min.
CN202210773888.7A 2022-07-01 2022-07-01 Graphene modified polypropylene resin and preparation method thereof Pending CN115011039A (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
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Publications (1)

Publication Number Publication Date
CN115011039A true CN115011039A (en) 2022-09-06

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