CN113321883A - Preparation method of homogeneous polytetrafluoroethylene self-lubricating three-layer composite material - Google Patents

Preparation method of homogeneous polytetrafluoroethylene self-lubricating three-layer composite material Download PDF

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Publication number
CN113321883A
CN113321883A CN202110500073.7A CN202110500073A CN113321883A CN 113321883 A CN113321883 A CN 113321883A CN 202110500073 A CN202110500073 A CN 202110500073A CN 113321883 A CN113321883 A CN 113321883A
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mixed solution
polytetrafluoroethylene
stirring
lubricating
composite material
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CN202110500073.7A
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Inventor
许永坤
樊学峰
孙志华
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Zhejiang Changsheng Sliding Bearings Co Ltd
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Zhejiang Changsheng Sliding Bearings Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • C08K2003/162Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Lubricants (AREA)

Abstract

A preparation method of a homogeneous polytetrafluoroethylene self-lubricating three-layer composite material comprises the following steps: step S1: mixing and stirring functional filler particles, nano particles and water to form a suspension; step S2: grinding the suspension by a colloid grinder to form emulsion; step S3: stirring the emulsion, the polytetrafluoroethylene concentrated dispersion and the reinforcing filler to form a first mixed solution; step S4: stirring the first mixed solution and polytetrafluoroethylene suspension powder to form a second mixed solution; step S5: heating and stirring the second mixed solution; step S6: and drying the second mixed solution until the second mixed solution is dried to be in a slurry state. The dispersion is uniform, agglomeration is avoided, and the mechanical property, the self-lubricating property and the friction resistance are improved.

Description

Preparation method of homogeneous polytetrafluoroethylene self-lubricating three-layer composite material
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a preparation method of a homogeneous polytetrafluoroethylene self-lubricating three-layer composite material.
Background
Polytetrafluoroethylene (PTFE, abbreviated as "plastic king") is a high molecular polymer prepared by polymerizing tetrafluoroethylene as a monomer. The coating is white wax-like, semitransparent, excellent in heat resistance and cold resistance, strong in corrosion resistance, resistant to acid and alkali, resistant to various organic solvents and extremely low in friction coefficient, and can be used at the temperature of minus 180-260 ℃ for a long time. And is therefore particularly suitable for use as a protective layer for self-lubricating materials. However, the existing polytetrafluoroethylene has poor dispersibility, and if inorganic fillers with the particle size of less than 10um, such as calcium fluoride, calcium oxide, silicon dioxide, barium sulfate and other particles, are directly added, the particles are easy to agglomerate and are unevenly distributed, and the performance is affected.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene, which has the advantages of uniform dispersion, avoiding agglomeration, and improving mechanical properties, self-lubricating property and friction resistance, so as to solve the above problems.
The preparation method of the homogeneous polytetrafluoroethylene self-lubricating three-layer composite material comprises the following steps: step S1: mixing and stirring functional filler particles, nano particles and water to form a suspension; step S2: grinding the suspension by a colloid grinder for 10-15 minutes to form emulsion; step S3: stirring the emulsion, the polytetrafluoroethylene concentrated dispersion and the reinforcing filler to form a first mixed solution, wherein the temperature is 30-50 ℃, and the stirring time is 30-60 minutes; step S4: stirring the first mixed solution and polytetrafluoroethylene suspension powder to form a second mixed solution, wherein the stirring time is 30-60 minutes; step S5: heating and stirring the second mixed solution at 80-90 ℃; step S6: and drying the second mixed solution until the second mixed solution is dried into a slurry state, wherein the heating temperature is 110 ℃.
Further, the functional filler particles are one or any combination of calcium fluoride, calcium oxide, silicon dioxide and barium sulfate.
Further, the volume ratio of the water powder in the suspension is more than 4: 1.
further, the reinforcing filler is one or any combination of glass fiber, carbon fiber, aramid fiber and potassium titanate whisker.
Further, the volume ratio of the reinforcing filler in the first mixed solution is 3-15%.
Further, the volume ratio of the fluoride in the first mixed solution is 1: 4.
further, the volume ratio of the polytetrafluoroethylene to the fluoride in the first mixed solution is 95: 20 to 70: 120.
further, the weight ratio of the alcohol in the second mixed solution is 1%.
Compared with the prior art, the preparation method of the homogeneous polytetrafluoroethylene self-lubricating three-layer composite material comprises the following steps: step S1: mixing and stirring functional filler particles, nano particles and water to form a suspension; step S2: grinding the suspension by a colloid grinder for 10-15 minutes to form emulsion; step S3: stirring the emulsion, the polytetrafluoroethylene concentrated dispersion and the reinforcing filler to form a first mixed solution, wherein the temperature is 30-50 ℃, and the stirring time is 30-60 minutes; step S4: stirring the first mixed solution and polytetrafluoroethylene suspension powder to form a second mixed solution, wherein the stirring time is 30-60 minutes; step S5: heating and stirring the second mixed solution at 80-90 ℃; step S6: and drying the second mixed solution until the second mixed solution is dried into a slurry state, wherein the heating temperature is 110 ℃. The dispersion is uniform, agglomeration is avoided, and the mechanical property, the self-lubricating property and the friction resistance are improved.
Drawings
Embodiments of the invention are described below with reference to the accompanying drawings, in which:
FIG. 1 is a schematic diagram of the steps of the preparation method of the homogeneous polytetrafluoroethylene self-lubricating three-layer composite material provided by the invention.
FIG. 2 is a bar graph comparing the amount of wear of the products of example 1, example 2 and comparative example.
Detailed Description
Specific embodiments of the present invention will be described in further detail below based on the drawings. It should be understood that the description herein of embodiments of the invention is not intended to limit the scope of the invention.
Referring to fig. 1, the preparation method of the homogeneous polytetrafluoroethylene self-lubricating three-layer composite material provided by the invention comprises the following steps:
step S1: mixing functional filler particles (such as one or more of calcium fluoride, calcium oxide, silicon dioxide, barium sulfate and the like), nanoparticles (such as one or more of silicon dioxide nanoparticles, silicon nitride nanoparticles and aluminum oxide nanoparticles) and water, and stirring to form a suspension (the volume ratio of water to powder is more than 4: 1);
step S2: grinding the suspension by a colloid grinder for 10-15 minutes to form emulsion;
step S3: stirring the ground emulsion, a polytetrafluoroethylene concentrated dispersion solution and a reinforcing filler (a fibrous structure filler such as one or more of glass fiber, carbon fiber, aramid fiber, potassium titanate whisker and the like) at a volume ratio of 3-15% to form a first mixed solution, wherein the temperature is 30-50 ℃ and the stirring time is 30-60 minutes; the volume ratio of the fluoride in the first mixed solution is 1: 4;
step S4: stirring the stirred first mixed solution and polytetrafluoroethylene suspension powder, wherein the volume ratio of polytetrafluoroethylene to fluoride in the first mixed solution is 95: 20 to 70: 120, forming a second mixed solution, adding alcohol in the stirring process, wherein the weight ratio of the alcohol in the second mixed solution is 1%, the solubility of the polytetrafluoroethylene suspension powder can be improved, and the stirring time is 30-60 minutes;
step S5: heating and stirring the mixed second mixed solution at the temperature of 80-90 ℃;
step S6: and drying the second mixed solution at the heating temperature of 110 ℃ to obtain slurry.
And then carrying out wet fluorine compounding, roll compounding the sintered spherical powder plate and the slurry, drying and sintering to form the membrane-shaped homogeneous polytetrafluoroethylene self-lubricating three-layer composite material.
Example 1
Step S1: mixing and stirring 20 wt.% of functional filler calcium fluoride particles and 1 wt.% of silicon dioxide nano particles with water at room temperature by using an electric stirrer, adding water in an amount which is 50 times of the weight of the calcium fluoride and the nano particles, and stirring to form a suspension;
step S2: grinding the suspension by a colloid grinder for 10-15 minutes to form emulsion;
step S3: stirring the ground emulsion, 33 wt.% of polytetrafluoroethylene concentrated dispersion and 4 wt.% of carbon fiber to form a first mixed solution, wherein the temperature is 30-50 ℃, and the stirring time is 30 minutes;
step S4: stirring the stirred first mixed solution and 55 wt.% of polytetrafluoroethylene suspension powder, adding alcohol in the stirring process, wherein the weight ratio of the alcohol in the second mixed solution is 1 wt.%, and stirring for 30 minutes;
step S5: heating and stirring the mixed second mixed solution at 80-90 ℃, and performing centrifugal dehydration after stirring;
step S6: and drying the dehydrated second mixed solution at the heating temperature of 110 ℃ to obtain slurry.
And then carrying out wet fluorine compounding, roll compounding the sintered spherical powder plate and the slurry, drying and sintering to form the membrane-shaped homogeneous polytetrafluoroethylene self-lubricating three-layer composite material.
Example 2
Step S1: mixing and stirring 20 wt.% of functional filler calcium fluoride particles and 2 wt.% of alumina nano particles with water at room temperature by using an electric stirrer, adding water in an amount which is 20 times of the weight of the calcium fluoride and the nano particles, and stirring to form a suspension;
step S2: grinding the suspension by a colloid grinder for 10-15 minutes to form emulsion;
step S3: stirring the ground emulsion, 33 wt.% of polytetrafluoroethylene concentrated dispersion and 3 wt.% of glass fiber to form a first mixed solution, wherein the temperature is 30-50 ℃, and the stirring time is 30 minutes;
step S4: stirring the stirred first mixed solution and 55 wt.% of polytetrafluoroethylene suspension powder, adding alcohol during stirring, wherein the weight ratio of acetone in the second mixed solution is 1 wt.%, and the stirring time is 30 minutes;
step S5: heating and stirring the mixed second mixed solution at 80-90 ℃, and performing centrifugal dehydration after stirring;
step S6: and drying the dehydrated second mixed solution at the heating temperature of 110 ℃ to obtain slurry.
And then carrying out wet fluorine compounding, roll compounding the sintered spherical powder plate and the slurry, drying and sintering to form the membrane-shaped homogeneous polytetrafluoroethylene self-lubricating three-layer composite material.
Comparative example:
step S1: firstly mixing 15 wt.% of polyphenyl ester, 5 wt.% of glass fiber, 1 wt.% of alumina particles and 30 wt.% of polytetrafluoroethylene suspension powder, and then stirring at high speed;
step S2: adding 100 wt.% of polytetrafluoroethylene emulsion (with the solid content of 60 wt%) into the stirred mixture, granulating and stirring to form slurry;
and then carrying out wet fluorine compounding, roll compounding the sintered spherical powder plate and the slurry, drying and sintering to form the membrane-shaped homogeneous polytetrafluoroethylene self-lubricating three-layer composite material.
Refer to FIG. 2, which is a bar graph comparing the wear loss of PTFE composite materials prepared in examples 1 and 2 and comparative example after continuous operation for 8h in oil lubrication (32# lube) medium at a load of 20MPa and a rotation speed of 1 m/s. The test was carried out using a standard MPV-20D friction wear tester. This figure shows that the amount of abrasion was significantly reduced for both samples of example 1 and example 2 compared to the comparative example.
Compared with the prior art, the preparation method of the homogeneous polytetrafluoroethylene self-lubricating three-layer composite material comprises the following steps: step S1: mixing and stirring functional filler particles, nano particles and water to form a suspension; step S2: grinding the suspension by using a colloid grinder to form emulsion; step S3: stirring the emulsion, the polytetrafluoroethylene concentrated dispersion and the reinforcing filler to form a first mixed solution; step S4: stirring the first mixed solution and polytetrafluoroethylene suspension powder to form a second mixed solution; step S5: heating and stirring the second mixed solution; step S6: and drying the second mixed solution until the second mixed solution is dried to be in a slurry state. The homogeneous polytetrafluoroethylene self-lubricating three-layer composite material formed in the way is uniformly dispersed, avoids agglomeration, and improves the mechanical property, self-lubricating property and friction resistance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, and any modifications, equivalents or improvements that are within the spirit of the present invention are intended to be covered by the following claims.

Claims (8)

1. A preparation method of a homogeneous polytetrafluoroethylene self-lubricating three-layer composite material is characterized by comprising the following steps: the method comprises the following steps:
step S1: mixing and stirring functional filler particles, nano particles and water to form a suspension;
step S2: grinding the suspension by a colloid grinder for 10-15 minutes to form emulsion;
step S3: stirring the emulsion, the polytetrafluoroethylene concentrated dispersion and the reinforcing filler to form a first mixed solution, wherein the temperature is 30-50 ℃, and the stirring time is 30-60 minutes;
step S4: stirring the first mixed solution and polytetrafluoroethylene suspension powder to form a second mixed solution, wherein the stirring time is 30-60 minutes;
step S5: heating and stirring the second mixed solution at 80-90 ℃;
step S6: and drying the second mixed solution until the second mixed solution is dried into a slurry state, wherein the heating temperature is 110 ℃.
2. The process for the preparation of the homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene according to claim 1, wherein: the functional filler particles are one or any combination of calcium fluoride, calcium oxide, silicon dioxide and barium sulfate.
3. The process for the preparation of the homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene according to claim 1, wherein: the volume ratio of water to powder in the suspension is more than 4: 1.
4. the process for the preparation of the homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene according to claim 1, wherein: the reinforcing filler is one or any combination of glass fiber, carbon fiber, aramid fiber and potassium titanate whisker.
5. The process for the preparation of the homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene according to claim 1, wherein: the volume ratio of the reinforcing filler in the first mixed solution is 3-15%.
6. The process for the preparation of the homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene according to claim 1, wherein: the volume ratio of fluoride in the first mixed solution is 1: 4.
7. the process for the preparation of the homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene according to claim 1, wherein: the volume ratio of the polytetrafluoroethylene to the fluoride in the first mixed solution is 95: 20 to 70: 120.
8. the process for the preparation of the homogeneous self-lubricating three-layer composite material of polytetrafluoroethylene according to claim 1, wherein: the weight ratio of the alcohol in the second mixed solution is 1%.
CN202110500073.7A 2021-05-08 2021-05-08 Preparation method of homogeneous polytetrafluoroethylene self-lubricating three-layer composite material Pending CN113321883A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049364A (en) * 1989-08-07 1991-02-20 斯塔特尼怀茨库尼乌斯塔夫物料公司 The matrix material and the manufacture method thereof that are used for sliding surface
CN103333442A (en) * 2013-06-08 2013-10-02 山东瑞特新材料有限公司 Preparation method of TiO2-SiC-fiber filled polytetrafluoroethylene composite material
WO2016034827A1 (en) * 2014-09-05 2016-03-10 Centre Technique Des Industries Mecaniques Matériau composite autolubrifiant
CN112608783A (en) * 2020-12-14 2021-04-06 合肥波林新材料股份有限公司 Three-layer composite self-lubricating material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049364A (en) * 1989-08-07 1991-02-20 斯塔特尼怀茨库尼乌斯塔夫物料公司 The matrix material and the manufacture method thereof that are used for sliding surface
CN103333442A (en) * 2013-06-08 2013-10-02 山东瑞特新材料有限公司 Preparation method of TiO2-SiC-fiber filled polytetrafluoroethylene composite material
WO2016034827A1 (en) * 2014-09-05 2016-03-10 Centre Technique Des Industries Mecaniques Matériau composite autolubrifiant
CN112608783A (en) * 2020-12-14 2021-04-06 合肥波林新材料股份有限公司 Three-layer composite self-lubricating material and preparation method thereof

Non-Patent Citations (1)

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Title
王晓波 等: "SiO2填充聚四氟乙烯复合材料的摩擦学行为研究", 《润滑与密封》 *

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