CN113462106A - Wear-resistant sealing ring and preparation method thereof - Google Patents
Wear-resistant sealing ring and preparation method thereof Download PDFInfo
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
The application relates to the field of sealing rings, and particularly discloses a wear-resistant sealing ring and a preparation method thereof. The wear-resistant sealing ring comprises a sealing ring body, and the sealing ring body comprises the following raw materials: polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, rosin resin-alcohol ether phosphate ester compound and molybdenum disulfide; the preparation method comprises the following steps: s1, mixing raw materials; and S2, die pressing and sintering. The polytetrafluoroethylene suspended particles and the rosin resin-alcohol ether phosphate ester compound are adopted, the polytetrafluoroethylene suspended particles have better dispersibility and can be mixed with raw materials more uniformly, the rosin resin-alcohol ether phosphate ester compound is adhered to the surface of the polytetrafluoroethylene suspended particles, the binding force between the raw materials is improved after mixing, the compatibility of PEEK and the polytetrafluoroethylene suspended particles is favorably improved, the wear resistance of the sealing ring body is improved, the sealing ring body is more durable, the material waste caused by the premature damage of the sealing ring body is reduced, and a certain energy-saving effect is achieved.
Description
Technical Field
The application relates to the field of sealing rings, in particular to a wear-resistant sealing ring and a preparation method thereof.
Background
The sealing ring, which is generally a supporting ring or piston ring, is a part used on the reciprocating compressor for supporting the motion of the piston or piston rod, and can prevent the piston or piston rod from directly contacting and rubbing with the cylinder in the motion process, thus playing a role of protecting the cylinder and the piston or piston rod from being damaged.
However, in the related art, the wear resistance of the sealing ring is poor, and after the sealing ring is used for a period of time, the wear rate of the sealing ring is high, so that the sealing ring is influenced to play a protection role and needs to be improved.
Disclosure of Invention
In order to solve the problem that the wear resistance of a sealing ring is poor, the application provides a wear-resistant sealing ring and a preparation method thereof.
In a first aspect, the present application provides a wear-resistant seal ring, which adopts the following technical scheme:
the wear-resistant sealing ring comprises a sealing ring body, wherein the sealing ring body comprises the following raw materials in parts by weight:
50-60 parts of polytetrafluoroethylene suspended particles;
15-20 parts of potassium titanate whisker;
10-14 parts of glass fiber;
10-14 parts of PEEK;
8-14 parts of rosin resin-alcohol ether phosphate ester compound;
8-10 parts of molybdenum disulfide.
By adopting the technical scheme, the polytetrafluoroethylene suspended particles have better dispersibility and good self-lubricating property, have the characteristic of low friction coefficient of polytetrafluoroethylene, can be mixed with other raw materials more uniformly, and ensure that the overall performance of the sealing ring body is better.
The addition of the potassium titanate whiskers can improve the wear resistance of the sealing ring body and reduce the friction coefficient of the sealing ring body, so that the wear rate of the sealing ring body is reduced.
The glass fiber is an inorganic non-metallic material with excellent performance, the heat resistance is good, the corrosion resistance is strong, the mechanical strength is high, the glass fiber and the PEEK have good affinity, the mechanical strength of the sealing ring body can be improved by adding the glass fiber and the PEEK in a synergistic mode, adhesion abrasion is inhibited, and the abrasion rate of the sealing ring body is reduced.
PEEK has good comprehensive properties, and the heat resistance is good, still has high strength, high rigidity, creep resistance and fine fatigue resistance to and from characteristics such as fire-retardant, resistant oil, resistant organic solvent, PEEK and polytetrafluoroethylene suspended particle mix, can remain the mechanical properties of PEEK, heat-resisting, hydrolysis resistance and wear-resisting characteristic, can reduce the coefficient of friction of sealing ring body again, make the sealing ring body have better wearability.
The rosin resin-alcohol ether phosphate ester compound is a viscous substance and is adhered to the surface of the polytetrafluoroethylene suspended particles after being uniformly mixed with the polytetrafluoroethylene suspended particles, so that the polytetrafluoroethylene suspended particles are more tightly combined with other raw materials, the binding force between the raw materials is improved, and when the sealing ring body is impacted, the raw materials are not easy to peel off, so that the wear resistance of the sealing ring body is improved, and the wear rate of the sealing ring body is reduced.
The molecular structure of the rosin resin-alcohol ether phosphate compound contains ether bonds, the molecular structure of the PEEK contains ether bonds, according to the similar intermiscibility principle, the compatibility of the PEEK and the rosin resin-alcohol ether phosphate compound is good, and after the rosin resin-alcohol ether phosphate compound is adhered to the surface of the polytetrafluoroethylene suspended particles, the compatibility between the PEEK and the polytetrafluoroethylene suspended particles is favorably improved, so that the PEEK and the polytetrafluoroethylene suspended particles are mixed more uniformly, and the wear resistance of the sealing ring body is favorably improved.
Molybdenum disulfide has better dispersibility and good lubricity, and chemical stability and thermal stability are good, adds molybdenum disulfide can prolong the life of sealing ring body, improves the lubricity of sealing ring body, reduces the coefficient of friction on sealing ring body surface to reduce the wear rate of sealing ring body.
Through the combined action of polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, rosin resin-alcohol ether phosphate ester compounds and molybdenum disulfide, the wear resistance of the sealing ring body is improved, the wear rate of the sealing ring body is reduced, the sealing ring body is more durable, the material waste caused by discarding the premature damage of the sealing ring body to prepare the sealing ring body is reduced, and a certain energy-saving effect is achieved.
Preferably, the raw materials further comprise 1-2 parts of tert-butyl lithium and 1-2 parts of ethylenediamine in parts by weight.
By adopting the technical scheme, tert-butyl lithium and ethylenediamine are mixed to form a free radical, the free radical is substituted by F atoms on polytetrafluoroethylene suspended particles, the tert-butyl replaces the F atoms on the original polytetrafluoroethylene suspended particles, the polarity of the surface of the polytetrafluoroethylene suspended particles is improved, so that a rosin resin-alcohol ether phosphate compound is easier to adhere to the surface of the polytetrafluoroethylene suspended particles, the adhesion force between the rosin resin-alcohol ether phosphate compound and the polytetrafluoroethylene suspended particles is stronger, the indirect improvement of the compatibility between PEEK and the polytetrafluoroethylene suspended particles is facilitated, and the wear resistance of the sealing ring body is better.
Preferably, the raw material also comprises 6 to 8 parts of glycidyl methacrylate by weight.
Through adopting above-mentioned technical scheme, the back takes place to replace with the F atom on the polytetrafluoroethylene suspended particle for the free radical, form carbon center free radical in the position of going F, carbon center free radical causes glycidyl methacrylate and polytetrafluoroethylene suspended particle to take place graft polymerization, the molecular weight of polytetrafluoroethylene suspended particle has been increased, make the molecular appeal increase between the polytetrafluoroethylene suspended particle molecule after the grafting, thereby the cohesion between the inside raw materials of sealing ring body has been improved, make more difficult emergence split or peel off between the raw materials, from this the wear rate of sealing ring body has been reduced, reach comparatively ideal wear-resisting effect.
Preferably, the preparation method of the rosin resin-alcohol ether phosphate ester compound comprises the following steps of: heating 4-5 parts of rosin resin to 180 ℃ at 170 ℃ and stirring until the rosin resin is completely melted, adding 8-10 parts of alcohol ether phosphate and 0.1-0.2 part of zirconium oxide, stirring for reacting for 3-4h, and cooling to room temperature to obtain the rosin resin-alcohol ether phosphate compound.
By adopting the technical scheme, the molecular structure of the rosin resin has a carboxyl active group, and the rosin resin and the hydroxyl on the alcohol ether phosphate ester are subjected to esterification reaction under the catalysis of the zirconium oxide, so that a product with higher viscosity is obtained.
Preferably, the raw materials also comprise 3-5 parts of urea-formaldehyde resin by weight.
Through adopting above-mentioned technical scheme, urea-formaldehyde resin's surface tension is less than the raw materials system of sealing ring body, easily migrate to sealing ring body surface after mixing, surface tension is low because of urea-formaldehyde resin, urea-formaldehyde resin can level gradually at sealing ring body surface, make sealing ring body surface more smooth, be favorable to reducing the coefficient of friction on sealing ring body surface, and reduced glass fiber and potassium titanate whisker protrusion in sealing ring body surface, lead to the condition that sealing ring body surface wear aggravates, be favorable to reducing the wear rate of sealing ring body, improve the wearability of sealing ring body.
Preferably, the raw materials also comprise 0.4 to 0.6 part of fluorocarbon surface modifier and 2 to 3 parts of ethanol according to parts by weight.
By adopting the technical scheme, ethanol is used as a solvent, and the potassium titanate whisker is modified by the fluorocarbon surface modifier, so that the surface energy of the potassium titanate whisker is reduced, the dispersibility of the potassium titanate whisker in raw materials is improved, the potassium titanate whisker and other raw materials are more uniformly mixed, the agglomeration of the potassium titanate whisker is reduced, and the wear resistance of the sealing ring body is indirectly improved.
In a second aspect, the present application provides a method for preparing a wear-resistant seal ring, which adopts the following technical scheme:
a preparation method of a wear-resistant sealing ring comprises the following steps:
s1, mixing raw materials: uniformly stirring and mixing polytetrafluoroethylene suspended particles and a rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting PEEK at 340-350 ℃, adding the mixture A, uniformly stirring, adding potassium titanate whiskers, glass fibers and molybdenum disulfide, and uniformly stirring to prepare a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 320 ℃ for heat preservation for 20-30min, taking out the mold filled with the materials, cooling to 160 ℃ for heat preservation, demolding, and cooling to room temperature to obtain the sealing ring body.
Through adopting above-mentioned technical scheme, mix PEEK and mixture A earlier, reduced the interference of other raw materials to PEEK and mixture A mixing process, be favorable to PEEK and mixture A to mix more evenly.
Preferably, in the step S1, glycidyl methacrylate and ethanol are uniformly mixed in a mass ratio of 1:4 to prepare a mixed solution;
mixing tert-butyl lithium and ethylenediamine uniformly, adding polytetrafluoroethylene suspended particles, and introducing N2Stirring and reacting at 0 ℃ for 30-40min, taking out polytetrafluoroethylene suspended particles, washing with tetrahydrofuran at 0 ℃ for 2-3 times, adding the polytetrafluoroethylene suspended particles into the mixed solution, stirring and reacting at 70-75 ℃ for 8-9h, washing with distilled water at 50-55 ℃, performing suction filtration, washing with absolute ethyl alcohol, performing suction filtration, washing with acetone, and performing suction filtration to obtain a product A;
uniformly stirring and mixing the fluorocarbon surface modifier and ethanol to obtain a mixture B, spraying the mixture B on the surface of the potassium titanate whisker, stirring for 5-8min, and drying at the temperature of 100-110 ℃ for 6-7h to obtain a product B;
and uniformly stirring and mixing the product A and the rosin resin-alcohol ether phosphate compound to obtain a mixture C, then stirring and melting the PEEK at the temperature of 340-350 ℃, adding the mixture C, uniformly stirring, adding the product B, the glass fiber and the molybdenum disulfide, uniformly stirring, cooling to the temperature of 150-170 ℃, adding the urea-formaldehyde resin, and uniformly stirring to obtain the mixed raw material.
By adopting the technical scheme, the reaction of the polytetrafluoroethylene suspended particles and the glycidyl methacrylate, the reaction of the fluorocarbon surface modifier and the potassium titanate whisker and the mixing of other raw materials are separately carried out, so that the interference of the other raw materials on the reaction is reduced, and the product A and the product B are favorably obtained.
In summary, the present application has the following beneficial effects:
1. because the polytetrafluoroethylene suspended particles and the rosin resin-alcohol ether phosphate ester compound are adopted, the polytetrafluoroethylene suspended particles have better dispersibility and can be mixed with other raw materials more uniformly, and the rosin resin-alcohol ether phosphate ester compound is adhered to the surface of the polytetrafluoroethylene suspended particles, so that the binding force between the raw materials is improved after mixing, and the compatibility between PEEK and the polytetrafluoroethylene suspended particles is favorably improved, thereby improving the wear resistance of the sealing ring body and reducing the wear rate of the sealing ring body.
2. Preferably adopt tert-butyl lithium and ethylenediamine in this application, tert-butyl lithium and ethylenediamine mix and form the free radical, and the F atom on free radical and the polytetrafluoroethylene suspended particle takes place to replace, has improved the polarity on polytetrafluoroethylene suspended particle surface, is favorable to indirectly improving the compatibility between PEEK and the polytetrafluoroethylene suspended particle for the wearability of sealing ring body is better.
3. The preferred glycidyl methacrylate that adopts in this application, the glycidyl methacrylate takes place graft polymerization with polytetrafluoroethylene suspended particle, has increased polytetrafluoroethylene suspended particle's molecular weight, has improved the cohesion between the inside raw materials of sealing ring body for more difficult emergence split between the raw materials or peel off, reach comparatively ideal wear-resisting effect.
Detailed Description
The present application will be described in further detail with reference to examples.
Polytetrafluoroethylene was purchased from Suzhou Changshu plastification, Inc. under the designation 340; the cargo number is 24G 62; the potassium titanate whisker is purchased from Shanghai Poncirus pelagina composite new material science and technology Limited company with the brand number of NP-TW 4; the glass fiber is purchased from Changzhou Tuwei building materials GmbH, and the specification is 3 mm; PEEK is purchased from Xinwang plastic industry official exclusive stores with the brand number of 450G; the molybdenum disulfide is purchased from a luxury official exclusive store, the product number is HY564645, and the granularity is 325 meshes; tert-butyl lithium was purchased from shaoxing poppy-wareny chemical ltd; glycidyl methacrylate was purchased from Shanghai Hao chemical Co., Ltd; the rosin resin is purchased from Zhengzhou Saibo chemical products Co., Ltd, and the brand number is 110; the alcohol ether phosphate is purchased from Haian petrochemical source manufacturers and has the model of MOA-9P; the urea-formaldehyde resin is purchased from Zhengzhou Xinke chemical products Co., Ltd, and the cargo number is 5892-568; the fluorocarbon surface modifier is purchased from Guangzhou Si Tuiyuan chemical Co., Ltd, and is a Dupont Zonyl-FSO surfactant; the silane coupling agent is purchased from Guangdong Kangjin chemical special shops and has the model number of 792.
The raw materials used in the following embodiments may be those conventionally commercially available unless otherwise specified.
Preparation examples of raw materials
Preparation example 1
Preparation of rosin resin-alcohol ether phosphate ester compound: heating 40g of rosin resin to 170 ℃, stirring until the rosin resin is completely melted, adding 80g of alcohol ether phosphate and 3g of zirconium oxide, stirring for reacting for 4 hours, and cooling to room temperature to obtain the rosin resin-alcohol ether phosphate compound.
Preparation example 2
Preparation of rosin resin-alcohol ether phosphate ester compound: heating 50g of rosin resin to 180 ℃, stirring until the rosin resin is completely melted, adding 100g of alcohol ether phosphate and 6g of zirconium oxide, stirring for reacting for 3 hours, and cooling to room temperature to obtain the rosin resin-alcohol ether phosphate compound.
Preparation example 3
Preparation of rosin resin-alcohol ether phosphate ester compound: heating 45g of rosin resin to 175 ℃, stirring until the rosin resin is completely melted, adding 90g of alcohol ether phosphate and 5g of zirconium oxide, stirring for reacting for 4 hours, and cooling to room temperature to obtain the rosin resin-alcohol ether phosphate compound.
Preparation example 4
Preparation of polytetrafluoroethylene suspension particles: the polytetrafluoroethylene is smashed and then ground, then washed with water for 2 times, dried at 40 ℃, and sieved by a 100-mesh sieve to prepare the polytetrafluoroethylene suspended particles.
Examples
Example 1
The application discloses wear-resisting sealing ring, including the sealing ring body, the sealing ring body includes following raw materials: the composite material comprises polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, a rosin resin-alcohol ether phosphate compound and molybdenum disulfide, wherein the polytetrafluoroethylene suspended particles are prepared from preparation example 4, the rosin resin-alcohol ether phosphate compound is prepared from preparation example 1, and the content of each component is shown in the following table 1-1.
The preparation method of the wear-resistant sealing ring comprises the following steps:
s1, mixing raw materials: uniformly stirring and mixing polytetrafluoroethylene suspended particles and a rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting PEEK at 340 ℃, adding the mixture A, uniformly stirring, adding potassium titanate whiskers, glass fibers and molybdenum disulfide, and uniformly stirring to prepare a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 300 ℃, preserving heat for 30min, taking out the mold filled with the materials, cooling to 150 ℃, demolding, and cooling to room temperature to obtain the sealing ring body.
Example 2
The application discloses wear-resisting sealing ring, including the sealing ring body, the sealing ring body includes following raw materials: the composite material comprises polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, a rosin resin-alcohol ether phosphate compound and molybdenum disulfide, wherein the polytetrafluoroethylene suspended particles are prepared from preparation example 4, the rosin resin-alcohol ether phosphate compound is prepared from preparation example 2, and the content of each component is shown in the following table 1-1.
The preparation method of the wear-resistant sealing ring comprises the following steps:
s1, mixing raw materials: uniformly stirring and mixing polytetrafluoroethylene suspended particles and a rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting PEEK at 350 ℃, adding the mixture A, uniformly stirring, adding potassium titanate whiskers, glass fibers and molybdenum disulfide, and uniformly stirring to prepare a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 320 ℃, preserving heat for 20min, taking out the mold filled with the materials, cooling to 160 ℃, demolding, and cooling to room temperature to obtain the sealing ring body.
Example 3
The application discloses wear-resisting sealing ring, including the sealing ring body, the sealing ring body includes following raw materials: the composite material comprises polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, a rosin resin-alcohol ether phosphate compound and molybdenum disulfide, wherein the polytetrafluoroethylene suspended particles are prepared from preparation example 4, the rosin resin-alcohol ether phosphate compound is prepared from preparation example 3, and the content of each component is shown in the following table 1-1.
The preparation method of the wear-resistant sealing ring comprises the following steps:
s1, mixing raw materials: uniformly stirring and mixing polytetrafluoroethylene suspended particles and a rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting PEEK at 345 ℃, adding the mixture A, uniformly stirring, adding potassium titanate whiskers, glass fibers and molybdenum disulfide, and uniformly stirring to prepare a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 310 ℃, preserving heat for 25min, taking out the mold filled with the materials, cooling to 155 ℃, demolding, and cooling to room temperature to obtain the sealing ring body.
Example 4
The difference from example 1 is that t-butyllithium and ethylenediamine were added to the raw material for the seal ring body, and the contents of the respective components are shown in the following Table 1-1.
S1, mixing raw materials: mixing tert-butyl lithium and ethylenediamine uniformly, adding polytetrafluoroethylene suspended particles, and introducing N2，0℃Stirring and reacting for 30min, then taking out the polytetrafluoroethylene suspended particles, and washing for 2 times by using tetrahydrofuran at the temperature of 0 ℃;
and uniformly stirring and mixing the washed polytetrafluoroethylene suspended particles and the rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting the PEEK at 340 ℃, adding the mixture A, uniformly stirring, adding the potassium titanate whisker, the glass fiber and the molybdenum disulfide, and uniformly stirring to prepare a mixed raw material.
Example 5
The difference from example 4 is that glycidyl methacrylate was added to the raw material for the seal ring body, and the contents of the respective components are shown in the following table 1-1.
S1, mixing raw materials: uniformly mixing glycidyl methacrylate and ethanol in a mass ratio of 1:4 to prepare a mixed solution, uniformly mixing tert-butyl lithium and ethylenediamine, adding polytetrafluoroethylene suspension particles, and introducing N2Stirring and reacting for 30min at 0 ℃, then taking out polytetrafluoroethylene suspended particles, washing for 2 times by tetrahydrofuran at 0 ℃, then adding the polytetrafluoroethylene suspended particles into the mixed solution, stirring and reacting for 9h at 70 ℃, then washing for 2h by distilled water at 50 ℃, carrying out suction filtration, repeating the steps of washing and suction filtration for three times, then washing for 2h by absolute ethyl alcohol, carrying out suction filtration, repeating the steps of washing and suction filtration for three times, then washing for 2h by acetone, carrying out suction filtration, repeating the steps of washing and suction filtration for three times, and preparing a product A;
and uniformly stirring and mixing the product A and the rosin resin-alcohol ether phosphate compound to prepare a mixture C, then stirring and melting the PEEK at 340 ℃, adding the mixture C, uniformly stirring, adding the potassium titanate whisker, the glass fiber and the molybdenum disulfide, and uniformly stirring to prepare a mixed raw material.
Example 6
The difference from example 1 is that urea resin was added to the raw material of the seal ring body, and the contents of the respective components are shown in the following table 1-1.
S1, mixing raw materials: uniformly stirring and mixing polytetrafluoroethylene suspended particles and a rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting PEEK at 340 ℃, adding the mixture A, uniformly stirring, adding potassium titanate whiskers, glass fibers and molybdenum disulfide, uniformly stirring, cooling to 150 ℃, adding urea-formaldehyde resin, uniformly stirring, and preparing a mixed raw material.
Example 7
The difference from the example 1 is that the fluorocarbon surface modifier and ethanol are added into the raw materials of the sealing ring body, and the contents of the components are shown in the following table 1-1.
S1, mixing raw materials: uniformly stirring and mixing the fluorocarbon surface modifier and ethanol to obtain a mixture B, spraying the mixture B on the surface of the potassium titanate whisker, stirring for 5min, and drying at 100 ℃ for 7h to obtain a product B;
uniformly stirring and mixing polytetrafluoroethylene suspended particles and a rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting PEEK at 340 ℃, adding the mixture A, uniformly stirring, adding a product B, glass fiber and molybdenum disulfide, and uniformly stirring to prepare a mixed raw material.
Example 8
The application discloses wear-resisting sealing ring, including the sealing ring body, the sealing ring body includes following raw materials: the composite material comprises polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, a rosin resin-alcohol ether phosphate ester compound, molybdenum disulfide, tert-butyl lithium, ethylenediamine, glycidyl methacrylate, urea resin, a fluorocarbon surface modifier and ethanol, wherein the polytetrafluoroethylene suspended particles are prepared from preparation example 4, the rosin resin-alcohol ether phosphate ester compound is prepared from preparation example 1, and the content of each component is shown in the following table 1-1.
The preparation method of the wear-resistant sealing ring comprises the following steps:
s1, mixing raw materials: uniformly mixing glycidyl methacrylate and ethanol in a mass ratio of 1:4 to prepare a mixed solution;
mixing tert-butyl lithium and ethylenediamine uniformly, adding polytetrafluoroethylene suspended particles, and introducing N2Stirring and reacting at 0 ℃ for 30min, then taking out the polytetrafluoroethylene suspended particles, washing with tetrahydrofuran at 0 ℃ for 2 times, then adding the polytetrafluoroethylene suspended particles into the mixed solution, stirring and reacting at 70 ℃ for 9h, then washing with distilled water at 50 ℃ for 2h, carrying out suction filtration, repeating the washing and suction filtration steps for three times,washing with absolute ethyl alcohol for 2 hours, carrying out suction filtration, repeating the washing and suction filtration steps for three times, then washing with acetone for 2 hours, carrying out suction filtration, repeating the washing and suction filtration steps for three times, and obtaining a product A;
uniformly stirring and mixing the fluorocarbon surface modifier and ethanol to obtain a mixture B, spraying the mixture B on the surface of the potassium titanate whisker, stirring for 5min, and drying at 100 ℃ for 7h to obtain a product B;
uniformly stirring and mixing the product A and the rosin resin-alcohol ether phosphate compound to prepare a mixture C, then stirring and melting PEEK at 340 ℃, adding the mixture C, uniformly stirring, adding the product B, the glass fiber and the molybdenum disulfide, uniformly stirring, cooling to 150 ℃, adding the urea-formaldehyde resin, uniformly stirring, and preparing a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 300 ℃, preserving heat for 30min, taking out the mold filled with the materials, cooling to 150 ℃, demolding, and cooling to room temperature to obtain the sealing ring body.
Example 9
The application discloses wear-resisting sealing ring, including the sealing ring body, the sealing ring body includes following raw materials: polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, a rosin resin-alcohol ether phosphate compound, molybdenum disulfide, tert-butyl lithium, ethylenediamine, glycidyl methacrylate, urea resin, a fluorocarbon surface modifier and ethanol, wherein the polytetrafluoroethylene suspended particles are prepared from preparation example 4, the rosin resin-alcohol ether phosphate compound is prepared from preparation example 2, and the content of each component is shown in the following table 1-1.
The preparation method of the wear-resistant sealing ring comprises the following steps:
s1, mixing raw materials: uniformly mixing glycidyl methacrylate and ethanol in a mass ratio of 1:4 to prepare a mixed solution;
mixing tert-butyl lithium and ethylenediamine uniformly, adding polytetrafluoroethylene suspended particles, and introducing N2Stirring and reacting at 0 deg.C for 40min, taking out the polytetrafluoroethylene suspended particles, washing with tetrahydrofuran at 0 deg.C for 3 times, and adding the polytetrafluoroethylene suspended particlesStirring and reacting the mixed solution for 8 hours at 75 ℃, washing the mixed solution for 2 hours by using distilled water at 55 ℃, performing suction filtration, repeating the steps of washing and suction filtration for three times, then washing the mixed solution for 2 hours by using absolute ethyl alcohol, performing suction filtration, repeating the steps of washing and suction filtration for three times, then washing the mixed solution for 2 hours by using acetone, performing suction filtration, repeating the steps of washing and suction filtration for three times, and obtaining a product A;
uniformly stirring and mixing a fluorocarbon surface modifier and ethanol to obtain a mixture B, spraying the mixture B on the surface of the potassium titanate whisker, stirring for 8min, and drying at 110 ℃ for 6h to obtain a product B;
uniformly stirring and mixing the product A and the rosin resin-alcohol ether phosphate compound to prepare a mixture C, then stirring and melting PEEK at 350 ℃, adding the mixture C, uniformly stirring, adding the product B, the glass fiber and the molybdenum disulfide, uniformly stirring, cooling to 170 ℃, adding the urea-formaldehyde resin, uniformly stirring, and preparing a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 320 ℃, preserving heat for 20min, taking out the mold filled with the materials, cooling to 160 ℃, demolding, and cooling to room temperature to obtain the sealing ring body.
Example 10
The application discloses wear-resisting sealing ring, including the sealing ring body, the sealing ring body includes following raw materials: polytetrafluoroethylene suspended particles, potassium titanate whiskers, glass fibers, PEEK, a rosin resin-alcohol ether phosphate compound, molybdenum disulfide, tert-butyl lithium, ethylenediamine, glycidyl methacrylate, urea resin, a fluorocarbon surface modifier and ethanol, wherein the polytetrafluoroethylene suspended particles are prepared from preparation example 4, the rosin resin-alcohol ether phosphate compound is prepared from preparation example 3, and the content of each component is shown in the following tables 1-2.
The preparation method of the wear-resistant sealing ring comprises the following steps:
s1, mixing raw materials: uniformly mixing glycidyl methacrylate and ethanol in a mass ratio of 1:4 to prepare a mixed solution;
mixing tert-butyl lithium and ethylenediamine uniformly, adding polytetrafluoroethylene suspended particles, and introducing N2Stirring and reacting at 0 DEG C35min, taking out the polytetrafluoroethylene suspended particles, washing the polytetrafluoroethylene suspended particles for 3 times by using tetrahydrofuran at 0 ℃, adding the polytetrafluoroethylene suspended particles into the mixed solution, stirring the mixed solution at 73 ℃ for reaction for 8 hours, washing the mixed solution by using distilled water at 53 ℃ for 2 hours, performing suction filtration, repeating the steps of washing and suction filtration for three times, washing the mixed solution by using absolute ethyl alcohol for 2 hours, performing suction filtration, repeating the steps of washing and suction filtration for three times, washing the mixed solution by using acetone for 2 hours, performing suction filtration, repeating the steps of washing and suction filtration for three times, and preparing a product A;
uniformly stirring and mixing a fluorocarbon surface modifier and ethanol to obtain a mixture B, spraying the mixture B on the surface of the potassium titanate whisker, stirring for 7min, and drying at 105 ℃ for 6h to obtain a product B;
uniformly stirring and mixing the product A and the rosin resin-alcohol ether phosphate compound to prepare a mixture C, then stirring and melting PEEK at 345 ℃, adding the mixture C, uniformly stirring, then adding the product B, the glass fiber and the molybdenum disulfide, uniformly stirring, cooling to 160 ℃, adding the urea-formaldehyde resin, uniformly stirring, and preparing a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 310 ℃, preserving heat for 25min, taking out the mold filled with the materials, cooling to 155 ℃, demolding, and cooling to room temperature to obtain the sealing ring body.
Example 11
The difference from example 4 is that t-butyl lithium was replaced with methyl t-butyl ketone, and the contents of the respective components are shown in tables 1 to 2 below.
Example 12
The difference from example 4 is that ethylenediamine was replaced with acetonitrile, and the contents of the respective components are shown in tables 1 to 2 below.
Example 13
The difference from example 5 is that glycidyl methacrylate was replaced with ethyl acetate and the contents of the respective components are shown in tables 1 to 2 below.
Example 14
The difference from example 6 is that the urea resin was replaced with a polyester resin, and the contents of the respective components are shown in tables 1 to 2 below.
Example 15
The difference from example 7 is that the fluorocarbon surface modifier is replaced with a silane coupling agent, and the contents of the respective components are shown in tables 1 to 2 below.
Comparative example
Comparative example 1
The difference from example 1 is that a seal ring body made of polytetrafluoroethylene, potassium titanate whisker, glass fiber, molybdenum disulfide and PEEK was used as a blank control.
Comparative example 2
The difference from example 1 is that the polytetrafluoroethylene suspension particles were replaced with polytetrafluoroethylene, and the contents of the respective components are shown in tables 1 to 2 below.
Comparative example 3
The difference from example 1 is that rosin resin-alcohol ether phosphate ester compound was replaced with rosin resin, and the contents of the respective components are shown in tables 1 to 2 below.
TABLE 1-1 ingredient content table (unit: g)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | Example 9 | |
| Polytetrafluoroethylene suspension particles/polytetrafluoroethylene | 500 | 600 | 550 | 500 | 500 | 500 | 500 | 500 | 600 |
| Potassium titanate whisker | 200 | 150 | 170 | 200 | 200 | 200 | 200 | 200 | 150 |
| Glass fiber | 100 | 140 | 120 | 100 | 100 | 100 | 100 | 100 | 140 |
| PEEK | 100 | 140 | 120 | 100 | 100 | 100 | 100 | 100 | 140 |
| Rosin resin-alcohol ether phosphate ester compound/rosin resin | 80 | 140 | 110 | 80 | 80 | 80 | 80 | 80 | 140 |
| Molybdenum disulfide | 80 | 100 | 90 | 80 | 80 | 80 | 80 | 80 | 100 |
| Tert-butyl lithium/methyl tert-butyl ketone | / | / | / | 10 | 10 | / | / | 10 | 20 |
| Ethylene diamine/acetonitrile | / | / | / | 10 | 10 | / | / | 10 | 20 |
| Glycidyl methacrylate/ethyl acetate | / | / | / | / | 60 | / | / | 60 | 80 |
| Urea-formaldehyde resin/polyester resin | / | / | / | / | / | 30 | / | 30 | 50 |
| Fluorocarbon surface modifier/silane coupling agent | / | / | / | / | / | / | 4 | 4 | 6 |
| Ethanol | / | / | / | / | / | / | 20 | 20 | 30 |
TABLE 1-2 ingredient content table (unit: g)
| Example 10 | Example 11 | Example 12 | Example 13 | Example 14 | Example 15 | Comparative example 2 | Comparative example 3 | |
| Polytetrafluoroethylene suspension particles/polytetrafluoroethylene | 550 | 500 | 500 | 500 | 500 | 500 | 500 | 500 |
| Potassium titanate whisker | 170 | 200 | 200 | 200 | 200 | 200 | 200 | 200 |
| Glass fiber | 120 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| PEEK | 120 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| Rosin resin-alcohol ether phosphate ester compound/rosin resin | 110 | 80 | 80 | 80 | 80 | 80 | 80 | 80 |
| Molybdenum disulfide | 90 | 80 | 80 | 80 | 80 | 80 | 80 | 80 |
| Tert-butyl lithium/methyl tert-butyl ketone | 15 | 10 | 10 | 10 | / | / | / | / |
| Ethylene diamine/acetonitrile | 15 | 10 | 10 | 10 | / | / | / | / |
| Glycidyl methacrylate/ethyl acetate | 70 | / | / | 60 | / | / | / | / |
| Urea-formaldehyde resin/polyester resin | 40 | / | / | / | 30 | / | / | / |
| Fluorocarbon surface modifier/silane coupling agent | 5 | / | / | / | / | 4 | / | / |
| Ethanol | 25 | / | / | / | / | 20 | / | / |
Performance test
The mixed raw materials prepared according to the preparation methods of examples 1 to 15 and comparative examples 1 to 3 were compression molded to form test pieces having a specification of 100mm × 100mm × 30 mm.
(1) And (3) wear resistance test:
and (3) wear rate testing: the test pieces of examples 1-15 and comparative examples 1-3 were tested according to the standard GB/T3960-.
Testing the friction coefficient; the test pieces of examples 1, 6 and 14 were tested according to the standard GB/T3960-.
(2) Basic performance test:
and (3) testing tensile strength: the test pieces of examples 1 to 15 and comparative examples 1 to 3 were tested according to the standard GB/1040.2-2006 "determination of tensile Properties of plastics", test temperature: 23 ℃, test load: 20000N, test speed: 20 mm/min.
Tensile elongation test: the test pieces of examples 1 to 15 and comparative examples 1 to 3 were tested according to the standard GB/1040.2-2006 "determination of tensile Properties of plastics", test temperature: 23 ℃, test load: 20000N, test speed: 20 mm/min.
Flexural strength and flexural modulus test: the test pieces of examples 1 to 15 and comparative examples 1 to 3 were tested according to the standard GB/T9341-2008 "determination of Plastic flexural Properties", test temperature: 23 ℃, test load: 20000N, test speed: 20 mm/min.
And (3) testing impact strength: the test pieces of examples 1 to 15 and comparative examples 1 to 3 were tested according to the standard GB/T1843-2008 "determination of Plastic Izod impact Strength", test temperature: 23 ℃, impact energy: 2.75J, test speed: 10 mm/min.
TABLE 2 test results of examples and comparative examples
| Rate of wear/%) | Coefficient of friction | |
| Example 1 | 0.74 | 0.13 |
| Example 2 | 0.69 | / |
| Example 3 | 0.71 | / |
| Example 4 | 0.66 | / |
| Example 5 | 0.62 | / |
| Example 6 | 0.65 | 0.07 |
| Example 7 | 0.68 | / |
| Example 8 | 0.53 | / |
| Example 9 | 0.49 | / |
| Example 10 | 0.52 | / |
| Example 11 | 0.72 | / |
| Example 12 | 0.73 | / |
| Example 13 | 0.66 | / |
| Example 14 | 0.71 | 0.11 |
| Example 15 | 0.72 | / |
| Comparative example 1 | 0.86 | / |
| Comparative example 2 | 0.77 | / |
| Comparative example 3 | 0.81 | / |
The results of the basic performance tests on the coupons of examples 1-15 and comparative examples 1-3 are as follows: tensile strength (MPa): 218-; tensile elongation (%): 1.2-1.5; flexural strength/MPa: 330-345; flexural modulus (GPa): 16.1-16.8; impact strength (kJ/m 2): 49-53, and the test results all reach the qualified standard of the sealing ring.
In summary, the following conclusions can be drawn:
1. as can be seen by combining example 1 and comparative examples 1-2, and table 2, the use of the polytetrafluoroethylene suspension particles improves the wear resistance of the seal ring, possibly due to: the polytetrafluoroethylene suspended particles have better dispersibility, and can be mixed with other raw materials more uniformly, so that the polytetrafluoroethylene suspended particles are better.
2. As can be seen by combining example 1 and comparative example 3 with table 2, the addition of the rosin resin-alcohol ether phosphate ester compound improves the wear resistance of the seal ring, probably because: the rosin resin-alcohol ether phosphate ester compound is a viscous substance and is uniformly mixed with the polytetrafluoroethylene suspended particles, so that the polytetrafluoroethylene suspended particles are more tightly combined with other raw materials, the binding force between the raw materials is improved, and when the sealing ring body is impacted, the raw materials are not easy to peel off, so that the wear resistance of the sealing ring body is improved.
The compatibility of the rosin resin-alcohol ether phosphate compound and the PEEK is good, and after the rosin resin-alcohol ether phosphate compound is adhered to the surface of the polytetrafluoroethylene suspended particles, the compatibility between the PEEK and the polytetrafluoroethylene suspended particles is improved, so that the PEEK and the polytetrafluoroethylene suspended particles are mixed more uniformly, and the wear-resisting property of the sealing ring body is further improved.
3. As can be seen by combining examples 1, 4, 11-12 and Table 2, the co-addition of t-butyllithium and ethylenediamine improved the wear resistance of the seal ring, probably due to: tert-butyl lithium and ethylenediamine are mixed to form free radicals, the free radicals are substituted by F atoms on polytetrafluoroethylene suspended particles, and the tert-butyl radicals substitute the F atoms on the original polytetrafluoroethylene suspended particles, so that the polarity of the surface of the polytetrafluoroethylene suspended particles is improved, the adhesion force between the rosin resin-alcohol ether phosphate ester compound and the polytetrafluoroethylene suspended particles is stronger, the indirect improvement of the compatibility between PEEK and the polytetrafluoroethylene suspended particles is facilitated, and the wear resistance of the sealing ring body is better.
4. As can be seen from the combination of examples 1, 4-5, and 13 and table 2, the co-addition of t-butyllithium, ethylenediamine, and glycidyl methacrylate is advantageous for improving the wear resistance of the seal ring, probably because: after the free radical and F atoms on the polytetrafluoroethylene suspended particles are substituted, a carbon center free radical is formed at the position of removing F, the carbon center free radical causes glycidyl methacrylate and the polytetrafluoroethylene suspended particles to generate graft polymerization, the molecular weight of the polytetrafluoroethylene suspended particles is increased, the molecular attraction between the grafted polytetrafluoroethylene suspended particle molecules is increased, the binding force between the raw materials inside the sealing ring body is improved, the raw materials are more difficult to split or peel, and therefore the wear resistance of the sealing ring body is improved.
5. As can be seen from the combination of examples 1, 6 and 14 and table 2, the addition of urea-formaldehyde resin is beneficial to improve the wear resistance of the seal ring, which may be due to: urea-formaldehyde resin's surface tension is less than the raw materials system of sealing ring body, easily migrate to sealing ring body surface after mixing, because of urea-formaldehyde resin's surface tension is low, urea-formaldehyde resin can level gradually at sealing ring body surface, make sealing ring body surface more smooth, be favorable to reducing the coefficient of friction on sealing ring body surface, and reduced glass fiber and potassium titanate whisker protrusion in sealing ring body surface, lead to the condition that sealing ring body surface wear aggravates, thereby be favorable to improving the wearability of sealing ring body.
6. As can be seen from the combination of examples 1, 7, and 15 and table 2, the addition of the fluorocarbon surface modifier can improve the wear resistance of the seal ring, which may be due to: the potassium titanate whisker is modified by the fluorocarbon surface modifier, so that the surface energy of the potassium titanate whisker is reduced, the dispersibility of the potassium titanate whisker in raw materials is improved, the potassium titanate whisker and other raw materials are more uniformly mixed, the agglomeration of the potassium titanate whisker is reduced, and the wear resistance of the sealing ring body is indirectly improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The wear-resistant sealing ring comprises a sealing ring body and is characterized in that the sealing ring body comprises the following raw materials in parts by weight:
50-60 parts of polytetrafluoroethylene suspended particles;
15-20 parts of potassium titanate whisker;
10-14 parts of glass fiber;
10-14 parts of PEEK;
8-14 parts of rosin resin-alcohol ether phosphate ester compound;
8-10 parts of molybdenum disulfide.
2. The wear resistant seal ring of claim 1, wherein: the raw materials also comprise 1-2 parts of tert-butyl lithium and 1-2 parts of ethylenediamine by weight.
3. The wear resistant seal ring of claim 2, wherein: the raw material also comprises 6-8 parts of glycidyl methacrylate by weight.
4. The wear resistant seal ring of claim 1, wherein: the preparation method of the rosin resin-alcohol ether phosphate compound comprises the following steps of: heating 4-5 parts of rosin resin to 180 ℃ at 170 ℃ and stirring until the rosin resin is completely melted, adding 8-10 parts of alcohol ether phosphate and 0.1-0.2 part of zirconium oxide, stirring for reacting for 3-4h, and cooling to room temperature to obtain the rosin resin-alcohol ether phosphate compound.
5. The wear resistant seal ring of claim 1, wherein: the raw materials also comprise 3-5 parts of urea-formaldehyde resin according to parts by weight.
6. The wear resistant seal ring of claim 1, wherein: the raw materials also comprise 0.4 to 0.6 portion of fluorocarbon surface modifier and 2 to 3 portions of ethanol according to the weight portion.
7. A method for preparing a wear resistant seal ring according to any one of claims 1 to 6, comprising the steps of:
s1, mixing raw materials: uniformly stirring and mixing polytetrafluoroethylene suspended particles and a rosin resin-alcohol ether phosphate compound to prepare a mixture A, then stirring and melting PEEK at 340-350 ℃, adding the mixture A, uniformly stirring, adding potassium titanate whiskers, glass fibers and molybdenum disulfide, and uniformly stirring to prepare a mixed raw material;
s2, mould pressing and sintering: selecting an adaptive mold, injecting the mixed raw materials into the mold, putting the mold filled with the materials into an oven heated to 320 ℃ for heat preservation for 20-30min, taking out the mold filled with the materials, cooling to 160 ℃ for heat preservation, demolding, and cooling to room temperature to obtain the sealing ring body.
8. The method for preparing a wear-resistant seal ring according to claim 7, wherein: in the step S1, uniformly mixing epoxypropyl methacrylate and ethanol in a mass ratio of 1:4 to prepare a mixed solution;
mixing tert-butyl lithium and ethylenediamine uniformly, adding polytetrafluoroethylene suspended particles, and introducing N2Stirring and reacting at 0 ℃ for 30-40min, taking out polytetrafluoroethylene suspended particles, washing with tetrahydrofuran at 0 ℃ for 2-3 times, adding the polytetrafluoroethylene suspended particles into the mixed solution, stirring and reacting at 70-75 ℃ for 8-9h, washing with distilled water at 50-55 ℃, performing suction filtration, washing with absolute ethyl alcohol, performing suction filtration, washing with acetone, and performing suction filtration to obtain a product A;
uniformly stirring and mixing the fluorocarbon surface modifier and ethanol to obtain a mixture B, spraying the mixture B on the surface of the potassium titanate whisker, stirring for 5-8min, and drying at the temperature of 100-110 ℃ for 6-7h to obtain a product B;
and uniformly stirring and mixing the product A and the rosin resin-alcohol ether phosphate compound to obtain a mixture C, then stirring and melting the PEEK at the temperature of 340-350 ℃, adding the mixture C, uniformly stirring, adding the product B, the glass fiber and the molybdenum disulfide, uniformly stirring, cooling to the temperature of 150-170 ℃, adding the urea-formaldehyde resin, and uniformly stirring to obtain the mixed raw material.
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