CN104558984B - Organobentonite Modified PolytetrafluoroethylOil Oil Seal material - Google Patents

Organobentonite Modified PolytetrafluoroethylOil Oil Seal material Download PDF

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Publication number
CN104558984B
CN104558984B CN201410683186.5A CN201410683186A CN104558984B CN 104558984 B CN104558984 B CN 104558984B CN 201410683186 A CN201410683186 A CN 201410683186A CN 104558984 B CN104558984 B CN 104558984B
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organobentonite
oil sealing
ptfe
modified
minutes
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CN104558984A (en
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杨辉
汪海风
吴春春
阙永生
沈志成
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Zigong Innovation Center of Zhejiang University
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Zigong Innovation Center of Zhejiang University
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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
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • 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
    • C08K3/346Clay
    • 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
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • 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
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The present invention relates to automobile engine field of sealing technology, it is desirable to provide a kind of organobentonite Modified PolytetrafluoroethylOil Oil Seal material.The mass percent of each component in this oil sealing material: politef 85 95%;Organobentonite 5 15%;Organobentonite is with the cationic surfactant strand alkyl quaternary ammonium salts modified organobentonite obtained of R N (CH3) 3+, and the carbon number of its R group is not less than 10, and organobentonite interlamellar spacing d (001) is not less than 2nm.The invention have the advantages that the lipophile having had, close with PTFE polarity, therefore it is uniformly dispersed in PTFE, the composite property of preparation is stable;Bentonite is easily stripped into flaky nanometer structure, has nanometer potentiation to PTFE.Abrasion loss is low, and coefficient of friction is little, and mechanical property is good, does not ftractures, and do not wear and tear mating plate, can play well application in oil sealing field.

Description

Organobentonite Modified PolytetrafluoroethylOil Oil Seal material
Technical field
The invention belongs to automobile engine field of sealing technology, be specifically related to a kind of organobentonite Modified PolytetrafluoroethylOil Oil Seal material Material.
Background technology
Along with the fast development of auto industry, user is more and more higher to engine reliability, sealing requirements, and along with sending out Motivation degree of turning improves constantly, and the operating mode that its oil sealing used especially rotary shaft oil seal bears is the harshest.Tetrafluoro Ethylene oil sealing (PTFE oil sealing) is the product that a kind of technology content is higher, begins to grind the eighties in 20th century abroad System, and the most just it has been in the starting stage in China, but the most gradually apply on the most medium-to-high grade car.
Though the performance that polytetrafluoroethyloil oil seals has had, it is inappropriate for only preparing with pure PTFE, because pure PTFE Easy to wear, creep is big, if directly using it to manufacture oil sealing, then the oil seal lip processed is poor with the trackability of axle, It is difficult to meet high speed, high-power, the use requirement of heavy-duty diesel engine, needs the most in practice PTFE is filled out Fill modification.The most conventional filler is mainly glass fibre, MoS2, graphite powder etc., but, this filler changes Property the PTFE oil sealing material that obtains there is following defect: filler and PTFE polarity spectrum are relatively big, and filler is at PTFE Middle skewness, the composite property of preparation is unstable;Filler adding proportion is big, and oil sealing mechanical property is bad, Fragility is big, and poor toughness easily ftractures;Oil sealing coefficient of friction is big, big to mating plate abrasion, easily causes leakage.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, it is provided that a kind of organobentonite modification gathers Tetrafluoroethene oil sealing material.The present invention is to be modified PTFE using organobentonite as packing material, to strengthen PTFE anti-wear performance and creep-resistant property, develop high-performance PTFE oil sealing.
For solving technical problem, the solution of the present invention is:
The invention provides a kind of organobentonite Modified PolytetrafluoroethylOil Oil Seal material, the matter of each component in this oil sealing material Amount percentage ratio is as follows:
Politef 85-95%;Organobentonite 5-15%;
Described organobentonite is with cationic surfactant strand alkyl quaternary ammonium salts R-N (CH3)3 +Modified obtain Organobentonite, the carbon number of its R group be not less than 10, organobentonite interlamellar spacing d(001)Not less than 2nm.
In the present invention, described organobentonite is to be prepared by following method modification:
(1) the commercially available sodium bentonite of particle diameter≤44 μm is added to the water, makes the suspension that mass percent is 10%; Stir-activating 30 minutes under room temperature, make breeze fully dispersed in water;
(2) add hot suspension to 80 DEG C, add surfactant strand alkyl quaternary ammonium salts R-N (CH3)3 +, live in surface Property agent and bentonitic mass ratio be 5~10: 100;After reacting 90 minutes, it is cooled to room temperature;
(3) excessively filter water, make to be washed with deionized 3 times to gained solid, remove remaining surfactant;
(4) solid after washing is 105 DEG C of drying, grinds, i.e. obtains modified organobentonite.
In the present invention, the oil sealing abrasion loss≤6mg of described oil sealing material, coefficient of friction≤0.18, hot strength >=15MPa, Elongation at break >=150%.
In the present invention, the preparation method of described organobentonite modified ptfe oil sealing material, comprise the following steps:
Step one, organobentonite are modified:
(1) the commercially available sodium bentonite of particle diameter≤44 μm be added to the water make the suspension that mass percent is 10%, Stir-activating 30 minutes under room temperature, make breeze fully dispersed in water;
(2) add hot suspension to after 80 DEG C, add surfactant strand alkyl quaternary ammonium salts R-N (CH3)3 +, surface Activating agent and bentonitic mass ratio are 5~10: 100;After reacting 90 minutes, it is cooled to room temperature;
(3) excessively filter water, make to be washed with deionized 3 times to the solid filtering gained, alive to remove remaining surface Property agent;
(4) solid after washing is dried under the conditions of 105 DEG C, grinds, i.e. obtains modified organobentonite.
Prepared by step 2, PTFE oil sealing:
(1) according to mass percent relation be politef 85-95%, the requirement of organobentonite 5-15%, weigh Oil sealing material component puts into blender;Below 10 DEG C in ambient temperature, first stir 5 points by the speed of≤30 revs/min Clock, the rear speed by >=200 revs/min stirs 10 minutes, makes raw material mix homogeneously, avoids politef to tie simultaneously Group;
(2) batch mixing is joined in moulding press and carry out room temperature mold pressing, pressure 25~30MPa, dwell time 3~5 points Clock;
(3) batch mixing after molding is put in high temperature furnace and is sintered, and sintering process controls: room temperature to 330 DEG C intensification 5h, 330 DEG C of insulations 0.5h, 330 DEG C to 370 DEG C of intensification 1h, 370 DEG C of insulation 3h, 370 DEG C to 220 DEG C of cooling 4h, 220 DEG C Naturally cool to room temperature;
(4) moulding as required, uses lathe to be processed the composite after sintering, makes satisfactory Oil sealing material.
The present invention realizes principle:
Organobentonite is a kind of inorganic mineral/organic ammonium complex, with bentonite as raw material, utilizes montmorillonite in bentonite Lamellar structure and swelling in water or organic solvent can be dispersed into colloid cosmid characteristic, pass through ion exchange technique Insert organic coverture and make.At present, studying and apply most is with strand alkyl quaternary amine salt R-N (CH3)3 + The organobentonite obtained for the cationic surfactant modification represented, and according to quaternary ammonium salt cationic alkyl chain (R-) Length, organobentonite also can be divided into Long carbon chain organobentonite (surfactant R-base usually containing 10-, 12-, The alkyl chain of 14-, 16-, 18-carbon) and short carbon chain organobentonite (R-base is usually methyl, ethyl, phenyl, benzyl Deng) this two class.Long carbon chain organobentonite is longer due to alkyl chain, and gap softened between bentonite bed lamellar is the most relatively Greatly, therefore in actual application, this kind of bentonite is easily stripped into the lamellar bentonite structure of nano thickness, energy Its base material is played nanometer potentiation.
The organobentonite Modified PolytetrafluoroethylOil Oil Seal that the present invention provides, can be used for oil seal for automobile engine field.
Compared with prior art, the invention have the advantages that
(1) organobentonite of the present invention uses the R group carbon number quaternary ammonium salt (R-N (CH not less than 103)3 +) modified, The lipophile having had, close with PTFE polarity, therefore it is uniformly dispersed in PTFE, the composite property of preparation is steady Fixed;
(2) organobentonite of the present invention d between layers(001)Gap is relatively big (>=2nm), sinters at PTFE composite During, along with ablation and the melted infiltration of PTFE of Long carbon chain organic components, bentonite is easily stripped into nanometer sheet Shape structure, has nanometer potentiation to PTFE.
(3) organobentonite modified ptfe oil sealing abrasion loss of the present invention is low, and coefficient of friction is little, and mechanical property is good, no Cracking, do not wear and tear mating plate, can play well application in oil sealing field.
Detailed description of the invention
Embodiment 1
In organobentonite modified ptfe oil sealing material each component mass percent as follows:
Politef 95%;
Organobentonite 5%;
Wherein, organobentonite is with C-10 strand alkyl quaternary ammonium salts (C10H21-N(CH3)3 +) cationic surface work The organobentonite that property agent modification obtains.
The preparation method of organobentonite modified ptfe oil sealing material, comprises the following steps:
(1) organobentonite is modified:
A, commercially available sodium bentonite (particle diameter 44 μm) is made the suspension that mass percent is 10%, stir-activating 30 minutes, make breeze fully dispersed in water;B, add hot suspension to 80 DEG C, add C10H21-N(CH3)3 +Table Face activating agent (being 5:100 with bentonite mass ratio), after reacting 90 minutes, is cooled to room temperature;C, mistake filter water, Solid makes to be washed with deionized 3 times, removes remaining surfactant;D, 105 DEG C of drying solids, grind, be Organobentonite, bentonite bed spacing d(001)=2.51nm.
(2) prepared by organobentonite modified ptfe oil sealing:
A. according to recipe requirements, weigh a certain amount of PTFE and organobentonite is put in homogenizer, in less than 10 DEG C In ambient temperature, first stirring at low speed (30 revs/min) 5 minutes, rear high-speed stirred (200 revs/min) 10 minutes, make Raw material mix homogeneously, avoids PTFE conglomeration simultaneously;B, joining in moulding press by mixed powder body, room temperature molds, Pressure 25MPa, 3 minutes dwell times;C, by after mold pressing mix material put in high temperature furnace sinter, sintering process is: Room temperature to 330 DEG C intensification 5h, 330 DEG C of insulations 0.5h, 330 DEG C to 370 DEG C of intensification 1h, 370 DEG C of insulation 3h, 370 DEG C are arrived 220 DEG C of cooling 4h, 220 DEG C naturally cool to room temperature;PTFE composite is processed by d, use fine turning lathe, system The suitable oil sealing material required of standby one-tenth, its performance is:
Abrasion loss 6mg (GB/T 3960-1983), coefficient of friction 0.17 (GB/T 3960-1983), hot strength 25MPa (HGT 2902-1997), elongation at break 250% (HGT 2902-1997).
Embodiment 2
In organobentonite modified ptfe oil sealing material each component mass percent as follows:
Politef 90%;
Organobentonite 10%;
Wherein, organobentonite is with C-12 strand alkyl quaternary ammonium salts (C12H25-N(CH3)3 +) cationic surface work The class organobentonite that property agent modification obtains.
The preparation method of organobentonite modified ptfe oil sealing material, comprises the following steps:
(1) organobentonite is modified:
A, commercially available sodium bentonite (particle diameter 20 μm) is made the suspension that mass percent is 10%, stir-activating 30 minutes, make breeze fully dispersed in water;B, add hot suspension to 80 DEG C, add C12H25-N(CH3)3 +Table Face activating agent (being 8:100 with bentonite mass ratio), after reacting 90 minutes, is cooled to room temperature;C, mistake filter water, Solid makes to be washed with deionized 3 times, removes remaining surfactant;D, 105 DEG C of drying solids, grind, be Organobentonite, bentonite bed spacing d(001)=2.67nm.
(2) prepared by organobentonite modified ptfe oil sealing:
A. according to recipe requirements, weigh a certain amount of PTFE and organobentonite is put in homogenizer, in less than 10 DEG C In ambient temperature, first stirring at low speed (30 revs/min) 5 minutes, rear high-speed stirred (300 revs/min) 10 minutes, make Raw material mix homogeneously, avoids PTFE conglomeration simultaneously;B, joining in moulding press by mixed powder body, room temperature molds, Pressure 30MPa, 5 minutes dwell times;C, put in high temperature furnace sinter mixing material after good for mold pressing, sintering process For: room temperature to 330 DEG C intensification 5h, 330 DEG C of insulations 0.5h, 330 DEG C to 370 DEG C of intensification 1h, 370 DEG C of insulation 3h, 370 DEG C To 220 DEG C of cooling 4h, 220 DEG C naturally cool to room temperature;PTFE composite is processed by d, use fine turning lathe, Being prepared as the oil sealing material properly required, its performance is:
Abrasion loss 5.1mg (GB/T 3960-1983), coefficient of friction 0.18 (GB/T 3960-1983), hot strength 17MPa (HGT 2902-1997), elongation at break 185% (HGT 2902-1997).
Embodiment 3
In organobentonite modified ptfe oil sealing material each component mass percent as follows:
Politef 85%;
Organobentonite 15%;
Wherein, organobentonite is with C-16 strand alkyl quaternary ammonium salts (C18H37-N(CH3)3 +) be representative sun from The class organobentonite that sub-surface activating agent modification obtains.
The preparation method of organobentonite modified ptfe oil sealing material, comprises the following steps:
(1) organobentonite is modified:
A, commercially available sodium bentonite (particle diameter 15 μm) is made the suspension that mass percent is 10%, stir-activating 30 minutes, make breeze fully dispersed in water;B, add hot suspension to 80 DEG C, add C18H37-N(CH3)3 +Table Face activating agent (being 10:100 with bentonite mass ratio), after reacting 90 minutes, is cooled to room temperature;C, mistake filter water, Solid makes to be washed with deionized 3 times, removes remaining surfactant;D, 105 DEG C of drying solids, grind, be Organobentonite, bentonite bed spacing d(001)=2.88nm.
(2) prepared by organobentonite modified ptfe oil sealing:
A. according to recipe requirements, weigh a certain amount of PTFE and organobentonite is put in homogenizer, in less than 10 DEG C In ambient temperature, first stirring at low speed (30 revs/min) 5 minutes, rear high-speed stirred (300 revs/min) 10 minutes, make Raw material mix homogeneously, avoids PTFE conglomeration simultaneously;B, joining in moulding press by mixed powder body, room temperature molds, Pressure 28MPa, 4 minutes dwell times;C, put in high temperature furnace sinter mixing material after good for mold pressing, sintering process For: room temperature to 330 DEG C intensification 5h, 330 DEG C of insulations 0.5h, 330 DEG C to 370 DEG C of intensification 1h, 370 DEG C of insulation 3h, 370 DEG C To 220 DEG C of cooling 4h, 220 DEG C naturally cool to room temperature;PTFE composite is processed by d, use fine turning lathe, Being prepared as the oil sealing material properly required, its performance is:
Abrasion loss 4.2mg (GB/T 3960-1983), coefficient of friction 0.18 (GB/T 3960-1983), hot strength 15MPa (HGT 2902-1997), elongation at break 150% (HGT 2902-1997).
Organobentonite modified ptfe oil sealing material wear ability in the present invention is good, coefficient of friction is low, mechanical property is high. Verified below by correction data:
Comparative example 1
Preparation process is same as embodiment 1, and bentonite does not does modification.
After testing, the performance data of oil sealing material is as follows:
Interlamellar spacing d(001)=1.23nm, PTFE oil sealing material property is: abrasion loss 12.0mg (GB/T 3960-1983), Coefficient of friction 0.19 (GB/T 3960-1983), hot strength 20MPa (HGT 2902-1997), elongation at break 195% (HGT 2902-1997).
Comparative example 2
Preparation process is same as embodiment 2, and Bentonite modifier is C8H11-N(CH3)3 +Surfactant.
After testing, the performance data of oil sealing material is as follows:
Interlamellar spacing d(001)=1.81nm, PTFE oil sealing material property is: abrasion loss 8.1mg (GB/T 3960-1983), Coefficient of friction 0.21 (GB/T 3960-1983), hot strength 14MPa (HGT 2902-1997), elongation at break 138% (HGT 2902-1997).
Finally, listed above is only several specific embodiments of the present invention, it is clear that the invention is not restricted to above enforcement Example, it is also possible to have many deformation.Those of ordinary skill in the art can directly derive from present disclosure or associate The all deformation arrived, are all considered as protection scope of the present invention.

Claims (2)

1. an organobentonite Modified PolytetrafluoroethylOil Oil Seal material, it is characterised in that each component in this oil sealing material Mass percent as follows:
Politef 85-95%;
Organobentonite 5-15%;
Described organobentonite is with cationic surfactant strand alkyl quaternary ammonium salts R-N (CH3)3 +Modified obtain Organobentonite, the carbon number of its R group be not less than 10, organobentonite interlamellar spacing d(001)Not less than 2nm;
Described organobentonite is to be prepared by following method modification:
(1) the commercially available sodium bentonite of particle diameter≤44 μm is added to the water, makes the suspension that mass percent is 10%; Stir-activating 30 minutes under room temperature, make breeze fully dispersed in water;
(2) add hot suspension to 80 DEG C, add surfactant strand alkyl quaternary ammonium salts R-N (CH3)3 +, live in surface Property agent and bentonitic mass ratio be 5~10: 100;After reacting 90 minutes, it is cooled to room temperature;
(3) excessively filter water, make to be washed with deionized 3 times to gained solid, remove remaining surfactant;
(4) solid after washing is 105 DEG C of drying, grinds, i.e. obtains modified organobentonite;
When each for oil sealing material component is mixed: below 10 DEG C in ambient temperature, first stir by the speed of≤30 revs/min Mixing 5 minutes, the rear speed by >=200 revs/min stirs 10 minutes, makes raw material mix homogeneously, avoids polytetrafluoro simultaneously Ethylene conglomeration.
Organobentonite Modified PolytetrafluoroethylOil Oil Seal material the most according to claim 1, it is characterised in that institute State the oil sealing abrasion loss≤6mg of oil sealing material, coefficient of friction≤0.18, hot strength >=15MPa, elongation at break >= 150%.
CN201410683186.5A 2014-11-18 2014-11-24 Organobentonite Modified PolytetrafluoroethylOil Oil Seal material Active CN104558984B (en)

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CN2014106638834 2014-11-18
CN201410663883 2014-11-18
CN201410683186.5A CN104558984B (en) 2014-11-18 2014-11-24 Organobentonite Modified PolytetrafluoroethylOil Oil Seal material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105385078B (en) * 2015-11-23 2017-07-28 扬州天健机械制造有限公司 A kind of polyetetrafluoroethycomposition composition and preparation method thereof
JP6997173B2 (en) 2016-08-19 2022-01-17 ヘンケル・アクチェンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフト・アウフ・アクチェン Method for manufacturing hydrophobically modified clay

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
纳米蒙脱石填充PTFE和UHMWPE的摩擦磨损性能;甄明晖等;《材料科学与工程学报》;20060630;第24卷(第3期);第410-413页 *
蒙脱土有机插层改性及其插层性能;廖丽丽等;《广东化工》;20111025;第38卷(第10期);第7-8、51页 *

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