CN1083479C - High-temp. dry film lubricant - Google Patents

High-temp. dry film lubricant Download PDF

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Publication number
CN1083479C
CN1083479C CN97118738A CN97118738A CN1083479C CN 1083479 C CN1083479 C CN 1083479C CN 97118738 A CN97118738 A CN 97118738A CN 97118738 A CN97118738 A CN 97118738A CN 1083479 C CN1083479 C CN 1083479C
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film lubricant
dry
high temperature
lubricant
present
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CN1212284A (en
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胡丽天
冶银平
陈建敏
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

The present invention relates to a bonding high-temperature dry film lubricant of half inorganic-organic resin. An adoptive adhesive is half inorganic-organic resin polysiloxane-phenolic epoxy resin, a lubricant is graphite, and a metallic oxide is adopted as an antiwear additive. The high-temperature dry film lubricant can be used for a long time under the condition of indoor temperature to 300DEG C and be used for a short time under the condition of 400DEG C, and the present invention can be used for positions, such as ten-level trays of an aerial engine high-pressure compressor, high-pressure rear axle fixed flange nozzle liners, accessory air-core pumps, etc., and the surfaces of other parts used under high temperature conditions; the present invention solves the problems of lubrication and wear-out failure at high temperature.

Description

High temperature resistant dry-film lubricant
The present invention is a kind of half inorganic-organic resin high temperature resistant dry-film lubricant that bonds, this high temperature resistant dry-film lubricant can be under the condition of room temperature~300 ℃ life-time service, 400 ℃ of following short-terms are used.
Dry-film lubricant is a kind of of solid lubrication, and it is to utilize tackiness agent that pulverous solid lubricant (as molybdenumdisulphide, graphite, tetrafluoroethylene etc.) and other filler are sticked on the metal substrate, thereby plays lubricated effect.The tackiness agent that is adopted can be the organic resin of natural or synthetic, also can be mineral compound.In general, the dry-film lubricant that adopts organic resin to make as tackiness agent, its sticking power, snappiness, shock resistance, preservative property and solvent resistance are better, frictional coefficient is low, but resistance to elevated temperatures is relatively poor, and when (>250 ℃) used under higher temperature, above-mentioned performance all can reduce significantly, this is because organic resin oxidation at high temperature or degraded cause organic resin agglutinating dry-film lubricant degradation.For example a kind of dry-film lubricant of Chinese patent (CN1031801C) description is a binding agent with polymeric amide-imide, and tetrafluoroethylene is a lubricant, PbO, Pb 3O 4, Cu 2O, fluorographite, MoS 2Be wear preventive additive, wear resistance and oilness are preferably arranged at normal temperatures, but after temperature is elevated to 300 ℃, descended 95% friction durability.So organic resin agglutinating dry-film lubricant (uses under<250 ℃=envrionment conditions at middle low temperature, can solve lubrication problem effectively, when use temperature is higher (>250 ℃), needing to adopt with the mineral compound is the inorganic bond dry-film lubricant of tackiness agent.The advantage of inorganic bond dry-film lubricant is that resistance to elevated temperatures is good, can use down in higher temperature (>300 ℃), but its wear resistance, snappiness, shock resistance, preservative property and solvent resistance is all poor than organic binding dry film lubricant.According to " solid wear-resistant material " report be binding agent with silicate, MoS 2Be the inorganic bond dry-film lubricant of lubricant, can use under 400 ℃ temperature, but have only 167m/um its friction durability, frictional coefficient is up to 0.20.
Given this, the objective of the invention is to utilize a kind of half inorganic-organic resin as tackiness agent, a kind of both had good adhesion, snappiness, shock resistance, preservative property and solvent resistance are provided, has resistance to elevated temperatures preferably again, can be under the condition of room temperature~300 ℃ life-time service, the dry-film lubricant that short-term is used under 400 ℃ the condition.
Purpose of the present invention can realize by following measure:
The high temperature resistant dry-film lubricant of the present invention is made up of tackiness agent, lubricant, wear preventive additive and mixed solvent, and its weight percentage consists of:
Tackiness agent 10-25
Graphite 3-15
Antimonous oxide 1-5
The mixed solvent surplus.Wherein tackiness agent is a kind of half inorganic-organic resin polysiloxane-novolac epoxy, and its structural formula is as follows:
Figure C9711873800051
M=200~250 n=10~50.
Its synthetic method is: novolac epoxy adds acetone makes it dissolving, adds polysiloxane then, and the weight ratio of novolac epoxy and polysiloxane is 1: 5, mixes, and heated and stirred 4 hours, temperature are controlled at 70-80 ℃.
The structural unit of novolac epoxy of the present invention is formula (II):
m=200~250
(II) structure of the polysiloxane that is adopted is formula (III):
n=10~50
(III)
The oxirane value of novolac epoxy of the present invention is 0.44 equivalent/100 grams, and it has good adhesive, snappiness, shock resistance, preservative property and solvent resistance.
Polysiloxane of the present invention be with-the Si-O-key is a main chain, methyl and oxyethyl group are side chain, hydroxy-end capped polymkeric substance, it has both the dual characteristics of organic materials and inorganic materials, and is big as molecular weight, sticking power a little less than, fragility is big, not shock-resistant, characteristics such as high temperature resistant, a kind of half inorganic materials of being known as.This polysiloxane can for a long time anti-360 ℃ temperature.
Characteristics of the present invention are that with this polysiloxane and novolac epoxy synthetic half inorganic-organic resin be the dry-film lubricant of tackiness agent, owing to contain soft segment-OCH simultaneously in its tackiness agent 2CH-and high bond energy-the Si-O-bond structure, make dry film not only have good adhesive, snappiness, shock resistance, preservative property and solvent resistance, and have a great high-temperature resistant, can be under 300 ℃ temperature life-time service, short-term is used under 400 ℃ the temperature.
Lubricant of the present invention is that purity is 99.85% graphite.
Wear preventive additive of the present invention is that granularity is 45~53 microns a antimonous oxide.
Solvent of the present invention is a mixed solvent, and its weight percentage consists of:
Acetone 10-20
Butanone 20-30
Toluene 20-30
Ethylene glycol monomethyl ether 20-30.
Preparation method of the present invention is: solid lubricant and wear preventive additive are pressed the said mixed of the present invention, put into ball grinder, the mixed solvent that adds 2~3 times of amount of solid, grind, carry out Ball milling, add tackiness agent afterwards, press simultaneously formula ratio again and add mixed solvent, grind, filter then, gained filtrate is the dry-film lubricant spray.With spray gun the dry-film lubricant spray that makes is sprayed on piece surface under the pressurized air (dewatering, do not have oil) of cleaning or compressed nitrogen.Piece surface needs oil removing in advance, rust cleaning, in order to increase the roughness of sprayed surface, can spray the piece surface blast of dry-film lubricant at need.The part that has sprayed dry-film lubricant is placed in the baking oven, and baking is 1.5 hours under 180 ℃ temperature, and is promptly curable.
The data of table 1 are to estimate the wear resistance of the high temperature resistant dry-film lubricant of the present invention under differing temps on bolt-disc type high temperature friction and wear trier.Dry film is coated on the dish that material is 1Cr18Ni9Ti, and dish is of a size of φ 45mm * 10mm; The material of friction pair bolt is identical with dish, is of a size of φ 5mm * 18mm.
The wear resistance of the high temperature resistant dry-film lubricant of table 1. the present invention
Test temperature (℃) 25 300 400
Wear resistance (rice/micron) 486 358 206
Annotate: test load 50N, rotating speed 800 changes
The result of table 1 shows that the high temperature resistant dry-film lubricant of the present invention has long friction durability in the time of 300 ℃, still possess certain wear resistance in the time of 400 ℃.And the high temperature resistant dry-film lubricant of the present invention can prevent intermetallic sintering, scribbles the dish of 1Cr18Ni9Ti of dry film of the present invention and bolt 600 ℃ of following calcinations, also can not stick together because of sintering.
Other physicochemical property of dry film of the present invention is listed in table 2.
The physicochemical property of the high temperature resistant dry-film lubricant of table 2. the present invention
Numbering Project Detection method The result
1 Viscosity Be coated with-4 glasss 11 seconds
2 The dry film snappiness GB1731-79 1mm
3 The dry film resistance to impact shock GB1732-79 50Kg.cm
4 The dry film adhesivity GB17320-79 One-level
5 The dry film thermotolerance 300 ℃ of calcinations 100 hours Above-mentioned 2,3,4 performances do not reduce
6 The dry film solvent resistance (1) 4611 hydraulic efficiency oil room temperature was soaked 100 hours; (2) the RP-3 fuel oil soaked 100 hours for 70 ℃; (3) 4050 aircraft oils soaked 100 hours for 150 ℃ Above-mentioned 2,3,4 performances do not reduce
Result as table 2 is indicated, the high temperature resistant dry-film lubricant of the present invention not only has good flexible, adhesivity and resistance to impact shock at ambient temperature, and with this dry film 300 ℃ of following calcinations after 100 hours, above-mentioned these performances are all less than reducing.
The part that scribbles this dry film soaked the regular hour under the differing temps respectively in 4611 hydraulic efficiency oil, RP-3 fuel oil and 4050 aircraft oils after, dry film does not only have variable color, feels like jelly, bubbles, comes off, and has still kept good snappiness, adhesivity and resistance to impact shock.
The result of associative list 1 and table 2, show that the high temperature resistant dry-film lubricant of the present invention not only can play good lubrication at ambient temperature, and when having 4611 hydraulic efficiency oil, RP-3 fuel oil and 4050 aircraft oils to exist, still can be well attached to piece surface, play lubrication, especially, under comparatively high temps (300~400 ℃) condition, dry-film lubricant of the present invention possesses long friction durability, can play lubricated effectively and prevents the agglomerating effect.
The high temperature resistant dry-film lubricant of the present invention can be realized by following embodiment:
Example 1. takes by weighing 6.5 parts of graphite and 4.5 parts of antimonous oxides, adds 33 parts of mixed solvents, grinds and disperses.Consisting of of mixed solvent: 18 parts in acetone, 26 parts of butanone, 30 parts of toluene, 26 parts of ethylene glycol monomethyl ether.Take by weighing 21 parts of tackiness agent, after 35 parts of mixed solvent dilutions, add in the above-mentioned grinding dispersive material, continue to grind, up to being uniformly dispersed, filter, gained filtrate is the dry-film lubricant spray.With spray gun the dry-film lubricant spray that makes is sprayed on piece surface under the pressurized air (dewatering, do not have oil) of cleaning or compressed nitrogen.Piece surface need be used sand papering in advance, and organic solvent cleans, to remove the rust staining and the greasy dirt on surface.The part that has sprayed dry-film lubricant is placed in the baking oven, and baking is 1.5 hours under 180 ℃ temperature, and is promptly curable.
Each component concentration of example 2. mixed solvents is with example 1, and other component prescription is as table 3.
Table 3:
Sequence number Tackiness agent Graphite Antimonous oxide Mixed solvent
1 12 5 3 80
2 16 5.5 3.5 75
3 19 6 4 71
4 23 7 5 65
5 24 8 5 63

Claims (5)

1. high temperature resistant dry-film lubricant, can be under the condition of room temperature~300 ℃ life-time service, its weight percentage consists of:
Tackiness agent 10-25
Graphite 3-15
Antimonous oxide 1-5
The mixed solvent surplus.
2. high temperature resistant dry-film lubricant as claimed in claim 1 is characterized in that tackiness agent is half inorganic-organic resin polysiloxane-novolac epoxy, and its structural formula is (I):
Figure C9711873800021
M=200~250 n=10~50 wherein.
(I)
3. high temperature resistant dry-film lubricant as claimed in claim 1, the granularity that it is characterized in that antimonous oxide is 45~53 microns.
4. high temperature resistant dry-film lubricant as claimed in claim 1 is characterized in that the mixed solvent weight percentage consists of:
Acetone 10-20
Butanone 20-30
Toluene 20-30
Ethylene glycol monomethyl ether 20-30.
5. high temperature resistant dry-film lubricant as claimed in claim 1 or 2, the synthetic method that it is characterized in that formula (I) half inorganic-organic resin polysiloxane-novolac epoxy is the novolac epoxy of formula (II), add acetone and make it dissolving, the polysiloxane that adds formula (III) then, the weight ratio of novolac epoxy and polysiloxane is 1: 5, mixes heated and stirred 4 hours, temperature is controlled at 70-80 ℃
Figure C9711873800031
m=200~250
(II)
n=10~50。
(III)
CN97118738A 1997-09-25 1997-09-25 High-temp. dry film lubricant Expired - Fee Related CN1083479C (en)

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CN1083479C true CN1083479C (en) 2002-04-24

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101870910B (en) * 2010-06-23 2013-02-20 河南省长城特种润滑脂有限公司 High temperature exposed gear grease and preparation method thereof
CN103059304B (en) * 2012-12-21 2015-02-18 海洋化工研究院有限公司 Preparation and application of long-acting anticorrosion temperature-resistant coating
CN106634392B (en) * 2016-11-22 2019-10-22 中国航发沈阳黎明航空发动机有限责任公司 A kind of high temperature lubricating graphite preparation and its preparation method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1120579A (en) * 1994-10-08 1996-04-17 中国科学院兰州化学物理研究所 Single component long-acting dry film lubricant
CN1120580A (en) * 1994-10-08 1996-04-17 中国科学院兰州化学物理研究所 Solvent-free dry film lubricant
CN1149074A (en) * 1995-04-07 1997-05-07 中国科学院兰州化学物理研究所 Dust-proof dried film lubricant cured at normal atmospheric temperature

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1120579A (en) * 1994-10-08 1996-04-17 中国科学院兰州化学物理研究所 Single component long-acting dry film lubricant
CN1120580A (en) * 1994-10-08 1996-04-17 中国科学院兰州化学物理研究所 Solvent-free dry film lubricant
CN1149074A (en) * 1995-04-07 1997-05-07 中国科学院兰州化学物理研究所 Dust-proof dried film lubricant cured at normal atmospheric temperature

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