CN108299786A - A kind of high temperature resistant self-lubricating sealing material and preparation method thereof - Google Patents
A kind of high temperature resistant self-lubricating sealing material and preparation method thereof Download PDFInfo
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- CN108299786A CN108299786A CN201810025806.4A CN201810025806A CN108299786A CN 108299786 A CN108299786 A CN 108299786A CN 201810025806 A CN201810025806 A CN 201810025806A CN 108299786 A CN108299786 A CN 108299786A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention belongs to sealing material fields, and in particular to arrive a kind of high temperature resistant self-lubricating sealing material and preparation method thereof.The sealing material is prepared by following raw material：60 parts of phenolic resin, 9 parts of nitrile rubber, 20 parts of polysiloxane, 4 parts of zinc oxide, 50 parts of soft graphite, 5 parts of brass powder, 1 part of butanone.The present invention is in high temperature resistant prepared by copolyreaction, high-adhesion phenolic aldehyde-organosilicon copolymerization adhesive, the sealing material prepared by the coordinated effect of each raw material, not only with high temperature resistance but also with higher mechanical strength, excellent self lubricity, wearability, ageing resistance.Suitable for large reciprocating compressor piston ring and piston rod packing letter filler, it can also be used to the washer of elevated temperature vessel connecting portion.
Description
Technical field
The invention belongs to sealing material fields, and in particular to arrive a kind of high temperature resistant self-lubricating sealing material and its preparation side
Method.
Technical background
Compressor is in ammonia synthesizing industry and other chemical industry extensive uses, the sealed letter filler and piston ring of piston rod
Majority uses cast steel material, and filling pump is needed ceaselessly to inject lubricating oil.From the eighties in last century, the material of low pressure stage sealing ring
Generally substituted with intefused tetratiuorine ethylene or PEK materials.It is gradually found in long-term actual application, filled polytetrafluoroethylene
Piston ring made of material and piston rod packing letter filler, just become soft and deformed, it is necessary to replace immediately at 180 DEG C or so.Often at present
160~170 DEG C of 1~6 temperature cylinder of large reciprocating compressor normal operating condition.Such as cylinder wall, piston ring groove or work
It is slightly improper that stopper rod is slightly distorted or operates, and cylinder temperature reaches 180 DEG C or more at once, and piston ring and sealed letter filler is caused to become
Shape is forced parking maintenance.Critical issue is existing intefused tetratiuorine vinyl material not only poor heat resistance, and wear-resisting property is also poor,
Service life is short, and normal condition operation must be replaced primary less than 3 months.It is the resistance to of polytetrafluoroethylene (PTFE) itself to analyze its reason one
Hot, bonding force difference, does not have lubricity；Second is that filler formulation owes reasonable, the filling polytetrafluoro material high temperature resistance of preparation
It is poor with wear-resisting property, it is processed into piston ring and packing seal element is fragile, short life, the cycle of operation are short, influence to produce.Therefore it grinds
It is very must to study carefully a kind of Compressor Piston Ring and sealed letter filler high temperature resistant, wear-resistant, long lifespan sealing material of can be suitably used for
It wants.
Invention content
The object of the present invention is to provide a kind of high temperature resistant suitable for compressor piston rod sealed letter filler and piston ring from
Lubricate sealing material.
The present invention also provides a kind of preparation methods of above-mentioned high temperature resistant self-lubricating sealing material.
To achieve the above object, this invention takes the following technical solutions：
The present invention provides a kind of high temperature resistant self-lubricating sealing materials, are prepared by following raw material：Phenolic resin
60 parts, 9 parts of nitrile rubber, 20 parts of polysiloxane, 4 parts of zinc oxide, 50 parts of soft graphite, 5 parts of brass powder, butanone
1 part.
Further, the granularity of the soft graphite and brass powder is 200 mesh.
The present invention also provides a kind of preparation methods of high temperature resistant self-lubricating sealing material, include the following steps：
（1）It takes in the phenolic resin and butanone input reaction kettle of parts by weight, under constant stirring, slowly heats up, be added poly- organic
Siloxanes, zinc oxide and imidazolidinyl urea, stir evenly, and carry out copolyreaction；After reaction, cool down, nitrile rubber be added,
Soft graphite, brass powder is added, is uniformly mixed, obtains colloid；
（2）By step（1）Triethanolamine and sodium tripolyphosphate are added in the colloid of preparation, insulated and stirred is uniform, is keeping temperature
With keep stirring down, material is sent into screw extruder with enclosed screw rod conveyer, cylinder blank is squeezed into, through cooling
Molding is fully cured.
Further, step（1）In, the copolyreaction is the insulation reaction 1h at 210~220 DEG C.
Further, after the copolyreaction, 160 DEG C is cooled to, nitrile rubber is then added.
Further, the phenolic resin is 30 with the mass ratio of imidazolidinyl urea：1.
Further, step（2）In, the triethanolamine is 1 with the mass ratio of phenolic resin：60.
Further, step（2）In, the mass ratio of the triethanolamine and sodium tripolyphosphate is 1：0.2.
Further, step（2）In, the uniform temperature of insulated and stirred is 150 DEG C.
High temperature resistant self-lubricating sealing material prepared by the present invention, is mainly used for large reciprocating compressor piston ring and piston
Bar sealed letter filler, changing formula can be used for the gasket of elevated temperature vessel connecting portion.Piston ring for reciprocating compressor
Or when piston rod packing letter filler, the blank of extrusion forming is subjected to refined processing with numerically controlled lathe before assembly, is machined to institute
The size needed, accuracy error is in 0.05~0.1mm.When for elevated temperature vessel washer, the soft graphite in formula is changed to
Acid-washed asbestos, to increase its extension strength, copper powder is changed to porcelain powder, to increase its compressive resistance, can directly be pressed with friction press
Type is made.
The present invention distinguishing feature be：
（1）In the high temperature resistant of copolyreaction preparation, high-adhesion phenolic aldehyde-organosilicon copolymerization adhesive, pass through the association of each raw material
With sealing material prepared by mating reaction, not only with high temperature resistance but also with higher mechanical strength, excellent profit certainly
Slip, wearability, ageing resistance.Suitable for large reciprocating compressor piston ring and piston rod packing letter filler, it can also be used to
The washer of elevated temperature vessel connecting portion；
（2）For the present invention by the preparation method, the copolymer the copolymerization rate of preparation is high, simple for process and easy to automate.
Specific implementation mode
A kind of preparation method of high temperature resistant self-lubricating sealing material of the present invention is made into one below by specific embodiment
Walk explanation.
Embodiment 1
A kind of preparation method of high temperature resistant self-lubricating sealing material, steps are as follows：
（1）It takes in the liquid phenolic resin and 1 part of butanone input reaction kettle of 60 mass parts, steam is passed through into reacting kettle jacketing,
Material is warming up to 210~220 DEG C in kettle, under constant stirring,（150~200r/min of rotating speed）It is slowly injected into the poly- of 20 mass parts
Organosiloxane adds the zinc oxide of 4 mass parts and the imidazolidinyl urea of 2 mass parts, is uniformly mixed, and keeps the temperature 1 hour
Carry out polymerisation；It is cooled to 160 DEG C after reaction, the nitrile rubber of 9 mass parts, the soft graphite of 50 mass parts is added
（200 mesh）, 5 mass parts brass powder（200 mesh）, it is uniformly mixed, obtains copolymerization colloid；
（2）It will be copolymerized the sodium tripolyphosphate that 1 mass parts triethanolamine and 0.2 mass parts is added in colloid, keeps the temperature and stir at 150 DEG C
It mixes uniformly, colloid is discharged into closed screw conveyor from reactor bottom drain hole, by closed screw conveyor by colloid substances
Material be sent into extrusion forming machine inlet, under the conditions of 0.2MPa, material screw rod promotion under by ring mould at cylinder, can
To replace the mold of different size according to required size, then cures through cold water spray, cooling and be made for reciprocating compression
The embryo material of machine piston ring or piston rod packing letter filler；
（3）When for piston of reciprocating compressor ring or piston rod packing letter filler, by step（2）The cylinder of extrusion forming
Embryo material is put in piston ring or sealed letter filler that numerically-controlled machine tool turning refined or be ground into required size, machining accuracy deviation
Less than 0.05~0.1mm.
Comparative example 1
A kind of preparation method of high temperature resistant self-lubricating sealing material, steps are as follows：
（1）It takes in the liquid phenolic resin and 1 part of butanone input reaction kettle of 60 mass parts, steam is passed through into reacting kettle jacketing,
Material is warming up to 210~220 DEG C in kettle, under constant stirring,（150~200r/min of rotating speed）It is slowly injected into the poly- of 20 mass parts
Organosiloxane adds the zinc oxide of 4 mass parts, the imidazolidinyl urea of 2 mass parts, the nitrile rubber of 9 mass parts, 50 mass
The soft graphite of part（200 mesh）, 5 mass parts brass powder（200 mesh）, it is uniformly mixed, heat preservation carries out polymerizeing anti-for 1 hour
It answers, obtains copolymerization colloid；
（2）The sodium tripolyphosphate that 1 mass parts triethanolamine and 0.2 mass parts is added in colloid, the degree of heat preservation at 150 DEG C will be copolymerized
It stirs evenly, colloid is discharged into closed screw conveyor from reactor bottom drain hole, by closed screw conveyor by colloid
Material is sent into extrusion forming machine inlet, under the conditions of 0.2MPa, material under screw rod promotion by ring mould at cylinder,
The mold of different size can be replaced according to required size, then is made for reciprocating pressure through cold water spray, cooling solidification
The embryo material of contracting machine piston ring or piston rod packing letter filler；
（3）When for piston of reciprocating compressor ring or piston rod packing letter filler, by step（2）The cylinder of extrusion forming
Embryo material is put in piston ring or sealed letter filler that numerically-controlled machine tool turning refined or be ground into required size, machining accuracy deviation
Less than 0.05~0.1mm.
Comparative example 2
A kind of preparation method of high temperature resistant self-lubricating sealing material, steps are as follows：
（1）It takes in the liquid phenolic resin and 1 part of butanone input reaction kettle of 60 mass parts, steam is passed through into reacting kettle jacketing,
Material is warming up to 210~220 DEG C in kettle, under constant stirring,（150~200r/min of rotating speed）It is slowly injected into the poly- of 20 mass parts
Organosiloxane adds the zinc oxide of 4 mass parts, is uniformly mixed, and keeps the temperature 1 hour and carries out polymerisation；Reaction terminates
After be cooled to 160 DEG C, the nitrile rubber of 9 mass parts, the soft graphite of 50 mass parts is added（200 mesh）, 5 mass parts brass powder
（200 mesh）, it is uniformly mixed, obtains copolymerization colloid；
（2）1 mass parts triethanolamine and 0.2 mass parts sodium tripolyphosphate, the insulated and stirred at 150 DEG C will be added in copolymerization colloid
Uniformly, colloid is discharged into closed screw conveyor from reactor bottom drain hole, by closed screw conveyor by colloid material
Be sent into extrusion forming machine inlet, under the conditions of 0.2MPa, material under screw rod promotion by ring mould at cylinder, can be with
The mold of different size is replaced according to required size, then is made for reciprocating compressor through cold water spray, cooling solidification
The embryo material of piston ring or piston rod packing letter filler；
（3）When for piston of reciprocating compressor ring or piston rod packing letter filler, by step（2）The cylinder of extrusion forming
Embryo material is put in piston ring or sealed letter filler that numerically-controlled machine tool turning refined or be ground into required size, machining accuracy deviation
Less than 0.05~0.1mm.
Comparative example 3
A kind of preparation method of high temperature resistant self-lubricating sealing material, steps are as follows：
（1）It takes in the liquid phenolic resin and 1 part of butanone input reaction kettle of 60 mass parts, steam is passed through into reacting kettle jacketing,
Material is warming up to 210~220 DEG C in kettle, under constant stirring,（150~200r/min of rotating speed）It is slowly injected into the poly- of 20 mass parts
Organosiloxane adds the zinc oxide of 4 mass parts and the imidazolidinyl urea of 2 mass parts, is uniformly mixed, and keeps the temperature 1 hour
Carry out polymerisation；It is cooled to 160 DEG C after reaction, the nitrile rubber of 9 mass parts, the soft graphite of 50 mass parts is added
（200 mesh）, 5 mass parts brass powder（200 mesh）, it is uniformly mixed, obtains copolymerization colloid；
（2）1 mass parts triethanolamine will be added in copolymerization colloid, insulated and stirred is uniform at 150 DEG C, and colloid is from reactor bottom
Drain hole is discharged into closed screw conveyor, and colloid material is sent into extrusion forming machine inlet by closed screw conveyor,
Under the conditions of 0.2MPa, material screw rod promotion under by ring mould at cylinder, can be replaced according to required size
The mold of different size, then be made for piston of reciprocating compressor ring or piston rod packing letter through cold water spray, cooling solidification
The embryo material of filler；
（3）When for piston of reciprocating compressor ring or piston rod packing letter filler, by step（2）The cylinder of extrusion forming
Embryo material is put in piston ring or sealed letter filler that numerically-controlled machine tool turning refined or be ground into required size, machining accuracy deviation
Less than 0.05~0.1mm.
（One）Material prepared by embodiment and comparative example is in the detection of 80 DEG C, 120 DEG C, 160 DEG C progress mechanical properties, tool
Body the results are shown in Table 1.
Table 1
（Two）Immersion oil experiment is carried out when sealing material prepared by embodiment and comparative example is used as washer（It is impregnated at 100 DEG C
48h）, meanwhile, carry out air oven aging test（At 200 DEG C, 200h）, then detect its variation in tensile strength and extension at break
Rate change rate, concrete outcome are shown in Table 2.
Tensile strength-initial tensile strength/initial Kang Qiang Du ╳ 100% after variation in tensile strength=experiment；
Elongation at break-initial elongation at break rate/initial elongation at break Shuai ╳ 100% after elongation at break change rate=experiment；
Table 2
Claims (9)
1. a kind of high temperature resistant self-lubricating sealing material, which is characterized in that be prepared by following raw material：Phenolic resin
60 parts, 9 parts of nitrile rubber, 20 parts of polysiloxane, 4 parts of zinc oxide, 50 parts of soft graphite, 5 parts of brass powder, butanone
1 part.
2. high temperature resistant self-lubricating sealing material according to claim 1, which is characterized in that the soft graphite and brass powder
Granularity be 200 mesh.
3. a kind of preparation method of high temperature resistant self-lubricating sealing material as claimed in claim 1 or 2, which is characterized in that including
Following steps：
（1）It takes in the phenolic resin and butanone input reaction kettle of parts by weight, under constant stirring, slowly heats up, be added poly- organic
Siloxanes, zinc oxide and imidazolidinyl urea, stir evenly, and carry out copolyreaction；After reaction, cool down, nitrile rubber be added,
Soft graphite, brass powder is added, is uniformly mixed, obtains colloid；
（2）By step（1）Triethanolamine and sodium tripolyphosphate are added in the colloid of preparation, insulated and stirred is uniform, is keeping temperature
With keep stirring down, material is sent into screw extruder with enclosed screw rod conveyer, cylinder blank is squeezed into, through cooling
Molding is fully cured.
4. preparation method according to claim 3, which is characterized in that step（1）In, the copolyreaction be 210~
At 220 DEG C, insulation reaction 1h.
5. preparation method according to claim 4, which is characterized in that after the copolyreaction, 160 DEG C are cooled to,
Then nitrile rubber is added.
6. preparation method according to claim 3, which is characterized in that mass ratio of the phenolic resin with imidazolidinyl urea
It is 30：1.
7. preparation method according to claim 3, which is characterized in that step（2）In, the same phenolic resin of triethanolamine
Mass ratio be 1：60.
8. the preparation method according to claim 3 or 7, which is characterized in that step（2）In, the triethanolamine and trimerization
The mass ratio of sodium phosphate is 1：0.2.
9. preparation method according to claim 8, which is characterized in that step（2）In, the uniform temperature of insulated and stirred
It is 150 DEG C.
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| JPS6030157A (en) * | 1983-07-29 | 1985-02-15 | Toshiba Chem Corp | Resin seal type semiconductor device |
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| CN105602189A (en) * | 2014-11-03 | 2016-05-25 | 袁辉 | Laminated plate having adhesion resistance |
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2018
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|---|---|---|---|---|
| JPS6030157A (en) * | 1983-07-29 | 1985-02-15 | Toshiba Chem Corp | Resin seal type semiconductor device |
| CN103173175A (en) * | 2013-03-23 | 2013-06-26 | 广东新展化工新材料有限公司 | Organic silicone modified epoxy resin sealant and preparation method thereof |
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| CN105602189A (en) * | 2014-11-03 | 2016-05-25 | 袁辉 | Laminated plate having adhesion resistance |
| CN105647108A (en) * | 2016-03-30 | 2016-06-08 | 西安交通大学 | Siloxane-modified phenolic resin for hot melt preimpregnation technology and preparation method of siloxane-modified phenolic resin for hot melt preimpregnation technology |
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| CN106700154A (en) * | 2017-01-18 | 2017-05-24 | 长春蓝天密封技术开发有限公司 | Graphite sealing material and preparation method thereof |
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