CN108676210A - A kind of processing method of low temperature resistant oil proof type rubber seal - Google Patents
A kind of processing method of low temperature resistant oil proof type rubber seal Download PDFInfo
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- CN108676210A CN108676210A CN201810416263.9A CN201810416263A CN108676210A CN 108676210 A CN108676210 A CN 108676210A CN 201810416263 A CN201810416263 A CN 201810416263A CN 108676210 A CN108676210 A CN 108676210A
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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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D99/00—Subject matter not provided for in other groups of this subclass
- B29D99/0053—Producing sealings
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a kind of processing methods of low temperature resistant oil proof type rubber seal, are related to sealing ring processing technique field, comprise the following steps that：(1) dispensing, (2) are kneaded, (3) vulcanization, (4) freezing, (5) post-cure, (6) finishing.The present invention is using nitrile rubber and rare earth polybutadiene rubber as rubber major ingredient, it is aided with filler kaolin, sepiolite powder and multiple functions auxiliary agent and sealing ring is made, made sealing ring has good mechanical property, especially there is excellent resistance to low temperature, oil resistance and incompressible deformation performance, ensure the sealing effect of sealing ring at low ambient temperatures, and extends its service life at low ambient temperatures.
Description
Technical field：
The present invention relates to sealing ring processing technique fields, and in particular to a kind of processing of low temperature resistant oil proof type rubber seal
Method.
Background technology：
With the rapid development of modern mechanical industry, the demand of rubber seal is continuously increased.China northeast, northwest
Area's winter minimum temperature at -40 DEG C hereinafter, these area, winter cold the time it is long, day and night temperature is big, have a large amount of electric power,
The equipment such as oil, chemical industry are exposed in large natural environment, to be not only subjected to exposing to the weather, also suffer the test of severe cold.At this
In a little equipment, there is plurality of rubber seal although small, but have very important work to the normal operation of equipment
With.These regional rubber seals are easy to become fragile because of low temperature in winter, fail and cause failure, so rubber seal is resistance to low
Warm nature can be particularly significant.
In the rubber packing material of numerous kinds, nitrile rubber is wide as a kind of universal oil resistivity caulking gum material
It is general to be used for the products such as oil, chemical industry, electric power, the diaphragm of rolling stock, Y-shaped ring, O-ring and rubber mount.Nitrile rubber because
There is preferable oil resistant, solvent resistant and heat resistance containing itrile group in molecule, especially middle high acrylonitrile nitrile rubber is long-term
Temperature in use is up to 150 DEG C.But as acrylonitrile content increases, oil resistance improves, and resistance to low temperature declines, brittleness temperature one
As be -30 DEG C, when applied to cold districts sealing element be difficult keep it is good elasticity and sealing performance.
Patent CN 104893028A are grafted butadiene rubber using nitrile rubber and maleic anhydride and prepare rubber seal as major ingredient
Material, although made rubber packing material resistance to low temperature is excellent, incompressible deformation performance and oil resistance are also to be hoisted,
To extend the service life of made rubber packing material.
Invention content：
Technical problem to be solved by the present invention lies in provide a kind of to significantly improve resistance to low temperature, oil resistance and anti-
Compressive deformation performance ensures sealing ring sealing effect at low ambient temperatures and extends the low temperature resistant oil proof type rubber of its service life
The processing method of glue sealing ring.
The technical problems to be solved by the invention are realized using technical solution below：
A kind of processing method of low temperature resistant oil proof type rubber seal, comprises the following steps that：
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
It is 50-70 parts of nitrile rubber, 10-20 parts of rare earth polybutadiene rubber, 5-10 parts of kaolin, 5-10 parts of sepiolite powder, ultra-fine
1-5 parts of polytetrafluorethylepowder powder, 1-5 parts of C5 hydrogenated petroleum resins, 0.5-2 parts of accelerating agent, 0.5-2 parts of anti-aging agent, sulfuration resistant are returned
Former agent 0.5-2 parts, 0.5-2 parts of lubricant；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 100-
120r/min, mixing time 5-10min are cooled to 20-30 DEG C after first stage mixing with the cooling rate of 10 DEG C/min
Heat preservation stands 3-5h, and 140-150 DEG C of second stage melting temperature is kneaded rotating speed 100-120r/min, mixing time 5-10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10-15MPa, 160-170 DEG C of temperature, duration 10-15min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5-8h in subzero 15-10 DEG C of environment, and in natural ring
Restore to room temperature in border；
(5) post-cure：By above-mentioned chilled treated sealing ring again in pressure 10-15MPa, temperature 160-170
Post-cure, duration 10-15min are carried out under the conditions of DEG C；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
The acrylonitrile content of the nitrile rubber is 31-35wt%.
The one kind of the rare earth polybutadiene rubber in rare earth polybutadiene rubber BR Nd40, BR Nd50, BR Nd60.
The one kind of the accelerating agent in accelerator TBSI, accelerating agent TBzTD, accelerating agent ZBEC, accelerating agent TiBTM.
The anti-aging agent is in anti-aging agent 4030, anti-aging agent 4050, aging inhibitor FR, anti-aging agent 688, anti-aging agent 44PD
It is a kind of.
The anti-recovery agent is selected from anti-recovery agent Perkalink900.
The one kind of the lubricant in talcum powder, mica powder, calcium stearate, graphite.
The kaolin is handled through intercalation modifying, and specific method of modifying is：It is first with 20-25 DEG C of water that water process grade is more
Saturated solution is made in polyglutamic acid, adds calcined kaolin powder, and utilize microwave reactor microwave return stirring 5-
Microwave return stirring 5-10min, gained mixture are centrifuged again after 10min, stopping 15-30min, remove supernatant liquor,
Residue is sent into freeze drier, and micro mist is made to get polyglutamic acid/kaolin through micronizer in dry obtained solid
Intercalated compound powder.
The water process grade polyglutamic acid, calcined kaolin powder mass ratio be 5-10:1-2.
Polyglutamic acid enters kaolin interlayer, after kaolin interlamellar spacing is extended to insertion by the 1nm before being inserted into
1.23nm, 95% or more intercalation rate；Polyglutamic acid is arranged in a manner of being parallel to kaolin lamella in single layer in kaolin interlayer
Row, contained carboxyl form hydrogen bond, the oxygen atom shape of contained amino and kaolin silica layer with kaolinic inner surface hydroxyl
At hydrogen bond.
The sepiolite powder is through the filling-modified processing of physics, specific method of modifying：Sepiolite powder is heated to 120-
Deionized water is added when after naturally cool to 50 DEG C or less in 130 DEG C of insulated and stirreds, adds N hydroxymethyl acrylamide, and profit
It is reacted with microwave reactor microwave return stirring, waits for that lotion is made in the reduced pressure of gained mixture after self-crosslinking reaction,
Lotion is sent into after cooled to room temperature in freeze drier, dry obtained solid through micronizer be made micro mist to get
Aqueous Acrylate Resin Filling sepiolite powder.
The sepiolite powder, deionized water, N hydroxymethyl acrylamide mass ratio be 5-10:30-50:1-5.
N hydroxymethyl acrylamide forms acrylic resin, and the acrylic resin generated under microwave action through self-crosslinking
Immediately it incorporates in the molecular channel of sepiolite, to enhance the fillibility that sepiolite is used as filler by physics filling mode
Energy.
The operating condition of the microwave reactor is microwave frequency 2450MHz, output power 700W.
The lubricant is made of aluminium-magnesium silicate, rilanit special and trihydroxymethylpropanyltri diglycidyl ether, specific
Preparation method is：Aluminium-magnesium silicate is heated to 115-125 DEG C of insulated and stirred, adds rilanit special and trimethylolpropane tris
Glycidol ether continues in 115-125 DEG C of insulated and stirred, until gained lotion viscosity no longer changes, then with 5-10 DEG C/min
Cooling rate be cooled to subzero 10-5 DEG C, and heat preservation stands 2h at subzero 10-5 DEG C, and obtained solid is extensive in natural environment
Again to room temperature, micro mist most is made to get lubricant through micronizer afterwards.
The aluminium-magnesium silicate, rilanit special, trihydroxymethylpropanyltri diglycidyl ether mass ratio be 1-5:0.1-1:
0.1-1。
The beneficial effects of the invention are as follows：
(1) present invention improves the blend uniformity of sizing material, and enhance made sealing ring by the mixing action in two stages
Mechanical property；
(2) present invention improves the mechanical property of made sealing ring, especially incompressible morphotropism by vulcanisation operation twice
Energy and oil resistance；
(3) present invention is by the freezing processing between vulcanisation operation twice, enhance made sealing ring resistance to low temperature and
Incompressible deformation performance；
(4) present invention is aided with filler kaolin, sepiolite powder using nitrile rubber and rare earth polybutadiene rubber as rubber major ingredient
And sealing ring is made in multiple functions auxiliary agent, made sealing ring has good mechanical property, especially has excellent low temperature resistant
Performance, oil resistance and incompressible deformation performance ensure the sealing effect of sealing ring at low ambient temperatures, and extend it in low temperature
Service life under environment.
Specific implementation mode：
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 60kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 2kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Embodiment 2
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Embodiment 3
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
The preparation of lubricant：5kg aluminium-magnesium silicates are heated to 115-125 DEG C of insulated and stirred, add 0.5kg hydrogenated castors
Oil and 0.5kg trihydroxymethylpropanyltri diglycidyl ethers continue in 115-125 DEG C of insulated and stirred, until gained lotion viscosity is not
Change again, be then cooled to subzero 10-5 DEG C with the cooling rate of 5-10 DEG C/min, and heat preservation stands 2h at subzero 10-5 DEG C,
Obtained solid is restored in natural environment to room temperature, and micro mist most is made to get lubricant through micronizer afterwards.
Embodiment 4
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
The preparation of lubricant：3kg aluminium-magnesium silicates are heated to 115-125 DEG C of insulated and stirred, add 0.5kg hydrogenated castors
Oil and 0.3kg trihydroxymethylpropanyltri diglycidyl ethers continue in 115-125 DEG C of insulated and stirred, until gained lotion viscosity is not
Change again, be then cooled to subzero 10-5 DEG C with the cooling rate of 5-10 DEG C/min, and heat preservation stands 2h at subzero 10-5 DEG C,
Obtained solid is restored in natural environment to room temperature, and micro mist most is made to get lubricant through micronizer afterwards.
Embodiment 5
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
The modification of sepiolite powder：8kg sepiolite powders are heated to 120-130 DEG C of insulated and stirred, after naturally cool to 50 DEG C
40kg deionized waters are added when following, add 3kg N hydroxymethyl acrylamides, and utilize microwave frequency 2450MHz, output
The microwave reactor microwave return stirring of power 700W reacts, and waits for that gained mixture being concentrated under reduced pressure after self-crosslinking reaction and makes
At lotion, lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is made micro- through micronizer
Powder is to get Aqueous Acrylate Resin Filling sepiolite powder.
Embodiment 6
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
The modification of sepiolite powder：10kg sepiolite powders are heated to 120-130 DEG C of insulated and stirred, after naturally cool to 50 DEG C
50kg deionized waters are added when following, add 5kg N hydroxymethyl acrylamides, and utilize microwave frequency 2450MHz, output
The microwave reactor microwave return stirring of power 700W reacts, and waits for that gained mixture being concentrated under reduced pressure after self-crosslinking reaction and makes
At lotion, lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is made micro- through micronizer
Powder is to get Aqueous Acrylate Resin Filling sepiolite powder.
Embodiment 7
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Modifying kaolin：Saturated solution is made in 5kg water process grade polyglutamic acids first with 20-25 DEG C of water, then is added
Enter 1kg calcined kaolin powder, and is stirred using the reflux of the microwave reactor microwave of microwave frequency 2450MHz, output power 700W
It mixes 10min, stops after 15min that microwave return stirring 10min, gained mixture are centrifuged again, remove supernatant liquor, it is remaining
Object is sent into freeze drier, and micro mist is made to get polyglutamic acid/kaolin intercalation through micronizer in dry obtained solid
Composite powder.
Embodiment 8
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Modifying kaolin：Saturated solution is made in 8kg water process grade polyglutamic acids first with 20-25 DEG C of water, then is added
Enter 2kg calcined kaolin powder, and is stirred using the reflux of the microwave reactor microwave of microwave frequency 2450MHz, output power 700W
It mixes 10min, stops after 15min that microwave return stirring 10min, gained mixture are centrifuged again, remove supernatant liquor, it is remaining
Object is sent into freeze drier, and micro mist is made to get polyglutamic acid/kaolin intercalation through micronizer in dry obtained solid
Composite powder.
Embodiment 9
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Modifying kaolin：Saturated solution is made in 8kg water process grade polyglutamic acids first with 20-25 DEG C of water, then is added
Enter 2kg calcined kaolin powder, and is stirred using the reflux of the microwave reactor microwave of microwave frequency 2450MHz, output power 700W
It mixes 10min, stops after 15min that microwave return stirring 10min, gained mixture are centrifuged again, remove supernatant liquor, it is remaining
Object is sent into freeze drier, and micro mist is made to get polyglutamic acid/kaolin intercalation through micronizer in dry obtained solid
Composite powder.
The modification of sepiolite powder：10kg sepiolite powders are heated to 120-130 DEG C of insulated and stirred, after naturally cool to 50 DEG C
50kg deionized waters are added when following, add 5kg N hydroxymethyl acrylamides, and utilize microwave frequency 2450MHz, output
The microwave reactor microwave return stirring of power 700W reacts, and waits for that gained mixture being concentrated under reduced pressure after self-crosslinking reaction and makes
At lotion, lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is made micro- through micronizer
Powder is to get Aqueous Acrylate Resin Filling sepiolite powder.
The preparation of lubricant：3kg aluminium-magnesium silicates are heated to 115-125 DEG C of insulated and stirred, add 0.5kg hydrogenated castors
Oil and 0.3kg trihydroxymethylpropanyltri diglycidyl ethers continue in 115-125 DEG C of insulated and stirred, until gained lotion viscosity is not
Change again, be then cooled to subzero 10-5 DEG C with the cooling rate of 5-10 DEG C/min, and heat preservation stands 2h at subzero 10-5 DEG C,
Obtained solid is restored in natural environment to room temperature, and micro mist most is made to get lubricant through micronizer afterwards.
Reference examples 1
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant aluminium-magnesium silicate 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Reference examples 2
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：110-120 DEG C of melting temperature is kneaded rotating speed 120r/min, mixing time 20min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Reference examples 3
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5h in subzero 15-10 DEG C of environment, and in natural environment
It is middle to restore to room temperature；
(5) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Reference examples 4
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
Nitrile rubber (acrylonitrile content 31-35wt%) 70kg, rare earth polybutadiene rubber BR Nd40 10kg, kaolin
5kg, sepiolite powder 5kg, ultra-fine polytetrafluorethylepowder powder 3kg, C5 hydrogenated petroleum resin 2kg, accelerating agent TiBTM 0.5kg, prevent
Old agent 44PD 0.5kg, anti-recovery agent Perkalink900 0.5kg, lubricant stearic acid calcium 0.5kg；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 120r/
Min, mixing time 10min are cooled to 20-30 DEG C of heat preservation with the cooling rate of 10 DEG C/min after first stage mixing and stand
3h, 140-150 DEG C of second stage melting temperature are kneaded rotating speed 120r/min, mixing time 10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, it is pressing
Vulcanizing treatment under the conditions of power 10MPa, 160-170 DEG C of temperature, duration 10min；
(4) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10MPa, temperature item
Post-cure, duration 10min are carried out under part；
(5) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
Embodiment 10
It is utilized respectively the sealing ring that embodiment 1-9 prepares same specification, and the performance of made sealing ring is tested,
Test result is as shown in table 1.Simultaneously be arranged lubricant using aluminium-magnesium silicate reference examples 1, using the reference examples 2 being once kneaded,
Using the reference examples 3 once vulcanized, without the reference examples 4 of freezing processing.
Compression set test condition：100 DEG C × for 24 hours × 25%
The cold-resistant coefficient test condition of compression：-50℃
Anti-aging property test condition：100℃×24h
The hydraulic oil of resistance to 15# test condition：100℃×24h
The performance test result of the made sealing ring of the table 1-1 present invention
The performance test result of the made sealing ring of the table 1-2 present invention
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (7)
1. a kind of processing method of low temperature resistant oil proof type rubber seal, which is characterized in that comprise the following steps that：
(1) dispensing：The raw material for weighing following parts by weight obtains sizing material after high-speed mixer mixes；
50-70 parts of nitrile rubber, 10-20 parts of rare earth polybutadiene rubber, 5-10 parts of kaolin, 5-10 parts of sepiolite powder, ultra-fine poly- four
1-5 parts of vinyl fluoride powder, 1-5 parts of C5 hydrogenated petroleum resins, 0.5-2 parts of accelerating agent, 0.5-2 parts of anti-aging agent, anti-recovery agent
0.5-2 parts, 0.5-2 parts of lubricant；
(2) it is kneaded：Calendering process is divided into two stages, and 110-120 DEG C of first stage melting temperature is kneaded rotating speed 100-120r/
Min, mixing time 5-10min, with the cooling rate of 10 DEG C/min to be cooled to 20-30 DEG C of heat preservation quiet after the first stage is kneaded
3-5h is set, 140-150 DEG C of second stage melting temperature is kneaded rotating speed 100-120r/min, mixing time 5-10min；
(3) vulcanize：The sizing material extrusion molding that will be kneaded, then film after molding is injected in vulcanizer mold, in pressure 10-
Vulcanizing treatment under the conditions of 15MPa, 160-170 DEG C of temperature, duration 10-15min；
(4) it freezes：Made sealing ring will be vulcanized and be placed in sealing freezing 5-8h in subzero 15-10 DEG C of environment, and in natural environment
Restore to room temperature；
(5) post-cure：By above-mentioned chilled treated sealing ring again in 160-170 DEG C of pressure 10-15MPa, temperature item
Post-cure, duration 10-15min are carried out under part；
(6) it finishes：Deburring is carried out to made sealing ring, through packaging and storage after the assay was approved.
2. the processing method of low temperature resistant oil proof type rubber seal according to claim 1, it is characterised in that：The butyronitrile
The acrylonitrile content of rubber is 31-35wt%.
3. the processing method of low temperature resistant oil proof type rubber seal according to claim 1, it is characterised in that：The rare earth
The one kind of butadiene rubber in rare earth polybutadiene rubber BR Nd40, BR Nd50, BR Nd60.
4. the processing method of low temperature resistant oil proof type rubber seal according to claim 1, it is characterised in that：The promotion
The one kind of agent in accelerator TBSI, accelerating agent TBzTD, accelerating agent ZBEC, accelerating agent TiBTM.
5. the processing method of low temperature resistant oil proof type rubber seal according to claim 1, it is characterised in that：It is described anti-old
The one kind of agent in anti-aging agent 4030, anti-aging agent 4050, aging inhibitor FR, anti-aging agent 688, anti-aging agent 44PD.
6. the processing method of low temperature resistant oil proof type rubber seal according to claim 1, it is characterised in that：The sulfur resistive
Change reverts agent selected from anti-recovery agent Perkalink900.
7. the processing method of low temperature resistant oil proof type rubber seal according to claim 1, it is characterised in that：The lubrication
The one kind of agent in talcum powder, mica powder, calcium stearate, graphite.
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| CN109666202A (en) * | 2018-12-27 | 2019-04-23 | 无锡市兰翔胶业有限公司 | A kind of elasticizer cushion rubber |
| CN111662491A (en) * | 2020-06-04 | 2020-09-15 | 江门市鑫辉密封科技有限公司 | Formula and preparation method of nitrile rubber |
| CN112405985A (en) * | 2020-10-29 | 2021-02-26 | 清华大学 | Forming method of rubber part |
| CN112406129A (en) * | 2020-10-29 | 2021-02-26 | 清华大学 | Production method and production system of rubber part |
| CN113527774A (en) * | 2020-04-16 | 2021-10-22 | 上海弗兆实业有限公司 | Processing technology of rubber sealing ring |
| CN114044986A (en) * | 2021-12-25 | 2022-02-15 | 常州坚正橡塑制品有限公司 | Low-temperature-resistant rubber, preparation method thereof and air spring end cover applying low-temperature-resistant rubber |
| CN114962640A (en) * | 2022-06-15 | 2022-08-30 | 爱奇迹(深圳)创新科技有限公司 | Oil leakage prevention sealing ring and machining method thereof |
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| CN112405985A (en) * | 2020-10-29 | 2021-02-26 | 清华大学 | Forming method of rubber part |
| CN112406129A (en) * | 2020-10-29 | 2021-02-26 | 清华大学 | Production method and production system of rubber part |
| CN112406129B (en) * | 2020-10-29 | 2021-11-30 | 清华大学 | Production method and production system of rubber part |
| CN114044986A (en) * | 2021-12-25 | 2022-02-15 | 常州坚正橡塑制品有限公司 | Low-temperature-resistant rubber, preparation method thereof and air spring end cover applying low-temperature-resistant rubber |
| CN114962640A (en) * | 2022-06-15 | 2022-08-30 | 爱奇迹(深圳)创新科技有限公司 | Oil leakage prevention sealing ring and machining method thereof |
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