CN108530705A - A kind of preparation method of ageing-resistant flexible nitrile rubber - Google Patents
A kind of preparation method of ageing-resistant flexible nitrile rubber Download PDFInfo
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of preparation methods of ageing-resistant flexible nitrile rubber, the technique is by 2, 2 two (4 hydroxy phenyl) butane, sodium chloride, acetyl triethyl citrate, nitrile rubber, butyl rubber, acid fiber by polylactic, linear phenol-aldehyde resin, manganese dioxide, odium stearate, paraffin, triphenyl first sulfenamide, three hydroxy stearic acid ester of glycerine, potassium sorbate, antifoaming agent and stabilizer mixed liquor, sulphur powder, the raw materials such as vulcanizing agent pass through back flow reaction respectively, high-temperature pressurizing is reacted, ultrasonic disperse, twin-screw extrusion, compression molding, high-temperature shaping cures, cooling dry and etc. ageing-resistant flexible nitrile rubber is prepared.The ageing-resistant flexible nitrile rubber being prepared, soft texture, ageing-resistant performance are good, can meet a variety of user demands.
Description
Technical field
The present invention relates to this technical fields of rubber material, are related specifically to a kind of preparation of ageing-resistant flexible nitrile rubber
Method.
Background technology
Nitrile rubber is also known as butadiene-propylene nitrile rubber, abbreviation NBR, average molecular weight 700,000 or so, and canescence is to pale yellow
Color lump shape or powdery solid, relative density 0.95~1.0 are dissolved in ethyl acetate, butyl acetate, chlorobenzene, methyl ethyl ketone etc..Butyronitrile rubber
Glue has excellent oil resistivity, and oil resistivity is only second to polysulfide rubber and fluorubber, and has wearability and air-tightness, extensively
Applied to industrial circles such as automobile, space flight, oil exploitations.Raising is concentrated mainly on for the research of nitrile rubber in the prior art
In terms of its proper property.But the nitrile rubber of the prior art, in machining process, the good sizing material of batch mixing is directly put
The sulfidization molding on vulcanizing press is placed in mold, but this process be there are problems that in process of production, such as
The product of some complicated shapes not easy mold release, exhaust problem causes product surface peeling or has bubble in process, product
It is easy to aging etc..Therefore the part with complicated structure qualification rate produced according to existing process is not high, and causes prodigious people
The waste of power material resources.
Invention content
It in order to solve the above-mentioned technical problem, should the invention discloses a kind of preparation method of ageing-resistant flexible nitrile rubber
Technique is by 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate, nitrile rubber, butyl rubber, polylactic acid
Fiber, linear phenol-aldehyde resin, manganese dioxide, odium stearate, paraffin, triphenyl first sulfenamide, three hydroxy stearic acid ester of glycerine, mountain
It is anti-that the raw materials such as potassium sorbate, antifoaming agent and stabilizer mixed liquor, sulphur powder, vulcanizing agent pass through back flow reaction, high-temperature pressurizing respectively
Answer, ultrasonic disperse, twin-screw extrusion, compression molding, high-temperature shaping solidification, cooling dry and etc. ageing-resistant flexibility is prepared
Nitrile rubber.The ageing-resistant flexible nitrile rubber being prepared, soft texture, ageing-resistant performance are good, can meet a variety of use
Family demand.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of ageing-resistant flexible nitrile rubber, includes the following steps:
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, and it is anti-to be filled with argon gas protection
It should carry out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride and the concentrated sulfuric acid as drier;
(2)By 10-20 parts of nitrile rubber, 10-16 parts of butyl rubber, 5-10 parts of acid fiber by polylactic, 4-10 parts of linear phenol-aldehyde resin,
In 2-3 parts of injection high-temperature calcination stoves of manganese dioxide, 2-6 parts of odium stearate, 1-2 parts of paraffin are then sequentially added, after being sufficiently stirred,
Pressurization, is filled with argon gas, high temperature sintering 150min, and calcination temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 1-3 parts of triphenyl first sulfenamide, glycerine
Three 1-4 parts of hydroxy stearic acid esters, 1-3 parts of potassium sorbate are ultrasonically treated 2-4h and obtain stock suspension;
(4)To step(3)Suspension in antifoaming agent and stabilizer mixed liquor, 2-4 parts of sulphur powder, 1-2 parts of vulcanizing agent is added,
Heat preservation stands 10-18h after stirring evenly, spare;
(5)By step(4)Mixed liquor injection double screw extruder in, it is extrusion, pressing mold, moulding;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, be filled with cycle CO2Gas, reaction
After 30-60min, takes out Temperature fall and dry, packaging is got product.
Preferably, the step(1)In the step(1)In reflux temperature be 98-102 DEG C.
Preferably, the step(2)In stove in pressure be 4-8MPa.
Preferably, the step(3)In supersound process frequency be 50-60KHz, power 800-1000W.
Preferably, the step(4)In antifoaming agent and stabilizer mixed liquor be silicone emulsion, dimethyl silicone polymer,
High-carbon alcohol fatty acid ester,(2- bromoethyls)Trimethylsilane, glycerine molal weight ratio are 2:3:1:2:5 mixed liquor.
Preferably, the step(4)In vulcanizing agent be selected from para-tert-butyl phenolic resin, p-tert-octyl phenol urea formaldehyde, six
One or more of methylene diamine carbaminate, ethylene amido formates.
Preferably, the step(5)In extruder temperature be 220-260 DEG C, screw speed be 1200-1500 revs/min.
Preferably, the step(6)In the condition of vulcanization be:175 DEG C, 25MPa, 30sec.
Preferably, the step(7)High temperature steam temperature is 1200-1500 DEG C.
Compared with prior art, the present invention advantage is:
(1)The preparation method of the ageing-resistant flexible nitrile rubber of the present invention is by 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, second
Acyl triethyl citrate, nitrile rubber, butyl rubber, acid fiber by polylactic, linear phenol-aldehyde resin, manganese dioxide, odium stearate, stone
Wax, triphenyl first sulfenamide, three hydroxy stearic acid ester of glycerine, potassium sorbate, antifoaming agent and stabilizer mixed liquor, sulphur powder,
The raw materials such as vulcanizing agent are fixed by back flow reaction, high-temperature pressurizing reaction, ultrasonic disperse, twin-screw extrusion, compression molding, high temperature respectively
Type solidification, cooling dry and etc. ageing-resistant flexible nitrile rubber is prepared.The ageing-resistant flexible nitrile rubber being prepared,
Its soft texture, ageing-resistant performance are good, can meet a variety of user demands.
(2)The ageing-resistant flexible nitrile rubber raw material of the present invention is easy to get, is simple for process, is suitable for heavy industrialization and uses,
It is highly practical.
Specific implementation mode
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, reflux temperature 98-
It 102 DEG C, is filled with argon gas protection reaction and carries out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride
With the concentrated sulfuric acid as drier;
(2)By 10 parts of nitrile rubber, 10 parts of butyl rubber, 5 parts of acid fiber by polylactic, 4 parts of linear phenol-aldehyde resin, 2 parts of manganese dioxide
It injects in high-temperature calcination stove, then sequentially adds 2 parts of odium stearate, 1 part of paraffin, after being sufficiently stirred, pressurize, pressure is in stove
4MPa, is filled with argon gas, high temperature sintering 150min, and calcination temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 1 part of triphenyl first sulfenamide, glycerine three
1 part of hydroxy stearic acid ester, 1 part of potassium sorbate are ultrasonically treated 2h and obtain stock suspension, and the frequency of supersound process is 50KHz, power
For 800W;
(4)To step(3)Suspension in antifoaming agent and stabilizer mixed liquor, 2 parts of sulphur powder, p-tert-butylphenol aldehyde tree is added
1 part of fat, heat preservation standing 10h, spare after stirring evenly, and wherein antifoaming agent and stabilizer mixed liquor are silicone emulsion, poly dimethyl
Siloxanes, high-carbon alcohol fatty acid ester,(2- bromoethyls)Trimethylsilane, glycerine molal weight ratio are 2:3:1:2:5 mixed liquor;
(5)By step(4)Mixed liquor injection double screw extruder in, extrusions, pressing mold, moulding, wherein extruder temperature is 220
DEG C, screw speed is 1200 revs/min;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, the condition of vulcanization is:175 DEG C,
25MPa, 30sec obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, high-temperature vapor temperature is 1200
DEG C, it is filled with cycle CO2Gas after reacting 30min, takes out Temperature fall and dries, packaging is got product.
The performance test results of ageing-resistant flexible nitrile rubber obtained are as shown in table 1.
Embodiment 2
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, reflux temperature 98-
It 102 DEG C, is filled with argon gas protection reaction and carries out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride
With the concentrated sulfuric acid as drier;
(2)By 13 parts of nitrile rubber, 12 parts of butyl rubber, 7 parts of acid fiber by polylactic, 6 parts of linear phenol-aldehyde resin, 2 parts of manganese dioxide
It injects in high-temperature calcination stove, then sequentially adds 3 parts of odium stearate, 1 part of paraffin, after being sufficiently stirred, pressurize, pressure is in stove
6MPa, is filled with argon gas, high temperature sintering 150min, and calcination temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 2 parts of triphenyl first sulfenamide, glycerine three
2 parts of hydroxy stearic acid ester, 1 part of potassium sorbate are ultrasonically treated 3h and obtain stock suspension, and the frequency of supersound process is 55KHz, power
For 900W;
(4)To step(3)Suspension in antifoaming agent and stabilizer mixed liquor, 3 parts of sulphur powder, p-tert-octyl phenol aldehyde tree is added
1 part of fat, heat preservation standing 12h, spare after stirring evenly, and wherein antifoaming agent and stabilizer mixed liquor are silicone emulsion, poly dimethyl
Siloxanes, high-carbon alcohol fatty acid ester,(2- bromoethyls)Trimethylsilane, glycerine molal weight ratio are 2:3:1:2:5 mixed liquor;
(5)By step(4)Mixed liquor injection double screw extruder in, extrusions, pressing mold, moulding, wherein extruder temperature is 230
DEG C, screw speed is 1300 revs/min;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, the condition of vulcanization is:175 DEG C,
25MPa, 30sec obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, high-temperature vapor temperature is 1300
DEG C, it is filled with cycle CO2Gas after reacting 40min, takes out Temperature fall and dries, packaging is got product.
The performance test results of ageing-resistant flexible nitrile rubber obtained are as shown in table 1.
Embodiment 3
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, reflux temperature 98-
It 102 DEG C, is filled with argon gas protection reaction and carries out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride
With the concentrated sulfuric acid as drier;
(2)By 17 parts of nitrile rubber, 15 parts of butyl rubber, 9 parts of acid fiber by polylactic, 9 parts of linear phenol-aldehyde resin, 3 parts of manganese dioxide
It injects in high-temperature calcination stove, then sequentially adds 5 parts of odium stearate, 2 parts of paraffin, after being sufficiently stirred, pressurize, pressure is in stove
7MPa, is filled with argon gas, high temperature sintering 150min, and calcination temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 2 parts of triphenyl first sulfenamide, glycerine three
3 parts of hydroxy stearic acid ester, 2 parts of potassium sorbate are ultrasonically treated 3.5h and obtain stock suspension, and the frequency of supersound process is 55KHz, work(
Rate is 950W;
(4)To step(3)Suspension in antifoaming agent and stabilizer mixed liquor, 3 parts of sulphur powder, hexamethylene diamine ammonia is added
2 parts of base formates, heat preservation standing 16h, spare after stirring evenly, and wherein antifoaming agent and stabilizer mixed liquor are silicone emulsion, gather
Dimethyl siloxane, high-carbon alcohol fatty acid ester,(2- bromoethyls)Trimethylsilane, glycerine molal weight ratio are 2:3:1:2:5
Mixed liquor;
(5)By step(4)Mixed liquor injection double screw extruder in, extrusions, pressing mold, moulding, wherein extruder temperature is 250
DEG C, screw speed is 1400 revs/min;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, the condition of vulcanization is:175 DEG C,
25MPa, 30sec obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, high-temperature vapor temperature is 1400
DEG C, it is filled with cycle CO2Gas after reacting 50min, takes out Temperature fall and dries, packaging is got product.
The performance test results of ageing-resistant flexible nitrile rubber obtained are as shown in table 1.
Embodiment 4
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, reflux temperature 98-
It 102 DEG C, is filled with argon gas protection reaction and carries out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride
With the concentrated sulfuric acid as drier;
(2)By 20 parts of nitrile rubber, 16 parts of butyl rubber, 10 parts of acid fiber by polylactic, 10 parts of linear phenol-aldehyde resin, manganese dioxide 3
In part injection high-temperature calcination stove, 6 parts of odium stearate, 2 parts of paraffin are then sequentially added, after being sufficiently stirred, is pressurizeed, pressure is in stove
8MPa, is filled with argon gas, high temperature sintering 150min, and calcination temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 3 parts of triphenyl first sulfenamide, glycerine three
4 parts of hydroxy stearic acid ester, 3 parts of potassium sorbate are ultrasonically treated 4h and obtain stock suspension, and the frequency of supersound process is 60KHz, power
For 1000W;
(4)To step(3)Suspension in antifoaming agent and stabilizer mixed liquor, 4 parts of sulphur powder, ethylene amido first is added
2 parts of hydrochlorate, heat preservation standing 18h, spare after stirring evenly, and wherein antifoaming agent and stabilizer mixed liquor are silicone emulsion, poly- diformazan
Radical siloxane, high-carbon alcohol fatty acid ester,(2- bromoethyls)Trimethylsilane, glycerine molal weight ratio are 2:3:1:2:5 mixing
Liquid;
(5)By step(4)Mixed liquor injection double screw extruder in, extrusions, pressing mold, moulding, wherein extruder temperature is 260
DEG C, screw speed is 1500 revs/min;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, the condition of vulcanization is:175 DEG C,
25MPa, 30sec obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, high-temperature vapor temperature is 1500
DEG C, it is filled with cycle CO2Gas after reacting 60min, takes out Temperature fall and dries, packaging is got product.
The performance test results of ageing-resistant flexible nitrile rubber obtained are as shown in table 1.
Comparative example 1
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, reflux temperature 98-
It 102 DEG C, is filled with argon gas protection reaction and carries out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride
With the concentrated sulfuric acid as drier;
(2)By in 2 parts of 10 parts of nitrile rubber, 10 parts of butyl rubber, manganese dioxide injection high-temperature calcination stoves, then sequentially add hard
2 parts of resin acid sodium, 1 part of paraffin after being sufficiently stirred, pressurize, and pressure is 4MPa in stove, are filled with argon gas, high temperature sintering 150min, calcining
Temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 1 part of triphenyl first sulfenamide, glycerine three
1 part of hydroxy stearic acid ester, 1 part of potassium sorbate are ultrasonically treated 2h and obtain stock suspension, and the frequency of supersound process is 50KHz, power
For 800W;
(4)To step(3)Suspension in antifoaming agent and stabilizer mixed liquor, 2 parts of sulphur powder, p-tert-butylphenol aldehyde tree is added
1 part of fat, heat preservation standing 10h, spare after stirring evenly, and wherein antifoaming agent and stabilizer mixed liquor are silicone emulsion, poly dimethyl
Siloxanes, high-carbon alcohol fatty acid ester,(2- bromoethyls)Trimethylsilane, glycerine molal weight ratio are 2:3:1:2:5 mixed liquor;
(5)By step(4)Mixed liquor injection double screw extruder in, extrusions, pressing mold, moulding, wherein extruder temperature is 220
DEG C, screw speed is 1200 revs/min;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, the condition of vulcanization is:175 DEG C,
25MPa, 30sec obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, high-temperature vapor temperature is 1200
DEG C, it is filled with cycle CO2Gas after reacting 30min, takes out Temperature fall and dries, packaging is got product.
The performance test results of ageing-resistant flexible nitrile rubber obtained are as shown in table 1.
Comparative example 2
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, reflux temperature 98-
It 102 DEG C, is filled with argon gas protection reaction and carries out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride
With the concentrated sulfuric acid as drier;
(2)By 20 parts of nitrile rubber, 16 parts of butyl rubber, 10 parts of acid fiber by polylactic, 10 parts of linear phenol-aldehyde resin, manganese dioxide 3
In part injection high-temperature calcination stove, 6 parts of odium stearate, 2 parts of paraffin are then sequentially added, after being sufficiently stirred, is pressurizeed, pressure is in stove
8MPa, is filled with argon gas, high temperature sintering 150min, and calcination temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 3 parts of triphenyl first sulfenamide, glycerine three
4 parts of hydroxy stearic acid ester, 3 parts of potassium sorbate are ultrasonically treated 4h and obtain stock suspension, and the frequency of supersound process is 60KHz, power
For 1000W;
(4)To step(3)Suspension in 4 parts of sulphur powder, 2 parts of ethylene amido formates is added, protected after stirring evenly
Temperature stands 18h, spare;
(5)By step(4)Mixed liquor injection double screw extruder in, extrusions, pressing mold, moulding, wherein extruder temperature is 260
DEG C, screw speed is 1500 revs/min;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, the condition of vulcanization is:175 DEG C,
25MPa, 30sec obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, high-temperature vapor temperature is 1500
DEG C, it is filled with cycle CO2Gas after reacting 60min, takes out Temperature fall and dries, packaging is got product.
The performance test results of ageing-resistant flexible nitrile rubber obtained are as shown in table 1.
Ageing-resistant flexibility nitrile rubber made from embodiment 1-4 and comparative example 1-2 is subjected to proportion, elasticity, pressure respectively
Compression permanent deformation, ageing-resistant this several performance tests.
Table 1
Proportion | Elasticity | Compression set | Resistance to ag(e)ing | |
Embodiment 1 | 0.87 | A | A | A |
Embodiment 2 | 0.86 | A | A | A |
Embodiment 3 | 0.87 | A | A | A |
Embodiment 4 | 0.86 | A | A | A |
Comparative example 1 | 0.99 | B | B | B |
Comparative example 2 | 0.96 | B | B | B |
The preparation method of the ageing-resistant flexible nitrile rubber of the present invention is by 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl
Triethyl citrate, nitrile rubber, butyl rubber, acid fiber by polylactic, linear phenol-aldehyde resin, manganese dioxide, odium stearate, stone
Wax, triphenyl first sulfenamide, three hydroxy stearic acid ester of glycerine, potassium sorbate, antifoaming agent and stabilizer mixed liquor, sulphur powder,
The raw materials such as vulcanizing agent are fixed by back flow reaction, high-temperature pressurizing reaction, ultrasonic disperse, twin-screw extrusion, compression molding, high temperature respectively
Type solidification, cooling dry and etc. ageing-resistant flexible nitrile rubber is prepared.The ageing-resistant flexible nitrile rubber being prepared,
Its soft texture, ageing-resistant performance are good, can meet a variety of user demands.The ageing-resistant flexible nitrile rubber raw material of the present invention is easy
It obtains, is simple for process, being suitable for heavy industrialization and use, it is highly practical.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of ageing-resistant flexible nitrile rubber, which is characterized in that include the following steps:
(1)By 2,2- bis- (4- hydroxy phenyls) butane, sodium chloride, acetyl triethyl citrate according to mass ratio 1:3:10 mixing,
It is sufficiently stirred, is placed in conical flask, conical flask, which is placed in dry return stirring reaction unit, to be reacted, and it is anti-to be filled with argon gas protection
It should carry out, reaction time 60min obtains modification liquid, wherein selecting anhydrous calcium chloride and the concentrated sulfuric acid as drier;
(2)By 10-20 parts of nitrile rubber, 10-16 parts of butyl rubber, 5-10 parts of acid fiber by polylactic, 4-10 parts of linear phenol-aldehyde resin,
In 2-3 parts of injection high-temperature calcination stoves of manganese dioxide, 2-6 parts of odium stearate, 1-2 parts of paraffin are then sequentially added, after being sufficiently stirred,
Pressurization, is filled with argon gas, high temperature sintering 150min, and calcination temperature is 620-625 DEG C;
(3)By step(2)Product and step(1)Modification liquid mixing, add 1-3 parts of triphenyl first sulfenamide, glycerine
Three 1-4 parts of hydroxy stearic acid esters, 1-3 parts of potassium sorbate are ultrasonically treated 2-4h and obtain stock suspension;
(4)To step(3)Suspension in antifoaming agent and stabilizer mixed liquor, 2-4 parts of sulphur powder, 1-2 parts of vulcanizing agent is added,
Heat preservation stands 10-18h after stirring evenly, spare;
(5)By step(4)Mixed liquor injection double screw extruder in, it is extrusion, pressing mold, moulding;
(6)By step(5)Pressure molded form be put on vulcanizing press and vulcanized, obtain vulcanization composite material;
(7)By step(6)Vulcanization composite material be put into sizing and solidifying in high-temperature vapor, be filled with cycle CO2Gas reacts 30-
After 60min, takes out Temperature fall and dry, packaging is got product.
2. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(1)
In reflux temperature be 98-102 DEG C.
3. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(2)
In stove in pressure be 4-8MPa.
4. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(3)
In supersound process frequency be 50-60KHz, power 800-1000W.
5. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(4)
In antifoaming agent and stabilizer mixed liquor be silicone emulsion, dimethyl silicone polymer, high-carbon alcohol fatty acid ester,(2- bromoethyls)Three
Monosilane, glycerine molal weight ratio are 2:3:1:2:5 mixed liquor.
6. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(4)
In vulcanizing agent be selected from para-tert-butyl phenolic resin, p-tert-octyl phenol urea formaldehyde, hexamethylene diamine carbamate, ethylidene
One or more of two Carbamates.
7. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(5)
In extruder temperature be 220-260 DEG C, screw speed be 1200-1500 revs/min.
8. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(6)
In the condition of vulcanization be:175 DEG C, 25MPa, 30sec.
9. the preparation method of ageing-resistant flexible nitrile rubber according to claim 1, which is characterized in that the step(7)
High temperature steam temperature is 1200-1500 DEG C.
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Citations (4)
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CN106188907A (en) * | 2016-08-30 | 2016-12-07 | 何仁英 | A kind of biological material being applicable to flexible pipe for medical purpose and preparation method thereof |
CN106893325A (en) * | 2017-03-14 | 2017-06-27 | 深圳市沃尔核材股份有限公司 | Fire resistant flame retardant heat-barrier material, preparation method and application that a kind of high temperature resistant resistance to compression becomes |
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CN105176403A (en) * | 2015-07-24 | 2015-12-23 | 中山市伯伦克专用化学产品有限公司 | High-temperature-resistant peelable blue glue |
CN106188907A (en) * | 2016-08-30 | 2016-12-07 | 何仁英 | A kind of biological material being applicable to flexible pipe for medical purpose and preparation method thereof |
CN106893325A (en) * | 2017-03-14 | 2017-06-27 | 深圳市沃尔核材股份有限公司 | Fire resistant flame retardant heat-barrier material, preparation method and application that a kind of high temperature resistant resistance to compression becomes |
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