CN105255021B - A kind of high intensity low compression set elastomeric material and preparation method thereof - Google Patents
A kind of high intensity low compression set elastomeric material and preparation method thereof Download PDFInfo
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- CN105255021B CN105255021B CN201510738057.6A CN201510738057A CN105255021B CN 105255021 B CN105255021 B CN 105255021B CN 201510738057 A CN201510738057 A CN 201510738057A CN 105255021 B CN105255021 B CN 105255021B
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K5/00—Use of organic ingredients
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
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Abstract
The invention discloses a kind of high intensity low compression set elastomeric material and preparation method thereof.The elastomeric material includes the component of following parts by weight：100 parts of ethylene propylene diene rubbers, 20~40 parts of hydrophobic type fume colloidal silicas, 2~4 parts of vulcanizing agents, 0.5~2 part of vulcanization aid, 2~4 parts of age resistor, 4~6 portions of activating agents, 0.5~1 part of processing aid.The MPa of the tensile strength for the high intensity low compression set elastomeric material that the present invention obtains >=16, compression set≤15%, excellent performance, products appearance are light color, and free from extraneous odour, preparation method technique is simple, convenient operation and control.
Description
Technical field
The invention belongs to rubber materials, more particularly to a kind of high intensity low compression set elastomeric material and its preparation side
Method.
Background technology
Ethylene propylene diene rubber is formed by three kinds of ethene, propylene, non-conjugated diene hydrocarbon monomer copolymerizations, and its molecular backbone is complete
Saturation and non-polar group, there is the performance such as excellent electrical insulating property, heat-resisting, resistance to ozone, ageing-resistant, resistance to polar solvent, therefore
It is widely used in auto parts machinery, waterproof roll, electric wire, heat-resistant rubber hose adhesive tape, door and window sealing strip, seal washer etc..
Ethylene propylene diene rubber right and wrong the limited strength provided in itself by rubber, are not filled by vulcanizate from reinforcing rubber
Tensile strength is generally less than 5 MPa, and no use value is, it is necessary to obtain good mechanical performance by packing strengthening agent.By
Larger pressure is subjected in use environment in some seals, this requires this rubber-like materials to have sufficiently large intensity to hold
By ambient pressure, otherwise rubber packing material is easily damaged under pressure, causes seal failure.
Rubber obtains high intensity, but the permanent change of now system compression often through high reinforcing filler is largely filled
Shape is big.Patent No. CN103865181 Chinese patent discloses a kind of elastomeric material, need to fill 30~37 parts of carbon black N330 and
30~37 parts of carbon black N550, system tensile strength reaches 20 MPa, but compression set is more than 15%.Patent No.
CN101633764 Chinese patent discloses a kind of rubber, when filling 20 parts of activated carbon powders and 50 parts of carbon black N660, system pressure
Compression permanent deformation is less than 15%, but tensile strength is less than 16 MPa, when filling 30 parts of activated carbon powders and 50 parts of carbon black N660, body
It is that tensile strength is more than 17 MPa, but compression set is more than 15%.Patent No. CN102924768 Chinese patent discloses
A kind of rubber composition, is matrix using nitrile rubber, system tensile strength is more than 18 MPa, and compression set can reach
20%.Patent No. CN104177677 Chinese patent discloses a kind of mixing of rubber and its packing ring, and system tensile strength is
23.8 MPa, compression set 18%.The size of compression set value is to weigh elastomeric material sealing property and damping property
Can fine or not and service life length important indicator.Compression set is smaller, and the sealing property and damping performance of material are better,
Sealing property and the reliability of damping performance can be kept for a long time.
Therefore, it is necessary to further improve formula and processing technology, rubber packing material had both been possessed high intensity, possess again
Low compression set performance.
The content of the invention
It is an object of the invention to provide a kind of high intensity low compression set elastomeric material and preparation method thereof, pass through
Formula design and process control, acquisition had not only had high intensity but also had possessed the elastomeric material of low compression set performance, outside product
See as light color, free from extraneous odour.
The invention provides a kind of high intensity low compression set elastomeric material, include the component of following parts by weight：
100 parts of ethylene propylene diene rubber；
20~40 parts of filler, the filler are hydrophobic type fume colloidal silica；
2~4 parts of vulcanizing agent；
0.5~2 part of vulcanization aid；
2~4 parts of age resistor；
4~6 parts of activating agent；
0.5~1 part of processing aid.
Preferably, described hydrophobic type fume colloidal silica, specific surface area are not less than 200m2/g。
The vulcanizing agent is peroxide vulcanizing agent；
Preferably, the peroxide vulcanizing agent is dual-tert-butyl dicumyl peroxide.
The age resistor includes radical-scavenging formulation age resistor and peroxide decomposer type age resistor；
Preferably, the age resistor is anti-aging agent RD and antioxidant MB.
The activating agent is zinc oxide；
The processing aid is stearic acid.
The invention provides a kind of preparation method of high intensity low compression set elastomeric material, comprise the following steps：
A) each component is rationally weighed by formula first, is kneaded by two-roll mill and elastomeric compound is made；
B) back mixing is carried out after elastomeric compound in the step a) is parked；
C) elastomeric compound after back mixing in the step b) is subjected to flat board molding vulcanization and vulcanizate is made；
D) post vulcanization is carried out after the vulcanizate in the step c) is parked, obtains high intensity low compression set rubber
Glue material.
When two-roll mill is kneaded in the step a), into rubber matrix, charging sequence is：Processing aid, activating agent,
Age resistor, filler, vulcanizing agent and vulcanization aid.
Mixing temperature is 80~100 DEG C in the step a).
The mill time is 20~30 minutes in the step a).
The storage period is more than 20 hours in the step b).
Step c) the middle plateforms molding curing temperature is 150~180 DEG C.
Step c) the middle plateforms molding cure time is 10~20 minutes.
Post vulcanization temperature is 140~160 DEG C in the step d).
The post vulcanization time is 1.5~3 hours in the step d).
The storage period is more than 20 hours in the step d).
Obtained elastomeric material is carried out quantitative measurement by the present invention, and detailed process is as follows：
Standard No. is used to be carried out for ASTM D412 standard to the obtained tensile strength of elastomeric material and elongation at break
Test.
Standard No. is used to be tested for the hardness of elastomeric material of the ASTM D2240 standard to obtaining.
Standard No. is used to be tested for the compression set of elastomeric material of the ASTM D395 standard to obtaining.
The present invention adds hydrophobic type fume colloidal silica, and reinforcing effect is excellent；The elastomeric compound of acquisition is parked,
Various auxiliary agents is further uniformly dispersed in rubber, further penetrate into rubber macromolecule chain, with rubber
Glue macromolecular chain interacts, and improves reinforcing effect；Back mixing is carried out to the rubber after parking, makes various auxiliary agents in sizing material
Further it is uniformly dispersed, improves rubber mobility, improves finished appearance and quality；Vulcanizing agent and vulcanization aid are used simultaneously, is carried
The high crosslink density of sizing material；Carry out post vulcanization and can further improve crosslink density, remove small molecule, drop low compression set becomes
Shape.The MPa of the tensile strength for the high intensity low compression set elastomeric material that the present invention obtains >=16, compression set≤
15%, excellent performance, products appearance is light color, and free from extraneous odour, preparation method technique is simple, convenient operation and control.
Specific implementation method
In following embodiment, the dosage of each component is by weight.Be necessary it is pointed out here that, example below only
It is the further explanation to the present invention, it is impossible to be interpreted as limiting the scope of the invention, person skilled in art can be with
Some nonessential modifications and adaptations are carried out to the present invention according to the invention described above content.
Embodiment 1
100 parts of ethylene propylene diene rubbers are placed in mill bag roller in mill, 100 DEG C of mixing temperature, then add 0.5 part firmly
Resin acid, 5 parts of zinc oxide, 2 parts of trimethyl -1,2- dihyaroquinoline condensates of age resistor 2,2,4-, 1 part of age resistor 2- sulfydryl benzo
Imidazoles, 20 parts of hydrophobic type fume colloidal silica AEROSIL R106,2.5 parts of vulcanizing agent dual-tert-butyl dicumyl peroxides, 1
Part vulcanization aid Triallyl isocyanurate, elastomeric compound is obtained after being kneaded 25 minutes, after parking 24 hours, carries out flat board molding
Vulcanizate is made after vulcanization, curing temperature is 170 DEG C, and cure time is 13 minutes, and two are carried out after vulcanizate is parked 24 hours
Section vulcanization, curing temperature are 150 DEG C, and cure time is 2 hours, finally gives high intensity low compression set elastomeric material,
Corresponding test result is as shown in table 1.
Embodiment 2
100 parts of ethylene propylene diene rubbers are placed in mill bag roller in mill, 100 DEG C of mixing temperature, then add 0.5 part firmly
Resin acid, 5 parts of zinc oxide, 2 parts of trimethyl -1,2- dihyaroquinoline condensates of age resistor 2,2,4-, 1 part of age resistor 2- sulfydryl benzo
Imidazoles, 30 parts of hydrophobic type fume colloidal silica AEROSIL R106,2.5 parts of vulcanizing agent dual-tert-butyl dicumyl peroxides, 1
Part vulcanization aid Triallyl isocyanurate, elastomeric compound is obtained after being kneaded 25 minutes, after parking 24 hours, carries out flat board molding
Vulcanizate is made after vulcanization, curing temperature is 170 DEG C, and cure time is 14 minutes, and two are carried out after vulcanizate is parked 24 hours
Section vulcanization, curing temperature are 150 DEG C, and cure time is 2 hours, finally gives high intensity low compression set elastomeric material,
Corresponding test result is as shown in table 1.
Embodiment 3
100 parts of ethylene propylene diene rubbers are placed in mill bag roller in mill, 100 DEG C of mixing temperature, then add 0.5 part firmly
Resin acid, 5 parts of zinc oxide, 2 parts of trimethyl -1,2- dihyaroquinoline condensates of age resistor 2,2,4-, 1 part of age resistor 2- sulfydryl benzo
Imidazoles, 40 parts of hydrophobic type fume colloidal silica AEROSIL R106,2.5 parts of vulcanizing agent dual-tert-butyl dicumyl peroxides, 1
Part vulcanization aid Triallyl isocyanurate, elastomeric compound is obtained after being kneaded 25 minutes, after parking 24 hours, carries out flat board molding
Vulcanizate is made after vulcanization, curing temperature is 170 DEG C, and cure time is 15 minutes, and two are carried out after vulcanizate is parked 24 hours
Section vulcanization, curing temperature are 150 DEG C, and cure time is 2 hours, finally gives high intensity low compression set elastomeric material,
Corresponding test result is as shown in table 1.
Comparative example 1
100 parts of ethylene propylene diene rubbers are placed in mill bag roller in mill, 100 DEG C of mixing temperature, then add 0.5 part firmly
Resin acid, 5 parts of zinc oxide, 2 parts of trimethyl -1,2- dihyaroquinoline condensates of age resistor 2,2,4-, 1 part of age resistor 2- sulfydryl benzo
Imidazoles, 20 parts of hydrophilic fume colloidal silica AEROSIL, 300,2.5 parts of vulcanizing agent dual-tert-butyl dicumyl peroxides, 1
Part vulcanization aid Triallyl isocyanurate, elastomeric compound is obtained after being kneaded 25 minutes, after parking 24 hours, carries out flat board molding
Vulcanizate is made after vulcanization, curing temperature is 170 DEG C, and cure time is 13 minutes, and two are carried out after vulcanizate is parked 24 hours
Section vulcanization, curing temperature are 150 DEG C, and cure time is 2 hours, finally gives elastomeric material, the corresponding test result such as institute of table 1
Show.
Comparative example 2
100 parts of ethylene propylene diene rubbers are placed in mill bag roller in mill, 100 DEG C of mixing temperature, then add 0.5 part firmly
Resin acid, 5 parts of zinc oxide, 2 parts of trimethyl -1,2- dihyaroquinoline condensates of age resistor 2,2,4-, 1 part of age resistor 2- sulfydryl benzo
Imidazoles, 30 parts of hydrophilic fume colloidal silica AEROSIL, 300,2.5 parts of vulcanizing agent dual-tert-butyl dicumyl peroxides, 1
Part vulcanization aid Triallyl isocyanurate, elastomeric compound is obtained after being kneaded 25 minutes, after parking 24 hours, carries out flat board molding
Vulcanizate is made after vulcanization, curing temperature is 170 DEG C, and cure time is 14 minutes, and two are carried out after vulcanizate is parked 24 hours
Section vulcanization, curing temperature are 150 DEG C, and cure time is 2 hours, finally gives elastomeric material, the corresponding test result such as institute of table 1
Show.
Comparative example 3
100 parts of ethylene propylene diene rubbers are placed in mill bag roller in mill, 100 DEG C of mixing temperature, then add 0.5 part firmly
Resin acid, 5 parts of zinc oxide, 2 parts of trimethyl -1,2- dihyaroquinoline condensates of age resistor 2,2,4-, 1 part of age resistor 2- sulfydryl benzo
Imidazoles, 40 parts of hydrophilic fume colloidal silica AEROSIL, 300,2.5 parts of vulcanizing agent dual-tert-butyl dicumyl peroxides, 1
Part vulcanization aid Triallyl isocyanurate, elastomeric compound is obtained after being kneaded 25 minutes, after parking 24 hours, carries out flat board molding
Vulcanizate is made after vulcanization, curing temperature is 170 DEG C, and cure time is 15 minutes, and two are carried out after vulcanizate is parked 24 hours
Section vulcanization, curing temperature are 150 DEG C, and cure time is 2 hours, finally gives elastomeric material, the corresponding test result such as institute of table 1
Show.
Comparative example 4
100 parts of ethylene propylene diene rubbers are placed in mill bag roller in mill, 100 DEG C of mixing temperature, then add 0.5 part firmly
Resin acid, 5 parts of zinc oxide, 2 parts of trimethyl -1,2- dihyaroquinoline condensates of age resistor 2,2,4-, 1 part of age resistor 2- sulfydryl benzo
Imidazoles, 60 parts of carbon black N300,2.5 parts of vulcanizing agent dual-tert-butyl dicumyl peroxides, 1 part of vulcanization aid triallyl isocyanide
Urea acid esters, elastomeric compound is obtained after being kneaded 25 minutes, after parking 24 hours, vulcanizate, vulcanization is made after carrying out flat board molding vulcanization
Temperature is 170 DEG C, and cure time is 15 minutes, and post vulcanization, curing temperature 150 are carried out after vulcanizate is parked 24 hours
DEG C, cure time is 2 hours, finally gives elastomeric material, corresponding test result is as shown in table 1.
Compression set uses the method B in ASTM D395 to be tested (125 DEG C × 22 h, 25%) in the present invention.
Claims (4)
1. a kind of high intensity low compression set elastomeric material, include the component of following parts by weight：
100 parts of ethylene propylene diene rubber；
20~40 parts of filler,
The filler is hydrophobic type fume colloidal silica, and specific surface area is not less than 200 m2/g。
2~4 parts of vulcanizing agent；
0.5~2 part of vulcanization aid；
2~4 parts of age resistor；
4~6 parts of activating agent；
0.5~1 part of processing aid.
Prepared high intensity low compression set elastomeric material is characterised by the MPa of tensile strength >=16, compresses permanent become
Shape≤15%.
2. high intensity low compression set elastomeric material according to claim 1, it is characterised in that the age resistor bag
The age resistor of formulation containing radical-scavenging and peroxide decomposer type age resistor.
A kind of 3. method of the high intensity low compression set elastomeric material prepared described in claim 1, it is characterised in that bag
Include following steps：
A) each component is rationally weighed by formula first, is kneaded by two-roll mill and elastomeric compound is made；
B) back mixing is carried out after elastomeric compound in the step a) is parked；
C) elastomeric compound after back mixing in the step b) is subjected to flat board molding vulcanization and vulcanizate is made；
D) post vulcanization is carried out after the vulcanizate in the step c) is parked, obtains high intensity low compression set rubber material
Material.
4. the method according to claim 3 for preparing high intensity low compression set elastomeric material, it is characterised in that stop
The time is put as more than 20 hours.
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| CN106674770A (en) * | 2017-01-24 | 2017-05-17 | 新兴铸管股份有限公司 | Long-life pipe rubber sealing element and preparation method thereof |
| CN106905617B (en) * | 2017-03-01 | 2018-10-30 | 北京市城南橡塑技术研究所 | Long-life pipeline rubber seal |
| CN107674326A (en) * | 2017-10-31 | 2018-02-09 | 成都盛帮密封件股份有限公司 | A kind of ethylene-propylene-diene monomer matrix seal and preparation method thereof |
| CN110330750B (en) * | 2019-07-08 | 2021-07-30 | 四川青龙丙烯酸酯橡胶有限公司 | Low-compression permanent deformation carboxylic acid type acrylate rubber and preparation method thereof |
| CN113294601B (en) * | 2021-05-31 | 2022-11-11 | 东风商用车有限公司 | Automobile water delivery rubber pipe with wide application temperature range and preparation method thereof |
| CN113881118B (en) * | 2021-11-25 | 2023-07-14 | 南阳天一密封股份有限公司 | NBR (nitrile butadiene rubber) rubber with low compression set and preparation process thereof |
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| CN102382376B (en) * | 2011-09-06 | 2013-04-03 | 青岛开世密封工业有限公司 | Method for preparing colored ethylene-propylene rubber |
| CN102875905A (en) * | 2012-09-27 | 2013-01-16 | 青岛开世密封工业有限公司 | Low-pressure-variation ethylene-propylene rubber mixed compound and mixing method |
| CN103044786A (en) * | 2012-12-29 | 2013-04-17 | 山东美晨科技股份有限公司 | Ethylene propylene rubber with high temperature resistance and low compression deformation |
| CN103497428B (en) * | 2013-09-03 | 2015-04-08 | 江苏荣昌机械制造集团有限公司 | EPDM rubber with low compressive deformation and high elasticity |
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