CN108084352A - A kind of High-strength ethylene propylene diene monomer and preparation method thereof - Google Patents
A kind of High-strength ethylene propylene diene monomer and preparation method thereof Download PDFInfo
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- CN108084352A CN108084352A CN201711446823.7A CN201711446823A CN108084352A CN 108084352 A CN108084352 A CN 108084352A CN 201711446823 A CN201711446823 A CN 201711446823A CN 108084352 A CN108084352 A CN 108084352A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- 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
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- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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Abstract
The invention discloses a kind of High-strength ethylene propylene diene monomers, are formed including following parts by weight：10-20 parts of ethylene；15-25 parts of propylene；45-55 parts of Third monomer；0.6-1.2 parts of catalyst；800-900 parts of organic solvent；0.03-0.05 parts of terminator；0.01-0.05 parts of stabilizer；15-30 parts of modified carbon fiber.The modified ethylene propylene diene rubber of modified carbon fiber is with the addition of, it is suitable when properties, coke burning performance and curability are with being not added with, but after adding modified carbon fiber, the tensile property of ethylene propylene diene rubber is greatly improved.
Description
Technical field
The present invention relates to chemical technology field, more specifically, it relates to a kind of High-strength ethylene propylene diene monomer and its system
Preparation Method.
Background technology
EP rubbers is a kind of copolymer rubber using ethylene and propylene as basic monomer.Compared with other rubber clones, second
Third rubber has the following advantages：First, without double bond, fully saturated, resistance to ozone, ageing-resistant, chemicals-resistant and resistance to height in main chain
Temperature；2nd, light specific gravity；3rd, excellent insulation performance；4th, being can the oil-filled rubber clone of height.EP rubbers is that most have hair at present
One of rubber types of future are opened up, since it is commercially produced, application field is constantly expanded, and has been widely used for automobile
Component, building materials, electric wire, heat-resistant rubber hose, advanced sealing material, lube oil additive and polyolefin modified etc..
EP rubbers due to strand have height saturability, make its present determined by saturated structures it is a series of
Excellent properties.Ethylene propylene diene rubber (EPDM) is the rubber formed by ethylene, propylene through solution copolymerization, and it is single to be re-introduced into the 3rd
Body.Ethylene propylene diene rubber is substantially a kind of high polymer of saturation, is the synthetic rubber of high comprehensive performance, has fabulous electricity
Performance, ageing properties.But due to being free of crystalline solid, so intensity is very low, the scope of application is very restricted.
In order to improve the intensity of EPDM materials, fiber is commonly used to enhance EPDM.Most studied in recent years is to use nylon
(PA) its tearing strength and tensile strength are improved to EPDM enhancings, the research to the formula and vulcanization process of EPDM-PA systems
It is 52 to show EPDM and PA proportionings:When 35, EPDM materials reach better mechanical property.In addition, recently studies have found that with three
The fibre-reinforced EPDM materials of poly cyanamid have good tensile strength, but also show the processing characteristics of plastics.But these
Enhancements are all to carry out strength improving again on the basis of synthetic EPDM, not to it from the preparation process of EPDM
It is improved.
Carbon fiber is the inorganic polymer fiber that phosphorus content is higher than 90%, has excellent mechanical property and is widely used
In the humidification of all kinds of organic and inorganic materials, also there is relevant report using fibre reinforced EPDM, but be all to synthesize
Carbon fiber modifying is added again on good EPDM, and carbon fiber is directly applied to have not been reported in the synthesis of EPDM.
The content of the invention
Increase carbon fiber from synthesis the object of the present invention is to provide one kind and improve ethylene propylene diene rubber intensity, so as to obtain
Ethylene propylene diene rubber of high intensity and preparation method thereof.
The first object of the present invention is to provide a kind of ethylene propylene diene rubber of high intensity.
To achieve the above object, realized by following technological means：A kind of High-strength ethylene propylene diene monomer, including weighing as follows
Measure part composition：
Further it is optimized for：A kind of High-strength ethylene propylene diene monomer is formed including following parts by weight：
Further it is optimized for：A kind of High-strength ethylene propylene diene monomer is formed including following parts by weight：
Further it is optimized for：The Third monomer is polybutadiene rubber of the 1,2- polybutadiene contents more than 9%
Or the polyisoprene rubber of 3,4- polyisoprene more than 9% or both combination.
Further it is optimized for：The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, described
Vanadium series catalyst be VOCl3、VO(P204)2、V(acac)3、VOCl3·nMOH、VO2Cl (trioctylamine), VO2Cl33 (phosphorus
Sour tributyl), VO (OH) (8-hydroxy-quinoline)2Or VO (OH) (ɑ-cupron)2One or more of combination, wherein M
For the alkyl of C5~C8,2.5≤n≤3.5；The alkyl aluminum compound is trimethyl aluminium, triethyl aluminum, ethylaluminum two
The combination of one or more of aluminium, ethyl aluminum dichloride, aluminium diethyl monochloride or dichloro aluminium isobutyl；The activation accelerating agent is
Ethyl trichloroacetate, CH3Cl、CH2Cl2Or CHCl3One or more of combination.
Further it is optimized for：The organic solvent is the saturated alkane of C5~C10.
Further it is optimized for：The terminator is sodium dimethyl dithiocarbamate, in sodium polysulfide, sodium nitrite
One or more combination.
Further it is optimized for：The stabilizer is lead sulfate tribasic, dibasic lead phosphite, dibasic lead stearate
One or more of combination.
The second object of the present invention is to provide a kind of preparation method of High-strength ethylene propylene diene monomer.To realize above-mentioned mesh
, it is realized by following technological means：A kind of preparation method of High-strength ethylene propylene diene monomer, includes the following steps：
(1) preparation of modified carbon fiber：Carbon fiber is put into soybean oil and is stirred, taking-up drains to obtain the final product；
(2) each raw material is weighed according to components by weight percent；
(3) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added to and use nitrogen in advance
In transposed reaction kettle, ethylene and propylene mixed gas are passed through into reaction kettle, 0.5~1.8MPa of pressure, temperature 40 are set
~60 DEG C, 40~50min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(4) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (3), and transfers the solution into flash distillation
In tank, 0.6~1.0MPa of pressure is set, 60~80 DEG C of temperature, 70~80min of flash distillation, the MONOMER RECOVERY evaporated, remaining the
Two colloidal solutions；
(5) ash disposal：Stabilizer is added in the second colloidal solution of gained into (4), normal temperature and pressure reacts 50~60min,
Up to the 3rd colloidal solution；
(6) precipitation：3rd colloidal solution of gained in (5) is transferred in flocculate tank, control pressure 0.35~
0.45MPa, 80~95 DEG C of temperature remove solvent after flocculation, obtain colloid；
(7) it is dry：The colloid of gained in (6) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Beneficial effects of the present invention are：Carbon fiber is placed in soybean oil after being modified, can be introduced on the surface of carbon fiber
A certain amount of active group, such as hydroxyl (- OH), carboxyl (- COOH), and the surface roughness of carbon fiber also increases.It is modified
Carbon fiber is added into ethylene, propylene and environment existing for Third monomer, and modified carbon fiber can pass through the active group on surface
With Third monomer polymerization occurs for group, and Third monomer on the other hand can be with ethylene, propylene polymerization, so modified carbon fiber quilt
It is grafted on the polymer formed after Third monomer and ethylene, propylene polymerization, is formed by the poly- of modified carbon fiber weave in
Object structure is closed, this pilotaxitic texture can increase the integral strength of finally formed polymer；Inherently a kind of intensity of carbon fiber
Very high substance, fibrous structure so that its tensile strength and fracture strength are all very high, and it is single that modified carbon fiber is entrained in the 3rd
In the polymer that body is formed with ethylene, propylene, the integral strength of polymer can be promoted, finally obtains the ethylene-propylene-diene monomer of high intensity
Glue.
Specific embodiment
Invention is described in further detail below by specific embodiment, following embodiment is descriptive, is not to limit
Protection scope of the present invention of property.
Embodiment 1
A kind of High-strength ethylene propylene diene monomer is formed including following parts by weight：
The Third monomer is polybutadiene rubber of the 1,2- polybutadiene contents 9%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VOCl3, the alkyl aluminum compound is trimethyl aluminium, and the activation accelerating agent is ethyl trichloroacetate.
The organic solvent is hexane.
The terminator is sodium dimethyl dithiocarbamate.
The stabilizer is lead sulfate tribasic.
A kind of preparation method of High-strength ethylene propylene diene monomer, includes the following steps：
(1) preparation of modified carbon fiber：Carbon fiber is put into soybean oil and is stirred, taking-up drains to obtain the final product；
(2) each raw material is weighed according to components by weight percent；
(3) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added to and use nitrogen in advance
In transposed reaction kettle, ethylene and propylene mixed gas are passed through into reaction kettle, pressure 0.5MPa is set, 40 DEG C of temperature,
40min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(4) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (3), and transfers the solution into flash distillation
In tank, pressure 0.6MPa is set, temperature 60 C flashes 70min, and the MONOMER RECOVERY evaporated is remaining to obtain the second colloidal solution；
(5) ash disposal：Add in stabilizer into (4) in second colloidal solution of gained, normal temperature and pressure react 50min to get
3rd colloidal solution；
(6) precipitation：3rd colloidal solution of gained in (5) is transferred in flocculate tank, control pressure 0.35MPa, temperature
80 DEG C, solvent is removed after flocculation, obtains colloid；
(7) it is dry：The colloid of gained in (6) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 2
A kind of High-strength ethylene propylene diene monomer is formed including following parts by weight：
The Third monomer is polyisoprene rubber of the 3,4- polyisoprene 9%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VO (P204)2, the alkyl aluminum compound is triethyl aluminum, and the activation accelerating agent is CH3Cl。
The organic solvent is octane.
The terminator is sodium polysulfide.
The stabilizer is dibasic lead phosphite.
A kind of preparation method of High-strength ethylene propylene diene monomer, includes the following steps：
(1) preparation of modified carbon fiber：Carbon fiber is put into soybean oil and is stirred, taking-up drains to obtain the final product；
(2) each raw material is weighed according to components by weight percent；
(3) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added to and use nitrogen in advance
In transposed reaction kettle, ethylene and propylene mixed gas are passed through into reaction kettle, pressure 0.6MPa is set, temperature 50 C,
50min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(4) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (3), and transfers the solution into flash distillation
In tank, pressure 1.0MPa is set, 80 DEG C of temperature flashes 80min, and the MONOMER RECOVERY evaporated is remaining to obtain the second colloidal solution；
(5) ash disposal：Add in stabilizer into (4) in second colloidal solution of gained, normal temperature and pressure react 60min to get
3rd colloidal solution；
(6) precipitation：3rd colloidal solution of gained in (5) is transferred in flocculate tank, control pressure 0.45MPa, temperature
95 DEG C, solvent is removed after flocculation, obtains colloid；
(7) it is dry：The colloid of gained in (6) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 3
A kind of High-strength ethylene propylene diene monomer is formed including following parts by weight：
The Third monomer is polybutadiene rubber of the 1,2- polybutadiene contents more than 16%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For V (acac)3, the alkyl aluminum compound is two aluminium of ethylaluminum, and the activation accelerating agent is CH2Cl2。
The organic solvent is pentane.
The terminator is sodium nitrite.
The stabilizer is dibasic lead stearate.
A kind of preparation method of High-strength ethylene propylene diene monomer, includes the following steps：
(1) preparation of modified carbon fiber：Carbon fiber is put into soybean oil and is stirred, taking-up drains to obtain the final product；
(2) each raw material is weighed according to components by weight percent；
(3) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added to and use nitrogen in advance
In transposed reaction kettle, ethylene and propylene mixed gas are passed through into reaction kettle, pressure 0.7MPa is set, 42 DEG C of temperature,
42min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(4) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (3), and transfers the solution into flash distillation
In tank, pressure 0.7MPa is set, 65 DEG C of temperature flashes 75min, and the MONOMER RECOVERY evaporated is remaining to obtain the second colloidal solution；
(5) ash disposal：Add in stabilizer into (4) in second colloidal solution of gained, normal temperature and pressure react 55min to get
3rd colloidal solution；
(6) precipitation：3rd colloidal solution of gained in (5) is transferred in flocculate tank, control pressure 0.38MPa, temperature
85 DEG C, solvent is removed after flocculation, obtains colloid；
(7) it is dry：The colloid of gained in (6) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 4
A kind of High-strength ethylene propylene diene monomer is formed including following parts by weight：
The Third monomer is polyisoprene rubber of the 3,4- polyisoprene 15%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VOCl3·3C5H12OH, the alkyl aluminum compound are ethyl aluminum dichloride, and the activation accelerating agent is trichloroacetic acid second
Ester and CH3The combination of Cl.
The organic solvent is heptane.
The terminator is sodium polysulfide.
The stabilizer is dibasic lead phosphite.
A kind of preparation method of High-strength ethylene propylene diene monomer, includes the following steps：
(1) preparation of modified carbon fiber：Carbon fiber is put into soybean oil and is stirred, taking-up drains to obtain the final product；
(2) each raw material is weighed according to components by weight percent；
(3) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added to and use nitrogen in advance
In transposed reaction kettle, ethylene and propylene mixed gas are passed through into reaction kettle, pressure 0.5MPa is set, 48 DEG C of temperature,
48min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(4) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (3), and transfers the solution into flash distillation
In tank, pressure 0.8MPa is set, temperature 70 C flashes 80min, and the MONOMER RECOVERY evaporated is remaining to obtain the second colloidal solution；
(5) ash disposal：Add in stabilizer into (4) in second colloidal solution of gained, normal temperature and pressure react 60min to get
3rd colloidal solution；
(6) precipitation：3rd colloidal solution of gained in (5) is transferred in flocculate tank, control pressure 0.38MPa, temperature
82 DEG C, solvent is removed after flocculation, obtains colloid；
(7) it is dry：The colloid of gained in (6) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 5
A kind of High-strength ethylene propylene diene monomer is formed including following parts by weight：
The Third monomer is polybutadiene rubber and 3,4- poly- isoamyl of the 1,2- polybutadiene contents more than 12%
Diene 13% polyisoprene rubber combination.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VO2Cl33 (tributyl phosphates), the alkyl aluminum compound are aluminium diethyl monochloride, and the activation accelerating agent is
CH2Cl2With CH3The combination of Cl.
The organic solvent is octane.
The terminator is the combination of sodium dimethyl dithiocarbamate and sodium polysulfide.
The stabilizer is the combination of lead sulfate tribasic and dibasic lead phosphite.
A kind of preparation method of High-strength ethylene propylene diene monomer, includes the following steps：
(1) preparation of modified carbon fiber：Carbon fiber is put into soybean oil and is stirred, taking-up drains to obtain the final product；
(2) each raw material is weighed according to components by weight percent；
(3) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added to and use nitrogen in advance
In transposed reaction kettle, ethylene and propylene mixed gas are passed through into reaction kettle, pressure 0.7MPa is set, temperature 45 C,
50min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(4) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (3), and transfers the solution into flash distillation
In tank, pressure 1.0MPa is set, 80 DEG C of temperature flashes 70min, and the MONOMER RECOVERY evaporated is remaining to obtain the second colloidal solution；
(5) ash disposal：Add in stabilizer into (4) in second colloidal solution of gained, normal temperature and pressure react 60min to get
3rd colloidal solution；
(6) precipitation：3rd colloidal solution of gained in (5) is transferred in flocculate tank, control pressure 0.43MPa, temperature
95 DEG C, solvent is removed after flocculation, obtains colloid；
(7) it is dry：The colloid of gained in (6) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Comparative example
A kind of ethylene propylene diene rubber is formed including following parts by weight：
The Third monomer is polybutadiene rubber and 3,4- poly- isoamyl of the 1,2- polybutadiene contents more than 16%
Diene 15% polyisoprene rubber combination.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VO (OH) (8-hydroxy-quinoline)2, the alkyl aluminum compound is dichloro aluminium isobutyl, and the activation accelerating agent is three
Ethyl chloroacetate and CHCl3Combination.
The organic solvent is hexane.
The terminator is the combination of sodium dimethyl dithiocarbamate and sodium nitrite.
The stabilizer is the combination of lead sulfate tribasic and dibasic lead stearate.
A kind of preparation method of ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added in advance through nitrogen
In transposed reaction kettle, ethylene and propylene mixed gas are passed through into reaction kettle, pressure 0.7MPa is set, temperature 45 C,
50min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(3) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (2), and transfers the solution into flash distillation
In tank, pressure 1.0MPa is set, 80 DEG C of temperature flashes 70min, and the MONOMER RECOVERY evaporated is remaining to obtain the second colloidal solution；
(4) ash disposal：Add in stabilizer into (3) in second colloidal solution of gained, normal temperature and pressure react 60min to get
3rd colloidal solution；
(5) precipitation：3rd colloidal solution of gained in (4) is transferred in flocculate tank, control pressure 0.45MPa, temperature
87 DEG C, solvent is removed after flocculation, obtains colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Ethylene propylene diene rubber obtained by above-described embodiment and comparative example is measured into raw rubber according to GB/T1232.1-2016
Can, test result is represented for 125 DEG C with ML (1+4)；Using mooney's viscosimeter by GB/T1233-1992 test rubber compounds 120,
Mooney scorch time t at 130,140 and 160 DEG C5With vulcanization time t35And vulcanization index △ t30Etc. parameters；According to GB/
T16584-1996 tests the vulcanization characteristics of rubber, and the tensile property of gained rubber is tested according to GB/T528-2009, all
Test result is as shown in table 1.
Properties, coke burning performance, curability and the tensile property of 1 gained rubber of table
From data in table, before addition modified carbon fiber, the ethylene propylene diene rubber of modified carbon fiber is with the addition of
It is suitable with the properties, coke burning performance and curability of the ethylene propylene diene rubber that is not added with modified carbon fiber, but add and change
After property carbon fiber, the tensile property of ethylene propylene diene rubber is greatly improved.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of High-strength ethylene propylene diene monomer, which is characterized in that formed including following parts by weight：
2. a kind of High-strength ethylene propylene diene monomer according to claim 1, which is characterized in that including following parts by weight group
Into：
3. a kind of High-strength ethylene propylene diene monomer according to claim 2, which is characterized in that including following parts by weight group
Into：
4. a kind of High-strength ethylene propylene diene monomer according to any one of claim 1 to 3, which is characterized in that described
Third monomer is polybutadiene rubber or 3,4- polyisoprene of the 1,2- polybutadiene contents more than 9% more than 9%
Polyisoprene rubber or both combination.
5. a kind of High-strength ethylene propylene diene monomer according to any one of claim 1 to 3, which is characterized in that described
Catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, and the vanadium series catalyst is VOCl3、VO
(P204)2、V(acac)3、VOCl3·nMOH、VO2Cl (trioctylamine), VO2Cl33 (tributyl phosphates), VO (OH) (eight hydroxyls
Base quinoline)2Or VO (OH) (ɑ-cupron)2One or more of combination, wherein M be C5~C8 alkyl, 2.5≤n≤
3.5；The alkyl aluminum compound is trimethyl aluminium, triethyl aluminum, two aluminium of ethylaluminum, ethyl aluminum dichloride, a chlorine diethyl
The combination of one or more of base aluminium or dichloro aluminium isobutyl；The activation accelerating agent is ethyl trichloroacetate, CH3Cl、
CH2Cl2Or CHCl3One or more of combination.
6. a kind of High-strength ethylene propylene diene monomer according to any one of claim 1 to 3, which is characterized in that described
Organic solvent is the saturated alkane of C5~C10.
7. a kind of High-strength ethylene propylene diene monomer according to any one of claim 1 to 3, which is characterized in that described
Terminator is the combination of one or more of sodium dimethyl dithiocarbamate, sodium polysulfide, sodium nitrite.
8. a kind of High-strength ethylene propylene diene monomer according to any one of claim 1 to 3, which is characterized in that described
Stabilizer is the combination of one or more of lead sulfate tribasic, dibasic lead phosphite, dibasic lead stearate.
9. a kind of preparation method of High-strength ethylene propylene diene monomer according to any one of claim 1 to 3, feature exist
In including the following steps：
(1) preparation of modified carbon fiber：Carbon fiber is put into soybean oil and is stirred, taking-up drains to obtain the final product；
(2) each raw material is weighed according to components by weight percent；
(3) it polymerize：The Third monomer weighed, modified carbon fiber, catalyst, organic solvent are added to and use nitrogen displacement in advance
In the reaction kettle crossed, ethylene and propylene mixed gas are passed through into reaction kettle, 0.5~1.8MPa of pressure, temperature 40~60 are set
DEG C, 40~50min is reacted under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(4) MONOMER RECOVERY：Terminator is added in the first colloidal solution of gained into (3), and is transferred the solution into flash tank,
0.6~1.0MPa of pressure is set, and 60~80 DEG C of temperature flashes 70~80min, and the MONOMER RECOVERY evaporated is remaining to obtain the second glue
Solution；
(5) ash disposal：Add in stabilizer into (4) in second colloidal solution of gained, normal temperature and pressure react 50~60min to get
3rd colloidal solution；
(6) precipitation：3rd colloidal solution of gained in (5) is transferred in flocculate tank, 0.35~0.45MPa of control pressure, temperature
80~95 DEG C of degree removes solvent after flocculation, obtains colloid；
(7) it is dry：The colloid of gained in (6) is dehydrated through dewaterer, drying machine drying is to get final ethylene-propylene-diene monomer
Glue.
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| CN114874394B (en) * | 2021-02-05 | 2023-11-14 | 中国石油化工股份有限公司 | Ethylene propylene diene monomer rubber and preparation method and application thereof |
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