CN105153500B - Preparation method of modified butadiene-acrylonitrile rubber - Google Patents
Preparation method of modified butadiene-acrylonitrile rubber Download PDFInfo
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- CN105153500B CN105153500B CN201510651800.4A CN201510651800A CN105153500B CN 105153500 B CN105153500 B CN 105153500B CN 201510651800 A CN201510651800 A CN 201510651800A CN 105153500 B CN105153500 B CN 105153500B
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Abstract
The invention discloses a preparation method of modified butadiene-acrylonitrile rubber. The method comprises the step of putting 100 parts of NBR, 0.2 to 0.3 part of an initiator, 30 to 36 parts of POE, and 20 to 30 parts of co-polymerized propene by weight into a double-screw extruder for reaction and extrusion, wherein the pitch diameter ratio of the double-screw extruder is 48:1. The method has the advantages that POE resin is grafted on NBR through a grafting reaction, and co-blending with co-polymerized propene is realized, so as to obtain the heat-proof, weather-proof and aging resistant modified butadiene-acrylonitrile rubber under the basis of not impacting other comprehensive performances.
Description
Technical field
The invention belongs to chemical technology field, it is related to a kind of preparation method of modified butadiene acrylonitrile rubber.
Background technology
Nitrile rubber is to be obtained through emulsion polymerization by butadiene and acrylonitrile, and nitrile rubber mainly adopts low temperature emulsion
Polymerization produces, and oil resistivity is fabulous, and wearability is higher, and preferably, bonding force is strong for heat resistance.It is widely used in the various oil resistant rubber systems of system
Product, multiple oil seat gasket, pad, sleeve pipe, flexible package, flexible rubber hose, printer's roll, cable glue material etc., in automobile, aviation, stone
Become requisite elastomeric material in the industries such as oil, duplicating, be a kind of preferable general purpose rubber of combination property, but existing
Nitrile rubber ageing properties are poor.
Content of the invention
The purpose of the present invention is to overcome above-mentioned weak point to provide a kind of preparation method of modified butadiene acrylonitrile rubber.
The purpose of the present invention is achieved in the following ways:
A kind of preparation method of modified butadiene acrylonitrile rubber, the method comprises the following steps:
Take nitrile rubber (nbr) 100 weight portion, initiator 0.2～0.3 weight portion, ethylene-octene copolymer (poe) 30
～36 weight portions, co-polypropylene 20～30 weight portion, prepared by following steps: after first nitrile rubber being plasticated 5 minutes
Discharging after adding initiator, poe to knead 10 minutes obtains nitrile rubber batch mixing, then nitrile rubber batch mixing and co-polypropylene are added
Screw rod lay ratio is extruding pelletization in double screw extruder in the hopper of double screw extruder of 48:1, double screw extruder
Temperature setting is as shown in the table:
| Region | Machine barrel 1 area | Machine barrel 2 area | Machine barrel 3 area | Machine barrel 4 area | Machine barrel 5 area | Machine barrel 6 area |
| Temperature | 100 DEG C～105 DEG C | 105 DEG C～110 DEG C | 110℃ | 115℃ | 115℃ | 120℃ |
| Region | Machine barrel 7 area | Machine barrel 8 area | Machine barrel 9 area | Machine barrel 10 area | Machine barrel 11 area | Machine barrel 12 area |
| Temperature | 120 DEG C～130 DEG C | 160 DEG C～170 DEG C | 180 DEG C～190 DEG C | 200 DEG C～220 DEG C | 190 DEG C～200 DEG C | 180 DEG C～190 DEG C |
The preparation method of above-mentioned modified butadiene acrylonitrile rubber can also pass through following steps:
Take nitrile rubber 100 weight portion, initiator 0.2～0.3 weight portion, ethylene-octene copolymer 30～36 weight portion,
Co-polypropylene 20～30 weight portion, is prepared by following steps: after first nitrile rubber being plasticated 5 minutes add initiator,
Discharging after poe kneads 10 minutes obtains nitrile rubber batch mixing, then nitrile rubber batch mixing is added screw rod lay ratio double for 48:1
In first hopper of screw extruder, in second hopper of double screw extruder of co-polypropylene addition lay ratio 48:1, second
The distance of hopper and the first hopper is 20:48 with the ratio of screw rod overall length, extruding pelletization in double screw extruder, twin-screw extrusion
Machine temperature setting is as shown in the table:
| Region | Machine barrel 1 area | Machine barrel 2 area | Machine barrel 3 area | Machine barrel 4 area | Machine barrel 5 area | Machine barrel 6 area |
| Temperature | 100 DEG C～105 DEG C | 105 DEG C～110 DEG C | 110℃ | 115℃ | 115℃ | 120℃ |
| Region | Machine barrel 7 area | Machine barrel 8 area | Machine barrel 9 area | Machine barrel 10 area | Machine barrel 11 area | Machine barrel 12 area |
| Temperature | 120 DEG C～130 DEG C | 160 DEG C～170 DEG C | 180 DEG C～190 DEG C | 200 DEG C～220 DEG C | 190 DEG C～200 DEG C | 180 DEG C～190 DEG C |
Initiator described in the inventive method is cumyl peroxide (dcp).
The spiral shell of 60-80 rev/min of the screw speed of the double screw extruder described in the inventive method, preferably double screw extruder
60 revs/min of bar rotating speed.
Co-polypropylene, is by propylene monomer c3h6Product with a small amount of vinyl monomer c2h4 (typically 1～4%) copolymerization.Altogether
Because of composition containing ethene in third, compared with homopolymerization pp, material transparent degree, rigidity, glossiness etc. decline, but lower temperature resistance and shock resistance
Performance enhancement.
Beneficial effects of the present invention compared with the prior art: the present invention adopts a kind of safe method, by graft reaction
Poe resin is grafted on nitrile rubber, and is blended with co-polypropylene, on the basis of not affecting other combination properties, obtain
Intensity is good, heat-resisting, weather-proof, ageing-resistant modified NBR.
Specific embodiment
Further illustrate the present invention below by way of specific embodiment.But the detail of embodiment is only used for explaining this
Bright, it should not be construed as limited overall technical solution.
Embodiment 1
Discharging after adding dcp, poe to knead after first nitrile rubber being plasticated 5 minutes according to aforementioned proportion 10 minutes obtains fourth
Nitrile rubber batch mixing, then nitrile rubber batch mixing and co-polypropylene (production of Zhejiang Guang Yuan petrochemical industry Co., Ltd) are added screw rod lay ratio
In the hopper of the double screw extruder for 48:1, extruding pelletization in double screw extruder, the screw speed of double screw extruder
60 revs/min, double screw extruder temperature setting is as shown in the table:
| Region | Machine barrel 1 area | Machine barrel 2 area | Machine barrel 3 area | Machine barrel 4 area | Machine barrel 5 area | Machine barrel 6 area |
| Temperature | 100 DEG C～105 DEG C | 105 DEG C～110 DEG C | 110℃ | 115℃ | 115℃ | 120℃ |
| Region | Machine barrel 7 area | Machine barrel 8 area | Machine barrel 9 area | Machine barrel 10 area | Machine barrel 11 area | Machine barrel 12 area |
| Temperature | 120 DEG C～130 DEG C | 160 DEG C～170 DEG C | 180 DEG C～190 DEG C | 200 DEG C～220 DEG C | 190 DEG C～200 DEG C | 180 DEG C～190 DEG C |
The modified butadiene acrylonitrile rubber that embodiment 1 method is obtained prepares detection strip through conventional method, detects its property
Can be as follows:
| Detection project | Detection method | Detection data |
| Tensile strength mpa | gb/t 1040-92 | 19.4 |
| Elongation at break % | gb/t 1040-92 | 460 |
| Aging condition | 100℃±2℃168h | |
| Aging after-drawing intensity mpa | gb/t 1040-92 | 18.6 |
| Aging rear elongation at break % | gb/t 1040-92 | 420 |
| Tensile strength rate of change % | / | 4 |
| Elongation at break rate of change % | / | 9 |
Note: compare the pure glue of nitrile rubber, the intensity of elastomeric compound, heat resistance, resistance to ag(e)ing have and significantly improve very much.
Embodiment 2
Discharging after adding dcp, poe to knead after first nitrile rubber being plasticated 5 minutes according to aforementioned proportion 10 minutes obtains fourth
In nitrile rubber batch mixing, then the first hopper of double screw extruder that nitrile rubber batch mixing addition screw rod lay ratio is 48:1, altogether
Polypropylene adds in second hopper of double screw extruder of lay ratio 48:1, the distance of the second hopper and the first hopper and screw rod
The ratio of overall length is 20:48, extruding pelletization in double screw extruder, 60 revs/min of the screw speed of double screw extruder, twin-screw
Extruder temperature setting is as shown in the table:
| Region | Machine barrel 1 area | Machine barrel 2 area | Machine barrel 3 area | Machine barrel 4 area | Machine barrel 5 area | Machine barrel 6 area |
| Temperature | 100 DEG C～105 DEG C | 105 DEG C～110 DEG C | 110℃ | 115℃ | 115℃ | 120℃ |
| Region | Machine barrel 7 area | Machine barrel 8 area | Machine barrel 9 area | Machine barrel 10 area | Machine barrel 11 area | Machine barrel 12 area |
| Temperature | 120 DEG C～130 DEG C | 160 DEG C～170 DEG C | 180 DEG C～190 DEG C | 200 DEG C～220 DEG C | 190 DEG C～200 DEG C | 180 DEG C～190 DEG C |
The modified butadiene acrylonitrile rubber that embodiment 2 method is obtained prepares detection strip through conventional method, detects its property
Can be as follows:
| Detection project | Detection method | Detection data |
| Tensile strength mpa | gb/t 1040-92 | 19.8 |
| Elongation at break % | gb/t 1040-92 | 470 |
| Aging condition | 100℃±2℃168h | |
| Aging after-drawing intensity mpa | gb/t 1040-92 | 19.2 |
| Aging rear elongation at break % | gb/t 1040-92 | 430 |
| Tensile strength rate of change % | / | 5 |
| Elongation at break rate of change % | / | 10 |
Note: compare the pure glue of nitrile rubber, the intensity of elastomeric compound, heat resistance, resistance to ag(e)ing have and significantly improve very much.
Claims (5)
1. a kind of preparation method of modified butadiene acrylonitrile rubber is it is characterised in that the method comprises the following steps:
Take nitrile rubber 100 weight portion, initiator 0.2～0.3 weight portion, ethylene-octene copolymer 30～36 weight portion, copolymerization
Propylene 20～30 weight portion；Described co-polypropylene, is by propylene monomer c3h6With 1～4% vinyl monomer c2h4The product of copolymerization
Thing；Prepared by following steps:
Discharging after adding initiator, ethylene-octene copolymer to knead after first nitrile rubber being plasticated 5 minutes 10 minutes obtains butyronitrile
Rubber compound, then nitrile rubber batch mixing and co-polypropylene are added the hopper of the double screw extruder that screw rod lay ratio is 48:1
In, extruding pelletization in double screw extruder, double screw extruder temperature setting is as shown in the table:
2. a kind of preparation method of modified butadiene acrylonitrile rubber is it is characterised in that the method comprises the following steps:
Take nitrile rubber 100 weight portion, initiator 0.2～0.3 weight portion, ethylene-octene copolymer 30～36 weight portion, copolymerization
Propylene 20～30 weight portion；Described co-polypropylene, is by propylene monomer c3h6With 1～4% vinyl monomer c2h4The product of copolymerization
Thing；Prepared by following steps:
Discharging after adding initiator, ethylene-octene copolymer to knead after first nitrile rubber being plasticated 5 minutes 10 minutes obtains butyronitrile
Rubber compound, then nitrile rubber batch mixing is added in the first hopper of the double screw extruder that screw rod lay ratio is 48:1, copolymerization
Propylene adds in second hopper of double screw extruder of lay ratio 48:1, and the second hopper is total with screw rod with the distance of the first hopper
The ratio of length is 20:48, extruding pelletization in double screw extruder, and double screw extruder temperature setting is as shown in the table:
3. the preparation method of modified butadiene acrylonitrile rubber according to claim 1 and 2 was it is characterised in that described initiator was
Oxidation diisopropylbenzene (DIPB).
4. the preparation method of modified butadiene acrylonitrile rubber according to claim 1 and 2 is it is characterised in that described twin-screw extrusion
60-80 rev/min of the screw speed of machine.
5. the preparation method of modified butadiene acrylonitrile rubber according to claim 4 is it is characterised in that described double screw extruder
60 revs/min of screw speed.
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| CN201510651800.4A CN105153500B (en) | 2015-10-10 | 2015-10-10 | Preparation method of modified butadiene-acrylonitrile rubber |
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| CN105153500B true CN105153500B (en) | 2017-01-18 |
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| CN109233019A (en) * | 2018-08-01 | 2019-01-18 | 江苏益帆高分子材料有限公司 | A kind of nitrile rubber of high flame retardant and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313356A (en) * | 2001-04-04 | 2001-09-19 | 南开大学 | Modified nitrile rubber and its preparing process |
| CN102516558A (en) * | 2011-12-16 | 2012-06-27 | 山东大学 | Polysiloxane modified nitrile rubber, synthesis method and preparation of vulcanized rubber |
| CN103304857A (en) * | 2012-03-16 | 2013-09-18 | 比亚迪股份有限公司 | Preparation method of modified nitrile rubber and modified nitrile rubber |
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- 2015-10-10 CN CN201510651800.4A patent/CN105153500B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313356A (en) * | 2001-04-04 | 2001-09-19 | 南开大学 | Modified nitrile rubber and its preparing process |
| CN102516558A (en) * | 2011-12-16 | 2012-06-27 | 山东大学 | Polysiloxane modified nitrile rubber, synthesis method and preparation of vulcanized rubber |
| CN103304857A (en) * | 2012-03-16 | 2013-09-18 | 比亚迪股份有限公司 | Preparation method of modified nitrile rubber and modified nitrile rubber |
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