CN108976348A - A kind of method that rotary evaporation assists the maleic anhydride for preparing high grafting rate to be grafted ethylene propylene diene rubber - Google Patents
A kind of method that rotary evaporation assists the maleic anhydride for preparing high grafting rate to be grafted ethylene propylene diene rubber Download PDFInfo
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- CN108976348A CN108976348A CN201810730760.6A CN201810730760A CN108976348A CN 108976348 A CN108976348 A CN 108976348A CN 201810730760 A CN201810730760 A CN 201810730760A CN 108976348 A CN108976348 A CN 108976348A
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- epdm
- maleic anhydride
- rotary evaporation
- initiator
- mah
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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
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/04—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethene-propene copolymers
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The present invention provides the methods that a kind of rotary evaporation auxiliary prepares the maleic anhydride grafting ethylene propylene diene rubber of high grafting rate, EPDM and initiator cumyl peroxide are added to progress vacuum rotary steam pretreatment in rotary evaporation bottle first, penetrate into initiator in EPDM；Then using the EPDM pre-processed as raw material, using MAH as grafted monomers, the two is added to melt blending in torque rheometer after evenly mixing and is grafted, and prepares maleic anhydride grafting ethylene propylene diene rubber (EPDM-g-MAH).The EPDM-g-MAH of low-gel content, high grafting rate can be made using the initiator of less content by the present invention, and grafting rate is up to 0.53%-1.21%.The EPDM-g-MAH of preparation can effectively improve the compatibility with polar polymer coblended interface.The utilization rate of initiator DCP can effectively be improved by preparing EPDM-g-MAH using rotary evaporation.
Description
Technical field
The invention belongs to chemical fields, are related to a kind of macromolecule modified method, specifically a kind of rotary evaporation
The method that auxiliary prepares maleic anhydride grafting ethylene propylene diene rubber (EPDM-g-MAH) of high grafting rate.
Background technique
EPDM is the terpolymer of ethylene, propylene and non-conjugated diene hydrocarbon, have good resistance to oxidation, ozone-resistant,
It the advantages that low temperature resistant, shock resistance, good thermal stability, is blended with engineering plastics, can greatly improve the impact strength of engineering plastics
And lower temperature resistance.But EPDM itself be it is non-polar, it is poor with polyamide, polyester isopolarity Compatibility in Plastics, in order to improve
With the compatibility of these polar plas, the grafting to polar group is carried out is generally required.Wherein, maleic anhydride is most widely used
A kind of selection.
EPDM graft modification usually has melt-blending process grafting and grafting solution method.Grafting solution method, general elapsed time
It is long, need to consume a large amount of toxic solvents, higher cost is larger to actual bodily harm, and preparation process can not be continuous, produces in enormous quantities not
Reality.Shorter the time required to melt-blending process grafting, production equipment is simple, and technological operation is simple, at low cost, can be continuous large quantities of
Amount production.But existing melt-blending process grafting rate is low, gel content is high, and obtained EPDM has pungent smell.
Summary of the invention
For above-mentioned technical problem in the prior art, the present invention provides a kind of rotary evaporations to assist the high grafting of preparation
The method of the maleic anhydride grafting ethylene propylene diene rubber of rate, this rotary evaporation auxiliary prepare the Malaysia of high grafting rate
The EPDM-g-MAH grafting rate that the method for acid anhydrides grafting ethylene propylene diene rubber will solve to prepare in the prior art is low, gel contains
The technical problem that amount is big, smell is big.
The maleic anhydride for preparing high grafting rate the present invention provides a kind of rotary evaporation auxiliary is grafted ethylene propylene diene rubber
Method, include the following steps:
1) EPDM, initiator DCP and maleic anhydride are weighed according to mass percent；
EPDM 95.14wt% -99wt%；
Initiator cumyl peroxide 0.0099wt% -0.0951wt%；
Maleic anhydride 0.99wt% -4.7573wt%；
2) EPDM and initiator are added to progress vacuum rotary steam pretreatment, the water-bath of Rotary Evaporators in Rotary Evaporators
Pot water temperature is 40-80 DEG C, and the rotary evaporation time is 0.5-3h, and rotary evaporation revolving speed is 20-120rpm/min, permeates initiator
Into EPDM；
3) using the EPDM pre-processed as raw material, using maleic anhydride as grafted monomers, it is added to torque flow after evenly mixing
Become melt blending in instrument to be cut into small pieces, obtained maleic anhydride grafting ethylene propylene diene rubber, during melt blending, torque rheometer
Temperature be 140-200 DEG C, revolving speed 30-70rpm/min, the blendings time be 1-10min.
4), during melt blending, the temperature of torque rheometer is 140-200 DEG C, revolving speed 30-70rpm/min, is blended
Time is 1-10min.
The present invention provides a kind of rotary evaporation auxiliary to prepare maleic anhydride (MAH) grafting ethylene propylene diene rubber (EPDM)
Method, EPDM and suitable initiator cumyl peroxide (DCP) are added in rotary evaporation bottle and are depressurized first
Revolving pretreatment, penetrates into initiator DCP in EPDM；It then is that grafting is single with MAH using the EPDM pre-processed as raw material
Body, the two are added to melt blending grafting in torque rheometer after evenly mixing and prepare maleic anhydride grafting ethylene propylene diene rubber
(EPDM-g-MAH)。
The present invention is compared with prior art, and technological progress is significant.The present invention uses the initiator DCP of less content
The small EPDM-g-MAH of low-gel content, high grafting rate, smell can be made, grafting rate is up to 0.53%-1.21%.Preparation
EPDM-g-MAH can effectively improve the compatibility with polar polymer coblended interface.It is prepared using rotary evaporation
EPDM-g-MAH can effectively improve the utilization rate of initiator DCP.
Specific embodiment
Embodiment 1:
The maleic anhydride for preparing high grafting rate the present invention provides a kind of rotary evaporation auxiliary is grafted ethylene propylene diene rubber
Method, include the following steps:
1) EPDM, initiator DCP and maleic anhydride are weighed according to mass percent；
EPDM 95.14wt% -99wt%；
Initiator cumyl peroxide 0.0099wt% -0.0951wt%；
Maleic anhydride 0.99wt% -4.7573wt%；
2) EPDM and initiator are added to progress vacuum rotary steam pretreatment, the water-bath of Rotary Evaporators in Rotary Evaporators
Pot water temperature is 60 DEG C, and the rotary evaporation time is 1h, and rotary evaporation revolving speed is 60rpm/min, penetrates into initiator in EPDM；
3) using the EPDM pre-processed as raw material, using maleic anhydride as grafted monomers, it is added to torque flow after evenly mixing
Become melt blending in instrument to be cut into small pieces, obtained graft EPDM-g-MAH, during melt blending, be melted using torque rheometer
It is blended, three sections of temperature are 180 DEG C, revolving speed 30rpm/min, and the blend graft time is 4min.
Specifically, the EPDM uses EPDM 4725P (DuPont).
EPDM and initiator DCP are first weighed according to the above component；
Rotary Evaporators relevant parameter is set, EPDM and initiator DCP are added to rotation and steamed by goal condition to be achieved
Rotary evaporation is carried out in hair bottle.After the completion of rotary evaporation, pretreated EPDM cooling preservation is taken out.Open the electricity of torque rheometer
The trizonal temperature of torque rheometer and rotor speed, setting temperature to be achieved is arranged in source, inspection machine situation if normal
Start cleaning robot after degree, the EPDM pre-processed and suitable MAH can be mixed after completing cleaning operation to temperature stabilization
It gets togather and is then added into torque rheometer progress blend graft.Stop being blended after appropriate time, blend is then cut into block
Shape cooling preservation.
Embodiment 2:
A kind of method that rotary evaporation assists the maleic anhydride for preparing high grafting rate to be grafted ethylene propylene diene rubber, including such as
Lower step:
1) EPDM, initiator DCP and maleic anhydride are weighed according to mass percent；
EPDM 95.14wt% -99wt%；
Initiator cumyl peroxide 0.0099wt% -0.0951wt%；
Maleic anhydride 0.99wt% -4.7573wt%；
Using EPDM and initiator as raw material, using maleic anhydride as grafted monomers, it is added to torque rheometer after evenly mixing
Middle melt blending is cut into small pieces, and graft EPDM-g-MAH, the process conditions of direct melt-blending process are made are as follows: uses torque flow
Become instrument melt blending, three sections of temperature of melt blending are 180 DEG C, revolving speed 30rpm/min, and the blend graft time is 4min.
The grafting rate comparison of the EPDM-g-MAH of 1 two methods of table preparation
The above experimental data shows that the EPDM-g-MAH of rotary evaporation preparation compares direct blending under square one
The grafting rate of the EPDM-g-MAH of preparation wants high.
Claims (2)
1. a kind of method that rotary evaporation auxiliary prepares the maleic anhydride grafting ethylene propylene diene rubber of high grafting rate, feature exist
In including the following steps:
1) EPDM, initiator DCP and maleic anhydride are weighed according to mass percent；
EPDM 95.14 wt%—99 wt% ；
Initiator cumyl peroxide 0.0099 wt% -0.0951 wt%；
Maleic anhydride 0.99 wt% -4.7573 wt%；
2) EPDM and initiator are added to progress vacuum rotary steam pretreatment, the water-bath water of Rotary Evaporators in Rotary Evaporators
Temperature is 40-80 DEG C, and the rotary evaporation time is 0.5-3h, and rotary evaporation revolving speed is 20-120rpm/min, penetrates into initiator
In EPDM；
3) using the EPDM pre-processed as raw material, using maleic anhydride as grafted monomers, it is added to torque rheometer after evenly mixing
Middle melt blending is cut into small pieces, obtained maleic anhydride grafting ethylene propylene diene rubber, during melt blending, the temperature of torque rheometer
Degree is 140-200 DEG C, revolving speed 30-70rpm/min, and the blending time is 1-10min.
2. the maleic anhydride grafting ternary second that a kind of rotary evaporation auxiliary according to claim 1 prepares high grafting rate
The method of third rubber, it is characterised in that: the EPDM uses EPDM 4725P.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810730760.6A CN108976348B (en) | 2018-07-05 | 2018-07-05 | Method for preparing maleic anhydride grafted ethylene propylene diene monomer with high grafting rate in auxiliary manner by rotary evaporation method |
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|---|---|---|---|
| CN201810730760.6A CN108976348B (en) | 2018-07-05 | 2018-07-05 | Method for preparing maleic anhydride grafted ethylene propylene diene monomer with high grafting rate in auxiliary manner by rotary evaporation method |
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| CN108976348B CN108976348B (en) | 2020-10-09 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643391A (en) * | 2012-04-19 | 2012-08-22 | 深圳市科聚新材料有限公司 | Ethylene propylene diene monomer grafted maleic anhydride and preparation method thereof |
| CN105131203A (en) * | 2015-07-28 | 2015-12-09 | 绍兴佳华高分子材料股份有限公司 | Preparation method for polypropylene grafted maleic anhydride with high graft ratio and low odor |
| CN105859920A (en) * | 2016-04-19 | 2016-08-17 | 常熟理工学院 | High-grafting-ratio functionalization ethylene-propylene-diene monomer rubber and preparing method thereof |
| CN108192259A (en) * | 2017-12-22 | 2018-06-22 | 华南理工大学 | A kind of EPDM composite elastic body and preparation method thereof |
-
2018
- 2018-07-05 CN CN201810730760.6A patent/CN108976348B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643391A (en) * | 2012-04-19 | 2012-08-22 | 深圳市科聚新材料有限公司 | Ethylene propylene diene monomer grafted maleic anhydride and preparation method thereof |
| CN105131203A (en) * | 2015-07-28 | 2015-12-09 | 绍兴佳华高分子材料股份有限公司 | Preparation method for polypropylene grafted maleic anhydride with high graft ratio and low odor |
| CN105859920A (en) * | 2016-04-19 | 2016-08-17 | 常熟理工学院 | High-grafting-ratio functionalization ethylene-propylene-diene monomer rubber and preparing method thereof |
| CN108192259A (en) * | 2017-12-22 | 2018-06-22 | 华南理工大学 | A kind of EPDM composite elastic body and preparation method thereof |
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