CN101402710A - Production process for grafting maleic anhydride with ethylene propylene rubber solution method - Google Patents
Production process for grafting maleic anhydride with ethylene propylene rubber solution method Download PDFInfo
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- CN101402710A CN101402710A CNA2008102361051A CN200810236105A CN101402710A CN 101402710 A CN101402710 A CN 101402710A CN A2008102361051 A CNA2008102361051 A CN A2008102361051A CN 200810236105 A CN200810236105 A CN 200810236105A CN 101402710 A CN101402710 A CN 101402710A
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- propylene rubber
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- maleic anhydride
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Abstract
The invention discloses a production method of grafting maleic anhydride by an ethylene-propylene rubber solution method. The method is characterized in comprising the following steps: raw materials of ethylene-propylene rubber, benzoperoxide and maleic anhydride are respectively dissolved in dimethylbenzene to be prepared into solutions; the 3 solutions are filled into a reaction kettle in sequence, the reaction kettle is vacuumized and filled in with nitrogen, solutions in the kettle react for 5 minutes to 20 minutes with the temperature controlled between 110 DEG C to 180 DEG C and a stirring speed between 30 r/min to 100 r/min, and then ethylene-propylene rubber and maleic anhydride graft solution is obtained; and spray drying is carried out to the ethylene-propylene rubber and maleic anhydride graft solution so as to obtain powder ethylene-propylene rubber and maleic anhydride graft with particle size between 200nm and 50um. The method can save energy consumption by about 60 percent, improves grafting rate to 1.5 percent to 8.2 percent, has little residue of dimethylbenzene, damages the molecular structure of the graft during preparation process and has even dispersion and good compatibility when being applied to toughening engineering plastics.
Description
Technical field
The present invention relates to a kind of production method of grafting production method, particularly a kind of process for grafting maleic anhydride with ethylene propylene rubber solution.
Background technology
Ethylene-propylene rubber(EPR) (EPR) has good physical and chemical performance, and the application of aspect such as toughness reinforcing and anti-ozone ageing is very outstanding at engineering plastics.But,, be difficult to and the polar polymer blend because ethylene-propylene rubber(EPR) (EPR) belongs to non-polar rubber.Therefore ethylene-propylene rubber(EPR) (EPR) is carried out modification and seem particularly important with the consistency that strengthens itself and polar polymer.All adopt the distillation drying means to carry out gas-liquid separation in the graft reaction of ethylene-propylene rubber(EPR) of the prior art and maleic anhydride, reaction must have pulverizing process.The base defective is: energy consumption height, the residual height of dimethylbenzene, and reaction gained mixture is bonded to piece, and it is big to pulverize difficulty; And in the mechanical force course of processing, destroyed the structure of reactant, reduced percentage of grafting.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and the production method of a kind of method advantages of simple, energy consumption is little, percentage of grafting is high process for grafting maleic anhydride with ethylene propylene rubber solution is provided.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of production method of process for grafting maleic anhydride with ethylene propylene rubber solution, it is characterized in that, its step is,
(1) raw material ethylene-propylene rubber(EPR), benzoyl peroxide and maleic anhydride are dissolved in dimethylbenzene respectively, make solution;
(2) inject above-mentioned 3 kinds of solution successively in reactor, vacuumize the back nitrogen injection, controlled temperature 110-180 ℃, 30-100 rev/min of control stirring velocity reacted 5-20 minute, got ethylene-propylene rubber(EPR) and maleic anhydride grafts solution;
(3) to ethylene-propylene rubber(EPR) and the spray-dried processing of maleic anhydride grafts solution, making particle diameter is Powdered ethylene-propylene rubber(EPR) and the maleic anhydride grafts of 200nm-50um.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described production method is characterized in, described ethylene-propylene rubber(EPR) is terpolymer EP rubber or ethylene propylene rubber.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described production method is characterized in, in step (2), the vacuum tightness after vacuumizing is 0.001-0.01Mpa.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described production method is characterized in, when the spray drying treatment described in the step (3), reclaims dimethylbenzene with retrieving arrangement, and the dimethylbenzene that reclaims is entered repeated use in the step (1).So not only can eliminate environmental pollution, also can economize in raw materials.
In technical solution of the present invention; reactor vacuumizes the back nitrogen injection, its objective is protection peroxide radical concentration, extracts air (comprising airborne oxygen) and nitrogen injection; reduce oxygen ion concentration significantly, improved the grafting efficiency of ethylene-propylene rubber(EPR) and maleic anhydride.The present invention can make ultra-fine powder with the grafting reactant spraying drying of ethylene-propylene rubber(EPR) and maleic anhydride.Measure by ordinary method of the prior art through the contriver, find the inventive method compared with prior art, but the present invention's energy efficient about 60%, and the percentage of grafting of ethylene-propylene rubber(EPR) and maleic anhydride can be brought up to about 1.5%-8.2%; Dimethylbenzene is residual few in the prepared reactant, only is about 0.001%; Test according to a conventional method and test through the contriver, produce the molecular structure that does not destroy grafts in the process in the present invention; It is made in the toughness reinforcing engineering plastics of land used, be uniformly dispersed, consistency is good.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.A kind of production method of process for grafting maleic anhydride with ethylene propylene rubber solution, its step be,
(1) raw material ethylene-propylene rubber(EPR), benzoyl peroxide and maleic anhydride are dissolved in dimethylbenzene respectively, make solution;
(2) in reactor, inject above-mentioned 3 kinds of solution successively, vacuumize the back nitrogen injection, 110 ℃ of controlled temperature, 30 rev/mins of control stirring velocitys were reacted 20 minutes, got ethylene-propylene rubber(EPR) and maleic anhydride grafts solution;
(3) to ethylene-propylene rubber(EPR) and the spray-dried processing of maleic anhydride grafts solution, making particle diameter is Powdered ethylene-propylene rubber(EPR) and the maleic anhydride grafts of 200nm-50um.
Embodiment 2.A kind of production method of process for grafting maleic anhydride with ethylene propylene rubber solution, its step be,
(1) raw material ethylene-propylene rubber(EPR), benzoyl peroxide and maleic anhydride are dissolved in dimethylbenzene respectively, make solution;
(2) in reactor, inject above-mentioned 3 kinds of solution successively, vacuumize the back nitrogen injection, 180 ℃ of controlled temperature, 100 rev/mins of control stirring velocitys were reacted 5 minutes, got ethylene-propylene rubber(EPR) and maleic anhydride grafts solution;
(3) to ethylene-propylene rubber(EPR) and the spray-dried processing of maleic anhydride grafts solution, making particle diameter is Powdered ethylene-propylene rubber(EPR) and the maleic anhydride grafts of 200nm-50um.
Embodiment 3.A kind of production method of process for grafting maleic anhydride with ethylene propylene rubber solution, its step be,
(1) raw material ethylene-propylene rubber(EPR), benzoyl peroxide and maleic anhydride are dissolved in dimethylbenzene respectively, make solution;
(2) in reactor, inject above-mentioned 3 kinds of solution successively, vacuumize the back nitrogen injection, 150 ℃ of controlled temperature, 65 rev/mins of control stirring velocitys were reacted 10 minutes, got ethylene-propylene rubber(EPR) and maleic anhydride grafts solution;
(3) to ethylene-propylene rubber(EPR) and the spray-dried processing of maleic anhydride grafts solution, making particle diameter is Powdered ethylene-propylene rubber(EPR) and the maleic anhydride grafts of 200nm-50um.
Embodiment 4.A kind of production method of process for grafting maleic anhydride with ethylene propylene rubber solution, its step be,
(1) raw material ethylene-propylene rubber(EPR), benzoyl peroxide and maleic anhydride are dissolved in dimethylbenzene respectively, make solution;
(2) in reactor, inject above-mentioned 3 kinds of solution successively, vacuumize the back nitrogen injection, 130 ℃ of controlled temperature, 50 rev/mins of control stirring velocitys were reacted 8 minutes, got ethylene-propylene rubber(EPR) and maleic anhydride grafts solution;
(3) to ethylene-propylene rubber(EPR) and the spray-dried processing of maleic anhydride grafts solution, making particle diameter is Powdered ethylene-propylene rubber(EPR) and the maleic anhydride grafts of 200nm-50um.
Embodiment 5.A kind of production method of process for grafting maleic anhydride with ethylene propylene rubber solution, its step be,
(1) raw material ethylene-propylene rubber(EPR), benzoyl peroxide and maleic anhydride are dissolved in dimethylbenzene respectively, make solution;
(2) in reactor, inject above-mentioned 3 kinds of solution successively, vacuumize the back nitrogen injection, 170 ℃ of controlled temperature, 80 rev/mins of control stirring velocitys were reacted 15 minutes, got ethylene-propylene rubber(EPR) and maleic anhydride grafts solution;
(3) to ethylene-propylene rubber(EPR) and the spray-dried processing of maleic anhydride grafts solution, making particle diameter is Powdered ethylene-propylene rubber(EPR) and the maleic anhydride grafts of 200nm-50um.
Embodiment 6.In any one described production method of embodiment 1-5, described ethylene-propylene rubber(EPR) is terpolymer EP rubber or ethylene propylene rubber.
Embodiment 7.In any one described production method of embodiment 1-6, in step (2), the vacuum tightness after vacuumizing is 0.001Mpa.
Embodiment 8.In any one described production method of embodiment 1-6, in step (2), the vacuum tightness after vacuumizing is 0.01Mpa.
Embodiment 9.In any one described production method of embodiment 1-6, in step (2), the vacuum tightness after vacuumizing is 0.05Mpa.
Embodiment 10.In any one described production method of embodiment 1-6, in step (2), the vacuum tightness after vacuumizing is 0.03Mpa.
Embodiment 11.In any one described production method of embodiment 1-6, in step (2), the vacuum tightness after vacuumizing is 0.08Mpa.
Embodiment 12.In any one described production method of embodiment 1-11, when the spray drying treatment described in the step (3), reclaim dimethylbenzene, and the dimethylbenzene that reclaims is entered repeated use in the step (1) with retrieving arrangement.
Claims (4)
1, a kind of production method of process for grafting maleic anhydride with ethylene propylene rubber solution is characterized in that, its step is,
(1) raw material ethylene-propylene rubber(EPR), benzoyl peroxide and maleic anhydride are dissolved in dimethylbenzene respectively, make solution;
(2) inject above-mentioned 3 kinds of solution successively in reactor, vacuumize the back nitrogen injection, controlled temperature 110-180 ℃, 30-100 rev/min of control stirring velocity reacted 5-20 minute, got ethylene-propylene rubber(EPR) and maleic anhydride grafts solution;
(3) to ethylene-propylene rubber(EPR) and the spray-dried processing of maleic anhydride grafts solution, making particle diameter is Powdered ethylene-propylene rubber(EPR) and the maleic anhydride grafts of 200nm-50um.
2, production method according to claim 1 is characterized in that, described ethylene-propylene rubber(EPR) is terpolymer EP rubber or ethylene propylene rubber.
3, production method according to claim 1 is characterized in that, in step (2), the vacuum tightness after vacuumizing is 0.001-0.01Mpa.
4, production method according to claim 1 is characterized in that, when the spray drying treatment described in the step (3), reclaims dimethylbenzene with retrieving arrangement, and the dimethylbenzene that reclaims is entered repeated use in the step (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2008102361051A CN101402710A (en) | 2008-11-24 | 2008-11-24 | Production process for grafting maleic anhydride with ethylene propylene rubber solution method |
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| CNA2008102361051A CN101402710A (en) | 2008-11-24 | 2008-11-24 | Production process for grafting maleic anhydride with ethylene propylene rubber solution method |
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| CN101402710A true CN101402710A (en) | 2009-04-08 |
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| CNA2008102361051A Pending CN101402710A (en) | 2008-11-24 | 2008-11-24 | Production process for grafting maleic anhydride with ethylene propylene rubber solution method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593162A (en) * | 2017-09-30 | 2019-04-09 | 中国石化扬子石油化工有限公司 | Graft process after a kind of polymerisation in solution |
| CN113105789A (en) * | 2021-04-10 | 2021-07-13 | 曾伟峰 | Weather-resistant composite flame-retardant coating and preparation method thereof |
-
2008
- 2008-11-24 CN CNA2008102361051A patent/CN101402710A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593162A (en) * | 2017-09-30 | 2019-04-09 | 中国石化扬子石油化工有限公司 | Graft process after a kind of polymerisation in solution |
| CN109593162B (en) * | 2017-09-30 | 2021-07-27 | 中国石化扬子石油化工有限公司 | Grafting process after solution polymerization |
| CN113105789A (en) * | 2021-04-10 | 2021-07-13 | 曾伟峰 | Weather-resistant composite flame-retardant coating and preparation method thereof |
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