CN107602743A - A kind of preparation method of extra high-molecular polythene catalyst - Google Patents
A kind of preparation method of extra high-molecular polythene catalyst Download PDFInfo
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- CN107602743A CN107602743A CN201710887907.8A CN201710887907A CN107602743A CN 107602743 A CN107602743 A CN 107602743A CN 201710887907 A CN201710887907 A CN 201710887907A CN 107602743 A CN107602743 A CN 107602743A
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Abstract
The present invention relates to a kind of preparation method of extra high-molecular polythene catalyst, comprise the following steps：(1) under the protection of nitrogen, Mg (OEt) 2 and varsol are reacted；(2) reacted to step (1) in the solution completed and add triethanolamine, reacted with Mg (OEt) 2；(3) addition titanium compound after two ethers internal electron donors fully react is added in the solution after the completion of reacting to step (2) to carry out carrying titanium reaction；(4) after the reaction of load titanium terminates, by the catalyst granules washing of generation, obtained High molecular weight polyethylene catalyst is dried.Extra high-molecular polythene catalyst high catalytic efficiency prepared by the present invention, amplification performance are stable, and particle diameter distribution is uniform, and the preparation method cycle is short, are adapted to industrialization.
Description
Technical field
The invention belongs to field of chemical technology, and in particular to a kind of preparation side of extra high-molecular polythene catalyst
Method.
Background technology
One of synthetic resin that polyethylene is most widely used and yield is maximum, is mainly used in industrial and agricultural production and people
The various aspects of class life.Polyethylene species is various, can be divided into according to the difference of molecular weight：It is low molecular weight polyethylene, common
Molecular weight polyethylene and ultra-high molecular weight polyethylene.Ultra-high molecular weight polyethylene be a kind of molecular weight more than 1,500,000, it is linear
Structure, there is the thermoplastic engineering plastic of Good All-around Property, its excellent properties having and its molecular weight have substantial connection,
So keeping its heavy molecular weight to be beneficial to keep its superior function, and ensure that the core of its molecular size range is then catalyst system
It is standby.
At present, extra high-molecular polythene catalyst numerous types, wherein with Ziegler-Natta catalyst research history
It is the longest, Development Techniques route is the most skillful.Ziegler-Natta catalyst can be divided into two classes again：The first is non-loaded
Ziegler-Natta catalyst, using saturated hydrocarbons as decentralized medium or solvent (such as heptane, gasoline), be catalyzed under normal temperature and pressure
Vinyl polymerization.Second is carrier model Ziegler-Natta catalyst, mainly using the porous tolerant matter such as alkyl magnesium, magnesium chloride as
Carrier.Carrier after activated is used as co-catalyst using organo-metallic compound.The main part of catalyst be containing titanium component and
Containing aluminum organic compound.But there is the shortcomings of catalytic activity is low, performance is unstable and long preparation period, preparation in the catalyst prepared
Process is complicated.
The content of the invention
It is an object of the invention to provide the extra high-molecular polythene catalyst that a kind of high catalytic efficiency, amplification performance are stable
Preparation method, short preparation period, be adapted to industrialization.
In order to realize the purpose of the present invention, adopt the following technical scheme that：
A kind of preparation method of extra high-molecular polythene catalyst, comprises the following steps：
(1) under the protection of nitrogen, by Mg (OEt)2Reacted with varsol；
(2) reacted to step (1) in the solution completed and add triethanolamine, with Mg (OEt)2Reaction；
(3) added in the solution after the completion of being reacted to step (2) after two ethers internal electron donors fully react and add titanizing
Compound carries out carrying titanium reaction；
(4) after the reaction of load titanium terminates, the catalyst granules washing of generation, dry obtained High molecular weight polyethylene are catalyzed
Agent.
Preferably, the reaction temperature of step (2) is 50~110 DEG C, and the reaction time is 1~2.5h.
Preferably, the mol ratio of two ethers internal electron donors and magnesium is 0.5~0.8:1.
Preferably, the amount for adding titanium compound is that titanium magnesium mol ratio is 2.5-4.5:1.
Preferably, the mol ratio of two ethers internal electron donors and magnesium is 0.6:1.
Preferably, the amount for adding titanium compound is that titanium magnesium mol ratio is 3:1.
Beneficial effects of the present invention：
Extra high-molecular polythene catalyst high catalytic efficiency prepared by the present invention, amplification performance are stable, and particle diameter distribution is equal
Even, the preparation method cycle is short, is adapted to industrialization.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
A kind of preparation method of extra high-molecular polythene catalyst, comprises the following steps：
(1) under the protection of nitrogen, by Mg (OEt)2Reacted with varsol；
(2) reacted to step (1) in the solution completed and add triethanolamine, with Mg (OEt)2Reaction, reaction temperature 50
DEG C, reaction time 2.5h；
(3) added in the solution after the completion of being reacted to step (2) after two ethers internal electron donors fully react and add titanizing
Compound carries out load titanium and reacted, and the mol ratio of two ethers internal electron donors and magnesium is 0.6:1, the amount for adding titanium compound is rubbed for titanium magnesium
You are than being 3:1；
(4) after the reaction of load titanium terminates, the catalyst granules washing of generation, dry obtained High molecular weight polyethylene are catalyzed
Agent.
Embodiment 2
A kind of preparation method of extra high-molecular polythene catalyst, comprises the following steps：
(1) under the protection of nitrogen, by Mg (OEt)2Reacted with varsol；
(2) reacted to step (1) in the solution completed and add triethanolamine, with Mg (OEt)2Reaction, reaction temperature 110
DEG C, reaction time 1.5h；
(3) added in the solution after the completion of being reacted to step (2) after two ethers internal electron donors fully react and add titanizing
Compound carries out load titanium and reacted, and the mol ratio of two ethers internal electron donors and magnesium is 0.6:1, the amount for adding titanium compound is rubbed for titanium magnesium
You are than being 3:1；
(4) after the reaction of load titanium terminates, the catalyst granules washing of generation, dry obtained High molecular weight polyethylene are catalyzed
Agent.
Embodiment 3
A kind of preparation method of extra high-molecular polythene catalyst, comprises the following steps：
(1) under the protection of nitrogen, by Mg (OEt)2Reacted with varsol；
(2) reacted to step (1) in the solution completed and add triethanolamine, with Mg (OEt)2Reaction, reaction temperature 70
DEG C, reaction time 1.5h；
(3) added in the solution after the completion of being reacted to step (2) after two ethers internal electron donors fully react and add titanizing
Compound carries out load titanium and reacted, and the mol ratio of two ethers internal electron donors and magnesium is 0.5:1, the amount for adding titanium compound is rubbed for titanium magnesium
You are than being 4.5:1；
(4) after the reaction of load titanium terminates, the catalyst granules washing of generation, dry obtained High molecular weight polyethylene are catalyzed
Agent.
Embodiment 4
A kind of preparation method of extra high-molecular polythene catalyst, comprises the following steps：
(1) under the protection of nitrogen, by Mg (OEt)2Reacted with varsol；
(2) reacted to step (1) in the solution completed and add triethanolamine, with Mg (OEt)2Reaction, reaction temperature 90
DEG C, reaction time 2h；
(3) added in the solution after the completion of being reacted to step (2) after two ethers internal electron donors fully react and add titanizing
Compound carries out load titanium and reacted, and the mol ratio of two ethers internal electron donors and magnesium is 0.8:1, the amount for adding titanium compound is rubbed for titanium magnesium
You are than being 3:1；
(4) after the reaction of load titanium terminates, the catalyst granules washing of generation, dry obtained High molecular weight polyethylene are catalyzed
Agent.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
1. a kind of preparation method of extra high-molecular polythene catalyst, it is characterised in that comprise the following steps：
(1) under the protection of nitrogen, by Mg (OEt)2Reacted with varsol；
(2) reacted to step (1) in the solution completed and add triethanolamine, with Mg (OEt)2Reaction；
(3) added in the solution after the completion of being reacted to step (2) after two ethers internal electron donors fully react and add titanium compound
Carry out carrying titanium reaction；
(4) after the reaction of load titanium terminates, by the catalyst granules washing of generation, obtained High molecular weight polyethylene catalyst is dried.
2. the preparation method of extra high-molecular polythene catalyst according to claim 1, it is characterised in that step (2)
Reaction temperature be 50~110 DEG C, the reaction time is 1~2.5h.
3. the preparation method of extra high-molecular polythene catalyst according to claim 1, it is characterised in that in two ethers
The mol ratio of electron donor and magnesium is 0.5~0.8:1.
4. the preparation method of extra high-molecular polythene catalyst according to claim 1, it is characterised in that add titanizing
The amount of compound is that titanium magnesium mol ratio is 2.5-4.5:1.
5. the preparation method of extra high-molecular polythene catalyst according to claim 3, it is characterised in that in two ethers
The mol ratio of electron donor and magnesium is 0.6:1.
6. the preparation method of extra high-molecular polythene catalyst according to claim 4, it is characterised in that add titanizing
The amount of compound is that titanium magnesium mol ratio is 3:1.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042547A (en) * | 1988-09-30 | 1990-05-30 | 希蒙特公司 | Olefinic polymerization composition and catalyzer |
| CN1084182A (en) * | 1992-07-17 | 1994-03-23 | 希蒙特公司 | The stabilization method of olefin polymer |
| CN101074275A (en) * | 2007-06-22 | 2007-11-21 | 上海化工研究院 | Extra high-molecular polythene catalyst and its production |
| CN101096389A (en) * | 2007-06-22 | 2008-01-02 | 上海化工研究院 | Super-high molecular weight polyethylene catalyzer and preparation method thereof |
| CN102417555A (en) * | 2010-09-28 | 2012-04-18 | 中国石油化工股份有限公司 | Preparation method of ultrahigh molecular weight polyethylene |
| CN104854033A (en) * | 2012-09-18 | 2015-08-19 | 纳米氟化物有限公司 | Process for production of magnesium fluoride sol solutions from alkoxides comprising addition of magnesium salts |
-
2017
- 2017-09-27 CN CN201710887907.8A patent/CN107602743A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042547A (en) * | 1988-09-30 | 1990-05-30 | 希蒙特公司 | Olefinic polymerization composition and catalyzer |
| CN1084182A (en) * | 1992-07-17 | 1994-03-23 | 希蒙特公司 | The stabilization method of olefin polymer |
| CN101074275A (en) * | 2007-06-22 | 2007-11-21 | 上海化工研究院 | Extra high-molecular polythene catalyst and its production |
| CN101096389A (en) * | 2007-06-22 | 2008-01-02 | 上海化工研究院 | Super-high molecular weight polyethylene catalyzer and preparation method thereof |
| CN102417555A (en) * | 2010-09-28 | 2012-04-18 | 中国石油化工股份有限公司 | Preparation method of ultrahigh molecular weight polyethylene |
| CN104854033A (en) * | 2012-09-18 | 2015-08-19 | 纳米氟化物有限公司 | Process for production of magnesium fluoride sol solutions from alkoxides comprising addition of magnesium salts |
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