CN102731695A - New preparation method for drag reducer polymer - Google Patents
New preparation method for drag reducer polymer Download PDFInfo
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- CN102731695A CN102731695A CN2012102031221A CN201210203122A CN102731695A CN 102731695 A CN102731695 A CN 102731695A CN 2012102031221 A CN2012102031221 A CN 2012102031221A CN 201210203122 A CN201210203122 A CN 201210203122A CN 102731695 A CN102731695 A CN 102731695A
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Abstract
The purpose of the present invention is to overcome problems of difficult material discharging, complex subsequent operations, and the like in the old process. According to the present invention, a new process adopting a small kettle to carry out controllable pre-polymerization is adopted, and is used in production of a HG pipe oil product drag reducer polymer. The preparation method for the drag reducer polymer can comprises the following steps: 1) adding an inert solvent, a small amount of a monomer, an assistant catalyst and a main catalyst to a pre-polymerization autoclave, and carrying out a polymerization reaction at a low temperature, such that the catalyst particles are suspended in the polyolefin solution to form a slurry with moderate viscosity; and 2) adding a monomer, an assistant catalyst, an external electron donor, and the material inside the pre-polymerization autoclave to a small reaction vessel according to a certain amounts, and carrying out polymerization.
Description
Technical field
The present invention relates to a kind of preparation method of high molecular polymer, particularly a kind of preparation method of drag reducer polymerization thing.
Background technology
As the superpolymer of oil phase dra, drag-reduction effect is reasonable at present mainly is alpha-olefin homo and multipolymer thereof.The general polymerization single polymerization monomer that adopts is 1-octene, 1-decene, 1-laurylene and 1-hexadecylene etc., and Primary Catalysts adopts the solvay-type titanous chloride, and promotor adopts aluminum alkyls.
Olefinic polymerization belongs to the polymerization of coordination ion type; It is a kind of polyreaction of under the complex catalyst effect, carrying out; Usually polymerization process is that complexing at first takes place for monomer and catalyzer (should be called initiator exactly); Through transition state, monomer " insertion " increases living chain between living chain and the catalyzer.
The present domestic two kinds of working methods that mainly contain.A kind of method adopts monomer and catalyzer prepolymerization in prepolymerization kettle, treats catalyzer no longer after the sedimentation, and the bleeder valve branch installs to the little reaction vessel (the domestic plastics bag that is generally) at the bottom of the prepolymerization kettle, in little reaction vessel, accomplishes polymerization then.Specifically can be referring to document " progress of oil product drag reducer " author Zuo Yanmei, Yangzhou Industry Polytechnic College's collection of essay, 2010 01 phases.But there is obvious defects in this method, mainly is: the limited time of (1) discharging.Material in the prepolymerization kettle exists material viscosity excessive so that stop up the danger of bleeder valve as can not in half a hour, in time draining, and operation easier is big; (2) in the arm little reaction vessel, be full of pre-polymerization liquid from bleeder valve, pre-polymerization liquid residual after the discharging continues polymerization, causes arm to be stopped up by solid-state flow improver, is difficult to cleaning; (3) in the discharging process, temperature of charge possibly go up near room temperature, cause should low-temp reaction material at room temperature reaction, quality product is defective.
Another kind method is in vacuum glove box, to operate, and wherein respectively monomer and catalyzer weighing in vacuum glove box is added in the little reaction vessel, changes over to then and carries out polymerization in the refrigeration chamber.This method is because operate in vacuum glove box, and the pump drainage displaced air is very loaded down with trivial details with the transfer material.
Summary of the invention
The problem that invention will solve
Difficult for overcoming the aging method discharging, problems such as subsequent operations complicacy, the inventor proposes to adopt the novel method of the controlled pre-polymerization of little still, is applied to HG drag reduction agent for oil product through pipelines polymer production.
The scheme that is used to deal with problems
In order to address the above problem, the present invention provides a kind of preparation method of drag reducer polymerization thing, it is characterized in that,
1) monomer, promotor and external electron donor are added in the batch mixing still, stir, be cooled to-10 ℃～10 ℃;
2) in prepolymerization kettle, add monomer, promotor and the Primary Catalysts of 1 quality % to 5 quality % of inert solvent, inert solvent, carry out polyreaction, form the slurries that granules of catalyst is suspended in pre-polymer solution at-10 ℃～10 ℃;
3) respectively the mixture in the batch mixing still and the slurries in the prepolymerization kettle mass ratio according to 20:1 to 100:1 is added in the little reaction vessel, carry out polymerization at-10 ℃～10 ℃ then.
In order to address the above problem, the present invention provides the preparation method of another kind of drag reducer polymerization thing, it is characterized in that,
1) in prepolymerization kettle, adds monomer, promotor and the Primary Catalysts of 1 quality % to 5 quality % of inert solvent, inert solvent, carry out polyreaction, form the slurries that granules of catalyst is suspended in pre-polymer solution at-10 ℃～10 ℃;
2) with monomer, promotor and external electron donor; And the slurries in the prepolymerization kettle add in the little reaction vessel; The mass ratio of the slurries in the total mass of said monomer, promotor and the external electron donor that wherein adds and the prepolymerization kettle of adding is 20:1 to 100:1, under-10 ℃～10 ℃ temperature, carries out polymerization then.
The preparation method of drag reducer polymerization thing of the present invention; It is characterized in that, in said little reaction vessel, the preceding quality of reaction based on total material in the little reaction vessel; The concentration range of monomer and prepolymer is 97 quality %～99.8 quality %; The concentration range of Primary Catalysts is 0.005 quality %～0.1 quality %, and the concentration range of promotor is 0.1 quality %～3 quality %, and the concentration range of external electron donor is 0.01 quality %～0.5 quality %.
The preparation method of drag reducer polymerization thing of the present invention is characterized in that, said Primary Catalysts is titanous chloride or titanium tetrachloride.
The preparation method of drag reducer polymerization thing of the present invention is characterized in that, said promotor is triethyl aluminum or triisobutyl aluminium.
The preparation method of drag reducer polymerization thing of the present invention is characterized in that, said external electron donor is diisopropyl dimethoxy silane and the dicyclopentyl dimethoxyl silane of mass ratio 5:1～1:5.
The preparation method of drag reducer polymerization thing of the present invention is characterized in that, said monomer is C
6～C
20Terminal olefin.
The preparation method of drag reducer polymerization thing of the present invention is characterized in that, said solvent is normal heptane or octane or normal hexane.
The preparation method of drag reducer polymerization thing of the present invention is characterized in that, said little reaction vessel is the pocket type reaction vessel.
The preparation method of drag reducer polymerization thing of the present invention is characterized in that, the viscosity of the said slurries that in prepolymerization kettle, form is 100mPas to 1000mPas.
The effect of invention
The monomer concentration that the present invention controls in the prepolymerization kettle keeps lower level, even the whole polymerizations of monomer in the prepolymerization kettle can not solidified yet.Therefore there is not the danger of line clogging in prepolymerization kettle, and the subsequent operations time is also very abundant.
Embodiment
The present invention has developed a kind of new process for producing of drag reducer polymerization thing, thereby synthetic HG drag reduction agent for oil product through pipelines is applied to long distance oil pipeline, improves pipeline transmission capacity.
The preparation method of drag reducer polymerization thing of the present invention; Can may further comprise the steps: 1) in prepolymerization kettle, add inert solvent, small amounts of monomer, promotor and Primary Catalysts; Carry out polyreaction at low temperatures, form the slurries that granules of catalyst is suspended in the modest viscosity of polyolefin solution; 2) respectively with monomer, promotor and external electron donor, and prepolymerization kettle in material dosing add in the little reaction vessel, carry out polymerization then.Wherein the 2nd) monomer, promotor and the external electron donor that add in the step can be added into little reaction vessel respectively, and also can in the batch mixing still, mix in advance, and stir, be added into little reaction vessel more together after the cooling.The present invention preferably mixes monomer, promotor and external electron donor earlier, cools off in the batch mixing still.
Little reaction vessel described in the present invention is meant that capacity is the reaction vessel that 1-50 rises, and is preferably the pocket type reaction vessel, its capacity is preferably 1 and rises to 10 liters.Said little reaction container materials does not have special qualification, as long as it is inertia for reaction of the present invention.
Polymerization temperature in prepolymerization kettle is generally-10 ℃～10 ℃, is preferably-5 ℃～5 ℃.The polymeric temperature is generally-10 ℃～10 ℃ in the little reaction vessel, is preferably-5 ℃～5 ℃.The temperature of batch mixing still internal cooling is-10 ℃～10 ℃, is preferably-5 ℃～5 ℃.
Drag reducer polymerization thing of the present invention comprises the homopolymer of terminal olefin or the multipolymer of terminal olefin, or its mixture.The general monomer that adopts is C
6～C
20Terminal olefin, for example be 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-hendecene, 1-laurylene and 1-hexadecylene etc., preferred C
8～C
16Terminal olefin.Polymkeric substance can be the homopolymer of terminal olefin, also can be the multipolymer of two or more terminal olefins.Preferred 1-octene, 1-decene and/or the 1-laurylene of using more preferably uses 1-octene, 1-decene and 1-laurylene as comonomer simultaneously.
As Primary Catalysts, can use titanous chloride or titanium tetrachloride, wherein preferred titanous chloride.Promotor can use triethyl aluminum or triisobutyl aluminium, preferred triisobutyl aluminium.
The solution that uses among the present invention comprises normal heptane, octane or normal hexane.Wherein, preferred normal heptane.
In the method for the present invention, the external electron donor that uses can be diisopropyl dimethoxy silane and dicyclopentyl dimethoxyl silane, and its mass ratio can be 5:1～1:5, and preferably its mass ratio is 2.5:1～1:2.5.
Embodiment
Embodiment 1
(1) with the octene of 200 kilograms of the monomers behind the purifying, 150 kilograms decene, (the weight ratio diisopropyl dimethoxy silane: dicyclopentyl dimethoxyl silane=5:1) add in the batch mixing still and stir is cooled to-10 ℃ to 150 kilograms triisobutyl aluminium and external electron donor 65 grams of 1.2 kilograms of laurylene and promotors, and monomer does not carry out polyreaction;
(2) in prepolymerization kettle, add the normal heptane of 11 kilograms (containing 3 quality % octenes approximately), add 0.3 kilogram triisobutyl aluminium then, be cooled to-10 ℃ after, add 100g titanous chloride (titanium content 2.7 quality %) through the catalyzer charging opening.Under agitation react and obtained the slurries that a kind of granules of catalyst is suspended in the viscosity 100mPa.s to 1000mPa.s of polyolefin solution in 30 minutes.
(3) with peristaltic pump the material in batch mixing still and the prepolymerization kettle is quantitatively added in the little reaction vessel according to the weight ratio of 50:1 respectively, put into freezer-10 ℃～10 ℃ then and carry out polymerization.
Embodiment 2
(1) with the octene of 150 kilograms of the monomers behind the purifying, 150 kilograms decene, (the weight ratio diisopropyl dimethoxy silane: dicyclopentyl dimethoxyl silane=1:5) add in the batch mixing still and stir is cooled to-10 ℃ to 200 kilograms triisobutyl aluminium and external electron donor 65 grams of laurylene and promotor 1.3, and monomer does not carry out polyreaction;
(2) in prepolymerization kettle, add the solvent of 11 kilograms (containing 3 quality % octenes approximately), add 0.2 kilogram of triisobutyl aluminium then, be cooled to-5 ℃ after, add 100g titanous chloride (titanium content 2.7 quality %) through the catalyzer charging opening.Under agitation react and obtained the slurries that a kind of granules of catalyst is suspended in the viscosity 100mPa.s to 1000mPa.s of polyolefin solution in 40 minutes.
(3) with peristaltic pump the material in batch mixing still and the prepolymerization kettle is quantitatively added in the little reaction vessel according to the weight ratio of 40:1 respectively, put into freezer-10 ℃～10 ℃ then and carry out polymerization.
Claims (10)
1. the preparation method of a drag reducer polymerization thing is characterized in that,
1) monomer, promotor and external electron donor are added in the batch mixing still, stir, be cooled to-10 ℃～10 ℃;
2) in prepolymerization kettle, add monomer, promotor and the Primary Catalysts of 1 quality % to 5 quality % of inert solvent, inert solvent, carry out polyreaction, form the slurries that granules of catalyst is suspended in pre-polymer solution at-10 ℃～10 ℃;
3) respectively the mixture in the batch mixing still and the slurries in the prepolymerization kettle mass ratio according to 20:1 to 100:1 is added in the little reaction vessel, carry out polymerization at-10 ℃～10 ℃ then.
2. the preparation method of a drag reducer polymerization thing is characterized in that,
1) in prepolymerization kettle, adds monomer, promotor and the Primary Catalysts of 1 quality % to 5 quality % of inert solvent, inert solvent, carry out polyreaction, form the slurries that granules of catalyst is suspended in pre-polymer solution at-10 ℃～10 ℃;
2) with monomer, promotor and external electron donor; And the slurries in the prepolymerization kettle add in the little reaction vessel; The mass ratio of the slurries in the total mass of said monomer, promotor and the external electron donor that wherein adds and the prepolymerization kettle of adding is 20:1 to 100:1, under-10 ℃～10 ℃ temperature, carries out polymerization then.
3. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that, in said little reaction vessel; The preceding quality of reaction based on total material in the little reaction vessel; The concentration range of monomer and prepolymer is 97 quality %～99.8 quality %, and the concentration range of Primary Catalysts is 0.005 quality %～0.1 quality %, and the concentration range of promotor is 0.1 quality %～3 quality %; The concentration range of external electron donor is 0.01 quality %～0.5 quality %, and surplus is a solvent.
4. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that said Primary Catalysts is titanous chloride or titanium tetrachloride.
5. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that said promotor is triethyl aluminum or triisobutyl aluminium.
6. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that said external electron donor is diisopropyl dimethoxy silane and the dicyclopentyl dimethoxyl silane of mass ratio 5:1～1:5.
7. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that said monomer is C
6～C
20Terminal olefin.
8. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that said solvent is normal heptane, octane or normal hexane.
9. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that said little reaction vessel is the pocket type reaction vessel.
10. according to the preparation method of the drag reducer polymerization thing of claim 1 or 2, it is characterized in that the viscosity of the said slurries that in prepolymerization kettle, form is 100mPas to 1000mPas.
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Cited By (7)
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| CN103936897A (en) * | 2013-01-17 | 2014-07-23 | 中国石油化工股份有限公司 | Drag reducer, and preparation method thereof |
| CN103936900A (en) * | 2013-01-17 | 2014-07-23 | 中国石油化工股份有限公司 | Drag reducer and preparation method thereof |
| CN111217953A (en) * | 2019-10-30 | 2020-06-02 | 中国石油化工股份有限公司 | Low-crystallinity high-molecular-weight polyolefin and synthesis and application thereof |
| CN113614116A (en) * | 2019-02-04 | 2021-11-05 | 因诺斯佩克有限公司 | Polymerization process and apparatus therefor |
| CN113614001A (en) * | 2019-02-04 | 2021-11-05 | 因诺斯佩克有限公司 | Polymer material |
| WO2022140743A1 (en) * | 2020-12-23 | 2022-06-30 | Liquidpower Specialty Products Inc. | Rapid dissolution of drag-reducing agents at low temperatures |
| US11951452B2 (en) | 2019-02-04 | 2024-04-09 | Innospec Limited | Method of assembling an apparatus for containing reagents for a chemical reaction |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936897A (en) * | 2013-01-17 | 2014-07-23 | 中国石油化工股份有限公司 | Drag reducer, and preparation method thereof |
| CN103936900A (en) * | 2013-01-17 | 2014-07-23 | 中国石油化工股份有限公司 | Drag reducer and preparation method thereof |
| CN103936900B (en) * | 2013-01-17 | 2016-03-16 | 中国石油化工股份有限公司 | A kind of flow improver and preparation method thereof |
| CN103936897B (en) * | 2013-01-17 | 2016-03-23 | 中国石油化工股份有限公司 | A kind of flow improver and preparation method thereof |
| CN113614116A (en) * | 2019-02-04 | 2021-11-05 | 因诺斯佩克有限公司 | Polymerization process and apparatus therefor |
| CN113614001A (en) * | 2019-02-04 | 2021-11-05 | 因诺斯佩克有限公司 | Polymer material |
| US11813602B2 (en) | 2019-02-04 | 2023-11-14 | Innospec Limited | Polymerisation method and apparatus therefor |
| US11951452B2 (en) | 2019-02-04 | 2024-04-09 | Innospec Limited | Method of assembling an apparatus for containing reagents for a chemical reaction |
| CN111217953A (en) * | 2019-10-30 | 2020-06-02 | 中国石油化工股份有限公司 | Low-crystallinity high-molecular-weight polyolefin and synthesis and application thereof |
| WO2022140743A1 (en) * | 2020-12-23 | 2022-06-30 | Liquidpower Specialty Products Inc. | Rapid dissolution of drag-reducing agents at low temperatures |
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Inventor after: Zhang Ning Inventor after: Su Hang Inventor after: Yin Shoucheng Inventor after: Ni Guangdi Inventor after: Jia Banglong Inventor after: Zu Haiyan Inventor after: Zhuang Jun Inventor after: Yang Hui Inventor after: Cui Di Inventor after: Wang Yiran Inventor after: Zhao Liang Inventor after: Cao Danfu Inventor after: Zhang Yiding Inventor after: Jiang Hesheng Inventor after: Fan Junzhong Inventor after: Jia Baofang Inventor after: Cheng Xuxia Inventor after: Wu Jie Inventor after: Wang Dezhi Inventor after: Li Hao Inventor before: Zhang Ning Inventor before: Cao Danfu Inventor before: Jiang Hesheng Inventor before: Fan Junzhong Inventor before: Jia Baofang |
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Free format text: CORRECT: INVENTOR; FROM: ZHANG NING CAO DANFU JIANG HESHENG FAN JUNZHONG JIA BAOFANG TO: ZHANG NING CAO DANFU JIANG HESHENG FAN JUNZHONG JIA BAOFANG CHENG XUXIA WU JIE WANG DEZHI LI HAO SU HANG YIN SHOUCHENG NI GUANGDI JIA BANGLONG ZU HAIYAN ZHUANG JUN YANG HUI CUI DI WANG YIRAN ZHAO LIANG ZHANG YIDING |
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Effective date of registration: 20220211 Address after: 100029 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: State pipe network group east crude oil storage and Transportation Co.,Ltd. Patentee after: XUZHOU JINQIAO PETROCHEMICAL PIPELINE TRANSPORTATION TECHNOLOGY CO.,LTD. Address before: 100029 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: PIPELINE STORAGE AND TRANSPORT BRANCH OF CHINA PETROLEUM & CHEMICAL Corp. Patentee before: XUZHOU JINQIAO PETROCHEMICAL PIPELINE TRANSPORTATION TECHNOLOGY CO.,LTD. |