CN107537413A - Olefin polymerization combined type method for controlling reaction temperature and device - Google Patents

Olefin polymerization combined type method for controlling reaction temperature and device Download PDF

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Publication number
CN107537413A
CN107537413A CN201610490022.XA CN201610490022A CN107537413A CN 107537413 A CN107537413 A CN 107537413A CN 201610490022 A CN201610490022 A CN 201610490022A CN 107537413 A CN107537413 A CN 107537413A
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thermostat
temperature
heater
pipe
temperature control
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CN201610490022.XA
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CN107537413B (en
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周建勇
李晓庆
李留忠
严婕
李功韬
徐晓
范大鹏
齐立芳
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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Abstract

The present invention relates to a kind of olefin polymerization combined type method for controlling reaction temperature and device, belong to chemical reaction temperature control technology field.Described olefin polymerization combined type method for controlling reaction temperature, its used device include thermostat, and thermostat connects into a circulation loop with overflow pipe, water supply tank, small pump, filling pipe successively;The bottom of thermostat connects circulating pump by outlet pipe;The top of thermostat side is provided with return pipe;Circulating pump is provided with more, and every circulating pump is connected with after-heater, after-heater connection circulation pipe.The present invention is controlled by DCS, is realized reaction temperature and is automatically controlled, while after-heater is devised in circulation line, realizes temperature control of the single thermostat to multiple different temperatures polymerisations, saves space, improves efficiency;The present invention can also realize the temperature control of multiple identical temperature polymerizations reactions;The present invention is closed-loop operation, will not increase operating space humidity.

Description

Olefin polymerization combined type method for controlling reaction temperature and device
Technical field
The present invention relates to a kind of olefin polymerization combined type method for controlling reaction temperature and device, belong to chemical reaction temperature Control technology field.
Background technology
Polyolefin is a kind of synthetic resin of excellent performance, is widely used.Catalyst used in olefinic polymerization mainly has Z-N The types such as type, chromium system, metallocene, substantial amounts of heat can be discharged, it is necessary to carry out removing heat in time in course of reaction, reach reaction temperature Stability contorting, so as to ensure the stable performance of vistanex, improve product quality.In present temprature control method, Temperature control is carried out using the corresponding reactor of a water-bath mostly, this will certainly increase equipment occupation space, cause space Waste, it is less efficient.And when a course of reaction needs priority to be carried out under two reaction temperatures, i.e., segmentation is reacted, mesh Preceding water-bath temperature control method lacks quick response mode, and warm area transit time is longer.
CN203870493U discloses a kind of novel and multifunctional water bath device, including casing and controller, is provided with casing Moisturizing pond and at least two sea water baths, moisturizing pond are connected respectively by priming valve with sea water bath, and having heaters is all provided with sea water bath, The liquid level sensor of induction level position and the temperature sensor of the internal bath temperature of measurement, level sensing are additionally provided with sea water bath Device and temperature sensor are connected with controller respectively.By using controller, temperature sensor, liquid level sensor, heater and Priming valve realize two sea water bath independent heatings, it is automatic add thermophilic hot water, timing alarm, overheat protector, anti-anhydrous heating and The purpose of bath temperature fluctuation is greatly lowered.Two water-baths are really grouped together and used by the invention, realize Respectively control of a set of control system to two water-baths, but the invention does not have the water-bath circulatory system, can not be poly- to outside Close reactor and carry out temperature control operation, while constant temperature method can only be carried out respectively in two water-baths, can not realize to enter water-bath The alternating temperature operation of row multi-temperature zone.
CN205109685U discloses a kind of self-watering multifunction constant temperature water-bath, there is provided One function is powerful, operation Convenient, time saving and energy saving thermostat water bath, achievable automatic uniform add water, increase pot cover height, convenient placement round center hole Sub- pot cover, draining are convenient;And it is furnished with more specification rack for test tubes, effectively reduces the workload of experimenter, it is time saving and energy saving, reduce peace Full hidden danger, it is convenient and practical.But the invention can not be controlled also without the water-bath circulatory system is set to outside polymer reactor Temperature operation, can only easily be operated in water-bath, can not realize that the alternating temperature that multi-temperature zone is carried out to water-bath operates.
The content of the invention
, can be simultaneously to differential responses it is an object of the invention to provide olefin polymerization combined type method for controlling reaction temperature Multiple polymerisations of temperature carry out temperature control, improve efficiency, save space;Present invention simultaneously provides the device that it is used.
Olefin polymerization combined type method for controlling reaction temperature of the present invention, its used device include constant temperature Groove, thermostat connect into a circulation loop with overflow pipe, water supply tank, small pump, filling pipe successively;The bottom of thermostat passes through Outlet pipe connects circulating pump;The top of thermostat side is provided with return pipe;Temperature sensor, agitator are provided with thermostat and is added Hot device;Circulating pump is provided with more, and every circulating pump is connected with after-heater, after-heater connection circulation pipe.
Control method comprises the following steps:
(1) agitator is started, by setting the temperature of thermostat, heater is begun to warm up, and is set when thermostat temperature reaches After constant temperature degree, heater is automatically stopped heating, and multiple polymerisations start to react;
(2) temperature control
Circulation pipe carries out temperature control to multiple polymerisations, and DCS system requires according to the temperature control of polymerisation, calculates each two The heating power of secondary heater, heated recirculated water are controlled through circulation pipe to polymerisation, the recirculated water through heat exchange Thermostat is entered by return pipe;
(3) thermostat temperature control
The measurement signal real-time display of temperature sensor is in DCS system in thermostat, when thermostat temperature is less than constant temperature When groove design temperature allows to fluctuate lower limit, heater automatic start;When thermostat temperature allows the fluctuation upper limit higher than design temperature When, small pump automatic start, the water at low temperature in water supply tank enters thermostat, and thermostat temperature is cooled;Constant temperature trough inner water When position reaches overfall, the recirculated water of super water level enters water supply tank through overflow pipe.
Device used in described olefin polymerization combined type method for controlling reaction temperature, including thermostat, thermostat Connect into a circulation loop with overflow pipe, water supply tank, small pump, filling pipe successively, the temperature in water supply tank is room temperature, moisturizing The startup time of pump is adjustable;The bottom of thermostat connects circulating pump by outlet pipe;The top of thermostat side is provided with return pipe, The recirculated water for completing heat exchange is back to thermostat through return pipe;Circulating pump is provided with more, and every circulating pump is and reheating Device is connected, after-heater connection circulation pipe.
Wherein:
The power adjustable of circulating pump
Rotating speed can be adjusted as needed for agitator
The side of thermostat offers form, and the water level in thermostat can be observed, and top is provided with detachable cover Plate, under normal circumstances thermostat be in air-tight state, trough inner water point will not evaporate, and avoid increasing humidity in operating space, this is right It is extremely important for the operation that space humidity requires, can be to detachable cover plate when thermostat needs maintenance.
Various types of signal in combined type reaction temperature control device is connected with control unit by DCS, to combined type temperature Water-bath is controlled to carry out remote control operation.
Beneficial effects of the present invention are as follows:
The present invention is controlled by DCS, is realized reaction temperature and is automatically controlled, while secondary add is devised in circulation line Hot device, temperature control of the single thermostat to multiple different temperatures polymerisations is realized, save space, improve efficiency;This hair The bright temperature control that can also realize multiple identical temperature polymerizations reactions;The present invention is closed-loop operation, will not increase operating space Humidity.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention.
In figure:1st, water supply tank;2nd, small pump;3rd, overflow pipe;4th, thermostat;5th, temperature sensor;6th, agitator;7th, heat Device;8th, return pipe;9th, circulation pipe;10th, outlet pipe;11st, circulating pump;12nd, after-heater;13rd, heating tube;14th, form;15、 Dismountable cover plate.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
Start agitator 6, set the temperature of thermostat 4 as 70 DEG C, heater 7 is begun to warm up, and is set when the temperature of thermostat 4 reaches After constant temperature degree, heater 7 is automatically stopped heating, and polymerisation one and polymerisation two start to react;
Temperature control one:A wherein circulation pipe 9 is to the temperature control of polymerisation one, and the power setting of circulating pump 11 is 30%, DCS system Required to calculate the heating power of after-heater 12 according to the temperature control of polymerisation one, heated recirculated water is through circulation pipe 9 to poly- Close reaction one to be controlled, the recirculated water through heat exchange enters thermostat 4 by return pipe 8;
Temperature control two:An other circulation pipe 9 is to the temperature control of polymerisation two, and temperature control method is as described in above-mentioned temperature control one.
Thermostat temperature control:The measurement signal real-time display of temperature sensor 5 works as perseverance in DCS system in thermostat 4 When the warm temperature of groove 4 allows to fluctuate lower limit less than the design temperature of thermostat 4, the automatic start of heater 7;When the temperature of thermostat 4 is higher than When design temperature allows to fluctuate the upper limit, the automatic start of small pump 2 in water supply tank 1, water at low temperature enters thermostat 4 in water supply tank 1, right The temperature of thermostat 4 is cooled;When water level reaches overfall in thermostat 4, the recirculated water of super water level enters moisturizing through overflow pipe 3 Case 1.
Embodiment 2
Polymerisation one:70 DEG C of temperature control
Polymerisation two:70 DEG C of temperature control
Start agitator 6, set the temperature of thermostat 4 as 70 DEG C, heater 7 is begun to warm up, and is set when the temperature of thermostat 4 reaches After constant temperature degree, heater 7 is automatically stopped heating, and polymerisation one and polymerisation two start to react;
Temperature control one:A wherein circulation pipe 9 is to the temperature control of polymerisation one, and the power setting of circulating pump 11 is 60%, DCS system Setting after-heater 12 does not start, and recirculated water is controlled through circulation pipe 9 to polymerisation one, and the recirculated water through heat exchange leads to Cross return pipe 8 and enter thermostat 4;
Temperature control two:An other circulation pipe 9 is to the temperature control of polymerisation two, and temperature control method is as described in above-mentioned temperature control one.
Thermostat temperature control:The measurement signal real-time display of temperature sensor 5 works as perseverance in DCS system in thermostat 4 When the warm temperature of groove 4 allows to fluctuate lower limit less than the design temperature of thermostat 4, the automatic start of heater 7;When the temperature of thermostat 4 is higher than When design temperature allows to fluctuate the upper limit, the automatic start of small pump 2 in water supply tank 1, water at low temperature enters thermostat 4 in water supply tank 4, right The temperature of thermostat 4 is cooled;When water level reaches overfall in thermostat 4, the recirculated water of super water level enters moisturizing through overflow pipe 3 Case 1.
Embodiment 3
Polymerisation one:85 DEG C of temperature control
Polymerisation two:70 DEG C of temperature control
Start agitator 6, set the temperature of thermostat 4 as 70 DEG C, heater 7 is begun to warm up, and is set when the temperature of thermostat 4 reaches After constant temperature degree, heater 7 is automatically stopped heating, and polymerisation one and polymerisation two start to react;
Temperature control one:A wherein circulation pipe 9 is to the temperature control of polymerisation one, and the power setting of circulating pump 11 is 30%, DCS system Required to calculate the heating power of after-heater 12 according to the temperature control of polymerisation one, heated recirculated water is right by circulation pipe 9 Polymerisation one is controlled, and the recirculated water through heat exchange enters thermostat 4 by return pipe 8;
Temperature control two:An other circulation pipe 9 is to the temperature control of polymerisation two, and the power setting of circulating pump 11 is 60%, DCS system Setting after-heater 12 does not start, and recirculated water is controlled by circulation pipe 9 to polymerisation two, the recirculated water through heat exchange Thermostat 4 is entered by return pipe 8;
Thermostat temperature control is the same as embodiment 1.

Claims (6)

1. a kind of olefin polymerization combined type method for controlling reaction temperature, its used device includes thermostat (4), thermostat (4) circulation loop is connected into overflow pipe (3), water supply tank (1), small pump (2), filling pipe successively;The bottom of thermostat (4) Portion connects circulating pump (11) by outlet pipe (10);The top of thermostat (4) side is provided with return pipe (8);Set in thermostat (4) There are temperature sensor (5), agitator (6) and heater (7), it is characterised in that:Circulating pump (11) is provided with more, every circulating pump (11) it is connected with after-heater (12), after-heater (12) connection circulation pipe (9);
The control method comprises the following steps:
(1) agitator (6) is started, by setting the temperature of thermostat (4), heater (7) is begun to warm up, when in thermostat (4) After temperature reaches design temperature, heater (7) is automatically stopped heating, and multiple polymerisations start to react;
(2) temperature control
Circulation pipe (9) carries out temperature control to multiple polymerisations, and DCS system requires according to the temperature control of polymerisation, calculates each two The heating power of secondary heater (12), heated recirculated water is controlled through circulation pipe (9) to polymerisation, through heat exchange Recirculated water enters thermostat (4) by return pipe (8);
(3) thermostat temperature control
The measurement signal real-time display of thermostat (4) interior temperature sensor (5) is in DCS system, and when thermostat (4), temperature is less than When thermostat (4) design temperature allows to fluctuate lower limit, heater (7) automatic start;When thermostat (4), temperature is higher than design temperature When allowing to fluctuate the upper limit, small pump (2) automatic start, the water at low temperature in water supply tank (1) enters thermostat (4), to thermostat (4) Temperature is cooled;When the interior water level of thermostat (4) reaches overfall, the recirculated water of super water level enters water supply tank through overflow pipe (3) (1)。
2. device used in the olefin polymerization combined type method for controlling reaction temperature described in a kind of claim 1, including perseverance Warm groove (4), thermostat (4) connect into one and are recycled back to overflow pipe (3), water supply tank (1), small pump (2), filling pipe successively Road;The bottom of thermostat (4) connects circulating pump (11) by outlet pipe (10);The top of thermostat (4) side is provided with return pipe (8), it is characterised in that:Circulating pump (11) is provided with more, and every circulating pump (11) is connected with after-heater (12), secondary to add Hot device (12) connection circulation pipe (9).
3. olefin polymerization combined type reaction temperature control device according to claim 2, it is characterised in that:Thermostat (4) side offers form (14).
4. device according to claim 2, it is characterised in that:The top of thermostat (4) is provided with dismountable cover plate (15).
5. device according to claim 2, it is characterised in that:Heating tube (13) is provided with after-heater (12).
6. device according to claim 2, it is characterised in that:Various types of signal in combined type reaction temperature control device with Control unit is connected by DCS, and remote control operation is carried out to the water-bath of combined type temperature control.
CN201610490022.XA 2016-06-29 2016-06-29 Olefin polymerization combined type method for controlling reaction temperature and device Active CN107537413B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657146A (en) * 2004-12-30 2005-08-24 清华大学 Material mixing system
US20140014089A1 (en) * 2011-03-30 2014-01-16 Japan Oil, Gas And Metals National Corporation Temperature control system, hydrocarbon synthesis reaction apparatus, hydrocarbon synthesis reaction system, and temperature control process
CN203629026U (en) * 2013-12-23 2014-06-04 新特能源股份有限公司 Heat conduction oil electric heating and circulating device in cold hydrogenation
CN103933916A (en) * 2014-04-04 2014-07-23 金发科技股份有限公司 Heating-cooling method and heating-cooling system utilizing fused salt as carrier
CN204084857U (en) * 2014-07-31 2015-01-07 广东万木新材料科技有限公司 A kind of conduction oil temperature-controlling system
CN104667855A (en) * 2015-01-20 2015-06-03 湖南省南岭化工集团有限责任公司 Heat-conducting oil transport system for reaction kettle
CN204693821U (en) * 2015-05-28 2015-10-07 常州市凯凯照明电器有限公司 Heat carrier heating system

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657146A (en) * 2004-12-30 2005-08-24 清华大学 Material mixing system
US20140014089A1 (en) * 2011-03-30 2014-01-16 Japan Oil, Gas And Metals National Corporation Temperature control system, hydrocarbon synthesis reaction apparatus, hydrocarbon synthesis reaction system, and temperature control process
CN203629026U (en) * 2013-12-23 2014-06-04 新特能源股份有限公司 Heat conduction oil electric heating and circulating device in cold hydrogenation
CN103933916A (en) * 2014-04-04 2014-07-23 金发科技股份有限公司 Heating-cooling method and heating-cooling system utilizing fused salt as carrier
CN204084857U (en) * 2014-07-31 2015-01-07 广东万木新材料科技有限公司 A kind of conduction oil temperature-controlling system
CN104667855A (en) * 2015-01-20 2015-06-03 湖南省南岭化工集团有限责任公司 Heat-conducting oil transport system for reaction kettle
CN204693821U (en) * 2015-05-28 2015-10-07 常州市凯凯照明电器有限公司 Heat carrier heating system

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