CN104177235B - A kind of catalyst recycle unit and method preparing polymethoxy dimethyl ether - Google Patents
A kind of catalyst recycle unit and method preparing polymethoxy dimethyl ether Download PDFInfo
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- CN104177235B CN104177235B CN201310613341.1A CN201310613341A CN104177235B CN 104177235 B CN104177235 B CN 104177235B CN 201310613341 A CN201310613341 A CN 201310613341A CN 104177235 B CN104177235 B CN 104177235B
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Abstract
The application relates to a kind of catalyst recycle unit and the method for preparing polymethoxy dimethyl ether.This catalyst recycle unit comprises catalyst charge groove, catalyst reaction circulation device and catalyst recovery devices; Described catalyst reaction circulation device comprises reactor, reaction mass water cooler; Described catalyst charge groove is connected with the entrance of described reactor; Between the outlet that described reaction mass water cooler is arranged on described reactor and entrance; Between the outlet of described reactor and described reaction mass water cooler, pipeline arranges discharge port, and described discharge port is connected with described catalyst recovery devices; The recovery catalyst outlet of described catalyst recovery devices is connected with recovery catalyst inlet, and described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor.The catalyst recycle unit that the application provides and method, effectively improve the recovery utilization rate of catalyzer, the environmental pollution avoided the waste of catalyzer and therefore bring.
Description
Technical field
The present invention relates to chemical field, in particular to a kind of catalyst recycle unit and the method for preparing polymethoxy dimethyl ether.
Background technology
In prior art, such as publication number is in the patent application of CN202808649, discloses a kind of system and device preparing polymethoxy dimethyl ether, comprising: reactive system, vacuum flashing system, extracting system, caustic washing system, rectifying separation system, wherein: reactive system comprises entry mixers, annular reactor, reactor cycles pump, compensator, recirculation cooler, reactive system makes catalyzer with ionic liquid, adopts annular reactor to realize polymethoxy dimethyl ether and produces, be equipped with chuck outside annular reactor, steam, hot water or cooling water circulationly carry out heating in chuck, constant temperature or remove heat, annular reactor outside is provided with circulation line and recirculation cooler simultaneously, by the temperature in of the cooling water inflow gate ring tubular reactor of controlled circulation water cooler, described reactive system also comprises voltage-stabilizing system, voltage-stabilizing system comprises the compensator be communicated with tubular reactor, compensator gate ring tubular reactor to be delivered to by one material pressure by pipeline is drawn from the outlet of annular reactor, compensator is provided with high pressure nitrogen reducing valve and variable valve, compensator blow-down pipe is provided with pressure regulator valve with the pressure of gate ring tubular reactor, two groups of variable valve adopt Staged cotrol, two groups of variable valve carry out the pressure of gate ring tubular reactor by seperating range control high pressure nitrogen and blow-off valve, being provided with hybrid element in annular reactor, keeping the abundant mixing of material and catalyzer on the one hand, is enhancement of heat transfer effect on the other hand, maintains the carrying out of stable reaction, vacuum flashing system, extracting system, caustic washing system, rectifying separation system.
In the prior art, the recycle of catalyzer is also insufficient, therefore needs a kind of new catalyst recycling system, so that efficient and reclaim fully and recycle catalyzer, reduces the loss of catalyzer.
Summary of the invention
The object of the application is to provide a kind of catalyst recycle unit preparing polymethoxy dimethyl ether, to solve the above problems one of at least.
The application provides a kind of catalyst recycle unit preparing polymethoxy dimethyl ether, comprising: catalyst charge groove, catalyst reaction circulation device and catalyst recovery devices; Described catalyst reaction circulation device comprises reactor, reaction mass water cooler; Described catalyst charge groove is connected with the entrance of described reactor; Between the outlet that described reaction mass water cooler is arranged on described reactor and entrance, with refrigeration cycle material; Pipeline between the outlet of described reactor and described reaction mass water cooler is provided with a discharge port, and described discharge port is connected with described catalyst recovery devices; The recovery catalyst outlet of described catalyst recovery devices is connected with recovery catalyst inlet, and described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor.
Preferably, described catalyst recovery devices comprises flash drum, extraction tower and thickener; Described discharge port, described flash drum, described extraction tower and described thickener are linked in sequence; Preferably, between described flash drum and described extraction tower, be provided with material-handling pump, be provided with between described thickener and described recovery catalyst inlet and reclaim catalyst transport pump.
Preferably, the material inlet of described extraction tower is arranged on the upper end of described extraction tower, and the catalyst outlet of described extraction tower is arranged on the bottom of described extraction tower; The material inlet of described thickener is arranged on the upper end of described thickener, and the recovery catalyzer discharge port of described thickener is arranged on the bottom of described thickener.
Preferably, the top of described thickener is provided with pressure regulating valve tank connected with nitrogen and the mouth of pipe be connected with vacuum pump; The pipeline be connected with the described outlet at bottom of described thickener is sequentially set with a valve and an intermediate storage tank, and between described outlet at bottom and described valve, is also provided with an outlet branch with purging valve.
Preferably, described reactor is annular-pipe reactor, and preferably, described annular-pipe reactor is multistage annular-pipe reactor, and annular-pipe reactor at different levels connects all in turn; More preferably, annular-pipe reactor at different levels is provided with one or more entrance and one or more outlet, and an outlet of upper level annular-pipe reactor is connected by pipeline with an entrance of next stage annular-pipe reactor.
Preferably, described annular-pipe reactor arranged outside at different levels has temperature control chuck, and described temperature control chuck internal recycle has the medium that can carry out heat exchange; Between the entrance of multistage annular-pipe reactor described in the outlet of multistage annular-pipe reactor described in upper level and next stage, pressure regulating tank is set; A Matter Transfer pump and a described reaction mass water cooler are set between the outlet of described multistage annular-pipe reactor at different levels and the entrance of respective entrance or other grade of described multistage annular-pipe reactor in turn.
Preferably, described discharge port can be arranged between the outlet of multistage annular-pipe reactor described in each and the entrance of corresponding described reaction mass water cooler or only be arranged between the outlet of multistage annular-pipe reactor described in last step and the entrance of corresponding described reaction mass water cooler; Matter Transfer pump described in every one-level and between described reaction mass water cooler or only Matter Transfer pump described in last step and be provided with spent catalyst discharge port between described reaction mass water cooler, described spent catalyst discharge port is connected with spent catalyst storage tank.
Preferably, catalyst make up tank, static mixer is also comprised; The outlet of described catalyst make up tank is connected with the entrance of described catalyst charge groove, and described static mixer is arranged between described catalyst charge groove and the entrance of described reactor; Described catalyst make up tank is provided with whipping appts, and described catalyst make up tank and described catalyst charge groove are provided with the chuck for catalyzer insulation; Hot water, hot steam or heat conduction wet goods heat-transfer medium is passed in described chuck; Described catalyst recycle unit also comprises discharging dashpot, and described discharging dashpot is arranged between described discharge port and described flash drum.
Preferably, catalyst transport pump is provided with between described catalyst charge groove and described static mixer; Feed back outlet is set between described catalyst transport pump and described static mixer; Described catalyst charge groove upper end is provided with the feed back entrance exporting with described feed back and be connected.
Preferably, described discharging dashpot internal space is divided into gas phase zone and liquid phase region; The material inlet of described discharging dashpot is arranged on the position corresponding with gas phase zone.
The application also provides a kind of method utilizing above-mentioned catalyst recycle unit to carry out catalyst recirculation, said method comprising the steps of: the catalyzer in catalyst charge groove enters catalyst reaction circulation device, described catalyst reaction circulation device comprises reactor, reaction mass water cooler; Described catalyst charge groove is connected with the entrance of described reactor; Between the outlet that described reaction mass water cooler is arranged on described reactor and entrance, recycle stock is cooled; Component loops material, by being arranged on the discharge port on the pipeline between the outlet of described reactor and described reaction mass water cooler, enters catalyst recovery devices; The catalyzer reclaimed in described catalyst recovery devices enters reactor by reclaiming catalyst inlet, and described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor;
Preferably, the process reclaiming catalyzer in described catalyst recovery devices is as follows: after for some time is carried out in reaction, carry out the partial material of autoreactor through discharge hole for discharge, this strand of material enters flash drum and carries out flash distillation, light constituent exports through flash drum top, heavy constituent containing catalyzer exports through the bottom of flash drum, under the effect of material-handling pump, enter extraction tower; Complete extraction process under the effect of extraction agent after, at the bottom of the tower of extraction tower, discharging enters thickener, exports after carrying out concentrating and separating in a heated condition by bottom thickener, then directly or indirectly gets back to reactor and continues catalyzed reaction.
By a kind of catalyst recycle unit and method preparing polymethoxy dimethyl ether that the application provides, following beneficial effect can be brought:
Catalyzer enters into reaction unit by catalyst charge groove and static mixer at catalyst make up tank after pre-treatment and preparation, and its state is advantageously in catalyzed reaction; Catalyzer recycles with raw material effect in the multistage catalyst reaction circulation device, not directly with product discharging from reactor, thus reach the object of catalyst recirculation use, improve utilization ratio and the catalytic efficiency of catalyzer, reduce production cost; After reaction for some time, partially catalyzed agent inactivation, can, from extraction pipeline, be stored in spent catalyst storage tank; When reaction product discharging, partially catalyzed agent can along with product discharge, and enter into catalyst recovery devices and carry out separating treatment, the recovery catalyzer obtained sends back in reaction unit, continues to recycle in catalyst reaction circulation device; Thickener is arranged pressure regulating valve and broken negative pressure valve, can make the catalyzer extraction from thickener smoothly of thickness, improve organic efficiency, the catalyzer of more than 95% at least percent can be recycled.
Accompanying drawing explanation
A kind of schematic diagram preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 1 provides for the embodiment of the present application;
A kind of schematic diagram (reclaiming catalyst inlet different from shown in Fig. 1) preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 2 provides for the embodiment of the present application;
A kind of schematic diagram (reclaiming catalyst inlet different from shown in Fig. 1, Fig. 2) preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 3 provides for the embodiment of the present application;
A kind of schematic diagram (showing concrete catalyst recovery devices) preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 4 provides for the embodiment of the present application;
A kind of schematic diagram preparing the thickener of the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 5 provides for the embodiment of the present application;
A kind of schematic diagram (showing waste catalyst recovery device and catalyst make up tank) preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 6 provides for the embodiment of the present application;
The schematic diagram of a kind of catalyst reaction circulation device prepared in the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 7 provides for the embodiment of the present application;
The schematic diagram of a kind of another kind of catalyst reaction circulation device prepared in the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 8 provides for the embodiment of the present application.
Embodiment
Below in conjunction with drawings and Examples, the application is described in further detail.Be understandable that, specific embodiment described herein is only for explaining the application, but not the restriction to the application.
The application provides a kind of catalyst recycle unit preparing polymethoxy dimethyl ether, comprising: catalyst charge groove, catalyst reaction circulation device and catalyst recovery devices; Described catalyst reaction circulation device comprises reactor, reaction mass water cooler; Described catalyst charge groove is connected with the entrance of described reactor; Between the outlet that described reaction mass water cooler is arranged on described reactor and entrance, with refrigeration cycle material; Pipeline between the outlet of described reactor and described reaction mass water cooler is provided with a discharge port, and described discharge port is connected with described catalyst recovery devices; The recovery catalyst outlet of described catalyst recovery devices is connected with recovery catalyst inlet, and described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor.
Preferably, described catalyst recovery devices comprises flash drum, extraction tower and thickener; Described discharge port, described flash drum, described extraction tower and described thickener are linked in sequence; Preferably, between described flash drum and described extraction tower, be provided with material-handling pump, be provided with between described thickener and described recovery catalyst inlet and reclaim catalyst transport pump.
Preferably, the material inlet of described extraction tower is arranged on the upper end of described extraction tower, and the catalyst outlet of described extraction tower is arranged on the bottom of described extraction tower; The material inlet of described thickener is arranged on the upper end of described thickener, and the recovery catalyzer discharge port of described thickener is arranged on the bottom of described thickener.
Preferably, the top of described thickener is provided with pressure regulating valve tank connected with nitrogen and the mouth of pipe be connected with vacuum pump; The pipeline be connected with the described outlet at bottom of described thickener is sequentially set with a valve and an intermediate storage tank, and between described outlet at bottom and described valve, is also provided with an outlet branch with purging valve.
Preferably, described reactor is annular-pipe reactor, and preferably, described annular-pipe reactor is multistage annular-pipe reactor, and annular-pipe reactor at different levels connects all in turn; More preferably, annular-pipe reactor at different levels is provided with one or more entrance and one or more outlet, and an outlet of upper level annular-pipe reactor is connected by pipeline with an entrance of next stage annular-pipe reactor.
Preferably, described annular-pipe reactor arranged outside at different levels has temperature control chuck, and described temperature control chuck internal recycle has the medium that can carry out heat exchange; Between the entrance of multistage annular-pipe reactor described in the outlet of multistage annular-pipe reactor described in upper level and next stage, pressure regulating tank is set.
Preferably, between the outlet of described multistage annular-pipe reactor at different levels and the entrance of respective entrance or other grade of described multistage annular-pipe reactor, a Matter Transfer pump and a described reaction mass water cooler are set in turn.
Preferably, described discharge port can be arranged between the outlet of multistage annular-pipe reactor described in each and the entrance of corresponding described reaction mass water cooler or only be arranged between the outlet of multistage annular-pipe reactor described in last step and the entrance of corresponding described reaction mass water cooler; Matter Transfer pump described in every one-level and between described reaction mass water cooler or only Matter Transfer pump described in last step and be provided with spent catalyst discharge port between described reaction mass water cooler, described spent catalyst discharge port is connected with spent catalyst storage tank.
Preferably, catalyst make up tank, static mixer is also comprised; The outlet of described catalyst make up tank is connected with the entrance of described catalyst charge groove, and described static mixer is arranged between described catalyst charge groove and the entrance of described reactor; Described catalyst make up tank is provided with whipping appts, and described catalyst make up tank and described catalyst charge groove are provided with the chuck for catalyzer insulation; Hot water, hot steam or heat conduction wet goods heat-transfer medium is passed in described chuck; Described catalyst recycle unit also comprises discharging dashpot, and described discharging dashpot is arranged between described discharge port and described flash drum.
Preferably, catalyst transport pump is provided with between described catalyst charge groove and described static mixer; Feed back outlet is set between described catalyst transport pump and described static mixer; Described catalyst charge groove upper end is provided with the feed back entrance exporting with described feed back and be connected.
Preferably, described discharging dashpot internal space is divided into gas phase zone and liquid phase region; The material inlet of described discharging dashpot is arranged on the position corresponding with gas phase zone.
A kind of schematic diagram preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 1 provides for the embodiment of the present application.
As shown in Figure 1, this catalyst recycle unit comprises catalyst charge groove 100, catalyst reaction circulation device 200 and catalyst recovery devices 300; Wherein catalyst reaction circulation device 200 comprises reactor 201 and reaction mass water cooler 202.The outlet of catalyst charge groove 100 is connected with the entrance of reactor 201, and the outlet of reactor 201 is connected with the entrance of reaction mass water cooler 202, and the outlet of reaction mass water cooler 202 is connected with the entrance of reactor 201; Between the outlet and the entrance of reaction mass water cooler 202 of reactor 201, be provided with discharge port 203 be connected with catalyst recovery devices 300; Be provided with between the outlet and the entrance of reactor 201 of catalyst charge groove 100 and reclaim catalyst inlet 204, reclaim catalyst inlet 204 and be connected with the recovery catalyst outlet 301 of catalyst recovery devices 300.
A kind of schematic diagram (reclaiming catalyst inlet different from shown in Fig. 1) preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 2 provides for the embodiment of the present application.As shown in Figure 2, in another embodiment, reclaim catalyst inlet 204 can be arranged on the pipeline before the entrance of catalyst charge groove 100.
A kind of schematic diagram (reclaiming catalyst inlet different from shown in Fig. 1, Fig. 2) preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 3 provides for the embodiment of the present application.As shown in Figure 3, in a preferred embodiment, reclaim catalyst inlet 204 also can be arranged on catalyst charge groove 100.
In other examples, the place that any one those skilled in that art on pipeline that catalyst inlet 204 can be arranged on before reactor 201 entrance consider appropriate is reclaimed.
A kind of schematic diagram preparing the catalyst recycle unit (showing concrete catalyst recovery devices) of polymethoxy dimethyl ether that Fig. 4 provides for the embodiment of the present application.
As shown in Figure 4, this catalyst recycle unit comprises catalyst charge groove 100, static mixer 102, reactor 201, reaction mass water cooler 202, flash drum 302, extraction tower 303 and thickener 304.
Catalyst transport pump 104 is provided with between the outlet of catalyst charge groove 100 and the entrance of static mixer 102; Be provided with feed back between the outlet of catalyst transport pump 104 and the entrance of static mixer 102 and export 105, feed back outlet 105 is connected with the feed back entrance 106 being arranged on catalyst charge groove 100 upper end by pipeline; The outlet of static mixer 102 is connected with the entrance of reactor 201, be provided with between the outlet and the entrance of reactor 201 of static mixer 102 and reclaim catalyst inlet 204, in other examples, the position possible arbitrarily that catalyst inlet 204 can be arranged on the pipeline before the entrance of reactor 201 is reclaimed.Other reaction masses except catalyzer also enter static mixer and catalyzer is mixed together, and are not shown specifically.
Catalyzer enters in static mixer 102 through catalyst charge groove 100 and fully mixes with unclassified stores under the effect of catalyst transport pump, then enters into reaction in reactor 201.The skin of catalyst charge groove is provided with the chuck (not shown) of insulation, passes into hot water, hot steam or heat conduction wet goods heat-transfer medium in chuck; Arranging of feed back outlet 105 and feed back entrance 106 one is work output in order to regulate catalyzer, and two is to make catalyst charge groove 100 itself form a partial circulating, to tackle the generation of the emergency case such as the improper or abnormal reaction of catalytic heating temperature.
The outlet of reactor 201 is connected with the entrance of Matter Transfer pump 206, and the outlet of Matter Transfer pump 206 is connected with the entrance of reaction mass water cooler 202, and the outlet of reaction mass water cooler 202 is connected with the entrance of reactor 201; After catalyzer reacts for some time along with raw material in reactor 201, remove heat through reaction mass water cooler 202 under the effect of Matter Transfer pump 206, get back in reactor 201 and continue reaction.
The setting of reaction cycle device, makes reaction unit itself form a circulation, effectively utilizes catalyzer, add the carrying out of fast response, and that impels reaction to carry out is more stable.
Discharge port 203 is provided with between the outlet of reactor 201 and Matter Transfer pump 206, discharge port 203 is connected with the entrance of flash drum, and the outlet of the catalyst mix material of flash drum 203 to be arranged on bottom cell body and to be connected with the material inlet of the extraction tower being arranged on extraction tower 303 upper end; Material-handling pump 305 is provided with between the material inlet of the catalyst mix material outlet of flash drum 203 and the extraction tower of extraction tower 303 upper end; The catalyst outlet of extraction tower 303 is arranged on bottom and is connected with the material inlet of thickener 304; The recovery catalyzer discharge port of thickener 304 is connected with recovery catalyst inlet 204, and the recovery catalyzer discharge port of thickener 304 and reclaim to be provided with between catalyst inlet 204 and reclaim catalyst transport pump 306.
After for some time is carried out in reaction, reactor 201 exports one material through discharge port 203.This strand of material enters flash drum 302 and carries out flash distillation, and light constituent exports through flash drum 302 top, and the heavy constituent containing catalyzer exports through the bottom of flash drum 302, under the effect of material-handling pump 305, enter extraction tower 303; Complete extraction process under the effect of extraction agent after, at the bottom of the tower of extraction tower 303, discharging enters thickener 304, export by bottom thickener 304 after carrying out concentrating and separating in a heated condition, under the effect of reclaiming catalyst transport pump 306, get back to reactor 201 through recovery catalyst inlet 204 continue catalyzed reaction.Catalyzer after certain recovery directly can get back in reaction system (as shown in the figure), also can be stored in and reclaim in catalyst carrier, then get back to reactor 201 from recovery catalyst carrier continue catalyzed reaction (this is indirect mode) through reclaiming catalyst inlet 204.
The schematic diagram of a kind of thickener prepared in the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 5 provides for the embodiment of the present application.
As shown in Figure 5, in a preferred embodiment, the top of thickener 304 is provided with pressure regulating valve tank connected with nitrogen 3041, mouth of pipe be connected with vacuum pump 3044 and thickener top discharge mouth (non-label); Pipeline between thickener 304 and recovery catalyst transport pump 306 is sequentially set with a broken negative pressure valve 3042, a valve 3045 is set after the branch of broken negative pressure valve 3042 again, avoid thickener to influence each other with device below like this, be provided with thereafter an intermediate storage tank 3043.
After having concentrated, working pressure due to thickener 304 is negative pressure, and it is larger owing to reclaiming Catalyst Viscosity, not easily extraction from thickener 304, now open pressure regulating valve 3041 and input nitrogen, increase the pressure of thickener 304, open brokenly negative pressure valve 3042 simultaneously, abolish the negative pressure state (also first can break negative pressure below) of thickener 304 up and down simultaneously, thus make to reclaim catalyzer at normal pressure even higher than (malleation) under the state of normal pressure, extraction from thickener 304 smoothly, enter in intermediate storage tank 3043, and then by under the effect of reclaiming catalyst transport pump 306, get back to reaction wherein to recycle.Can the operating time be reduced like this, increase work efficiency.
A kind of schematic diagram (showing waste catalyst recovery device and catalyst make up tank) preparing the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 6 provides for the embodiment of the present application.
As shown in Figure 6, compared with the catalyst recycle unit shown in Fig. 4, the difference of this catalyst recycle unit is: first, catalyst make up tank 101 was added before catalyst charge groove, catalyst make up tank 101 skin is provided with the chuck (not shown) of insulation, pass into hot water, hot steam or heat conduction wet goods heat-transfer medium in chuck, catalyst make up tank 101 inside is provided with whipping appts 103, for being stirred by catalyzer; The second, between discharge port 203 and flash drum 302, be provided with a discharging dashpot 205, for cushioning the material with certain pressure and temperature exported from reactor 201, and the material under preventing emergency case flows backwards.
The ionic-liquid catalyst that this reaction uses presents solid-state or solid-liquid mixing at normal temperatures, and when reacting in reactor, unclassified stores is liquid state, when catalyzer is liquid, result of use is best, therefore, need before use first to carry out necessary preparation to it in catalyst make up tank, make it meet the needs of reaction.
The schematic diagram of a kind of catalyst reaction circulation device prepared in the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 7 provides for the embodiment of the present application.
Catalyst reaction circulation device as shown in Figure 7, the difference of the catalyst reaction circulation device in the catalyst recycle unit shown in its from Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 6 is that the progression of its reactor 201 is different, and reaction mass water cooler 202 is different with the number of Matter Transfer pump 206.Specifically be described below:
Reactor 201 is as shown in Figure 7 two-stage annular-pipe reactor, is respectively the multistage annular-pipe reactor 2012 of the multistage annular-pipe reactor of the first step 2011 and the second stage; Be connected by pipeline between the entrance of the multistage annular-pipe reactor 2012 of the outlet of the multistage annular-pipe reactor of the first step 2011 and the second stage; The outside of the multistage annular-pipe reactor 2012 of the multistage annular-pipe reactor of the first step 2011 and the second stage is provided with temperature control chuck 2013, and temperature control chuck 2013 internal recycle has the medium that can carry out heat exchange, as water, hot steam, heat conduction wet goods; The outlet of the multistage annular-pipe reactor 2011 of the first step is connected with the entrance of a Matter Transfer pump 2061, the outlet of Matter Transfer pump 2061 is connected with the entrance of reaction mass water cooler 2021, and the outlet of reaction mass water cooler 2021 is connected in the entrance of the multistage annular-pipe reactor 2011 of the first step; Same, the outlet of the multistage annular-pipe reactor 2012 in the second stage is connected with the entrance of a Matter Transfer pump 2062, the outlet of Matter Transfer pump 2062 is connected with the entrance of reaction mass water cooler 2022, and the outlet of reaction mass water cooler 2022 is connected in the entrance of the multistage annular-pipe reactor 2012 of the first step.Between the entrance of the multistage annular-pipe reactor 2012 of outlet and the second stage of the multistage annular-pipe reactor of the first step 2011, be also provided with a pressure regulating tank 209 and the device such as attached pump and valve thereof.Between the outlet and the entrance of Matter Transfer pump 2062 of the multistage annular-pipe reactor 2012 in the second stage, be provided with discharge port 203, discharge port 203 is connected with discharging dashpot.
Hybrid reaction material containing catalyzer enters the multistage annular-pipe reactor 2011 of the first step through the entrance of the multistage annular-pipe reactor of the first step 2011, temperature control chuck 2013 by heat exchange medium be used for ensure the temperature of reaction needed; The outlet of the multistage annular-pipe reactor 2011 of the first step separates two strands of materials, one enters into the multistage annular-pipe reactor 2012 in the second stage and continues reaction, another strand enters into reaction mass water cooler 2021 under the effect of Matter Transfer pump 2061 to carry out removing heat, and the entrance then through the multistage annular-pipe reactor of the first step 2011 gets back to continuation reaction in the multistage annular-pipe reactor 2011 of the first step; When the reaction pressure of the multistage annular-pipe reactor 2012 of the multistage annular-pipe reactor of the first step 2011 and the second stage needs to regulate, valve open on pressure regulating tank 209, regulate reacting system pressure, a little material entering pressure regulating tank 209 is got back in the multistage annular-pipe reactor 2012 in the second stage and is reacted under the effect of pump; Material in the multistage annular-pipe reactor 2012 in the second stage can circulate under the effect of Matter Transfer pump 2062 and reaction mass water cooler 2022; When be reacted to a certain degree need extraction material time, discharge port 203 is opened, and one material of extraction enters in discharging surge tank 205, then carries out the work of recovery catalyzer.Through laboratory test, reaction of high order system operation more than this two-stage is more steadily easier, can quiet run for a long time., may there are the big ups and downs of 2-5 secondary response every day in the control relative difficulty of single-stage annular-pipe reactor comparatively speaking, and multistage annular-pipe reactor can reach continuous one week does not occur large fluctuation.。
The schematic diagram of a kind of another kind of catalyst reaction circulation device prepared in the catalyst recycle unit of polymethoxy dimethyl ether that Fig. 8 provides for the embodiment of the present application.
Catalyst reaction circulation device as shown in Figure 8, the difference of the catalyst reaction circulation device shown in itself and Fig. 7 is: add the multistage annular-pipe reactor 2014 of the third stage, adds a pressure regulating tank 209 and one group of Matter Transfer pump 2063, reaction mass water cooler 2023 accordingly.
In the catalyst reaction circulation device shown in Fig. 8, the multistage annular-pipe reactor of every one-level is corresponding with corresponding one group of Matter Transfer pump and reaction mass water cooler respectively, and Matter Transfer pump and reaction mass water cooler are arranged between the outlet of this grade of annular-pipe reactor and entrance all in turn; A pressure regulating tank is provided with between the multistage annular-pipe reactor of every two-stage neighboring; Discharge port is only arranged at the exit of the multistage annular-pipe reactor of last step.
In other examples, between the outlet that also can be arranged on the multistage annular-pipe reactor of one-level of one group of Matter Transfer pump and reaction mass water cooler and the entrance of other grade of multistage annular-pipe reactor; Between the outlet that discharge port 203 also can be arranged on the multistage annular-pipe reactor of every one-level and corresponding reaction mass water cooler; The number of multistage annular-pipe reactor also can change, as three grades, Pyatyi, ten grades or more multistage number.If small, preferred two-stage is to Pyatyi.
The method that the catalyst recycle unit utilizing the application to provide carries out catalyst recirculation is as follows, said method comprising the steps of: the catalyzer in catalyst charge groove enters catalyst reaction circulation device, described catalyst reaction circulation device comprises reactor, reaction mass water cooler; Described catalyst charge groove is connected with the entrance of described reactor; Between the outlet that described reaction mass water cooler is arranged on described reactor and entrance, recycle stock is cooled; Component loops material, by being arranged on the discharge port on the pipeline between the outlet of described reactor and described reaction mass water cooler, enters catalyst recovery devices; The catalyzer reclaimed in described catalyst recovery devices enters reactor by reclaiming catalyst inlet, and described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor.Wherein, the process reclaiming catalyzer in described catalyst recovery devices is roughly as follows: after for some time is carried out in reaction, carry out the partial material of autoreactor through discharge hole for discharge, this strand of material enters flash drum and carries out flash distillation, light constituent exports through flash drum top, heavy constituent containing catalyzer exports through the bottom of flash drum, under the effect of material-handling pump, enter extraction tower; Complete extraction process under the effect of extraction agent after, at the bottom of the tower of extraction tower, discharging enters thickener, exports after carrying out concentrating and separating in a heated condition by bottom thickener, then directly or indirectly gets back to reactor and continues catalyzed reaction.
Utilize the device and method of the application, the catalyzer of more than 95% (about 95%-99.8%, such as 96%, 98%, 99.5%) can recycle and reuse.
Use the method, two circulations of catalyzer can be formed.First circulation is reaction partial circulating, after catalyzer reacts for some time in the reactor, with reaction raw materials extraction simultaneously, enter in reaction mass water cooler and remove heat, then get back in reactor and continue reaction, under the prerequisite not increasing reactor, increase the flow process of reaction, also can reduce the severe degree of reaction simultaneously, effectively control the carrying out of reaction; Second circulation is reaction recovery systemic circulation, and catalyzer after extraction, carries out separation concentrate through flash tank, extraction tower, thickener, most of catalyst recovery utilized from reactor.
The foregoing is only the preferred embodiment of the application, be not limited to the application, for a person skilled in the art, the application can have various modifications and variations.Within all spirit in the application and principle, any amendment done, equivalent replacement, improvement etc., within the protection domain that all should be included in the application.
Claims (7)
1. prepare a catalyst recycle unit for polymethoxy dimethyl ether, it is characterized in that, comprising: catalyst charge groove, catalyst reaction circulation device and catalyst recovery devices; Described catalyst reaction circulation device comprises reactor, reaction mass water cooler; Described catalyst charge groove is connected with the entrance of described reactor; Between the outlet that described reaction mass water cooler is arranged on described reactor and entrance, with refrigeration cycle material; Pipeline between the outlet of described reactor and described reaction mass water cooler is provided with a discharge port, and described discharge port is connected with described catalyst recovery devices; The recovery catalyst outlet of described catalyst recovery devices is connected with recovery catalyst inlet, and described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor; Described catalyst recovery devices comprises flash drum, extraction tower and thickener; Described discharge port, described flash drum, described extraction tower and described thickener are linked in sequence; Be provided with material-handling pump between described flash drum and described extraction tower, be provided with between described thickener and described recovery catalyst inlet and reclaim catalyst transport pump; The material inlet of described extraction tower is arranged on the upper end of described extraction tower, and the catalyst outlet of described extraction tower is arranged on the bottom of described extraction tower; The material inlet of described thickener is arranged on the upper end of described thickener, and the recovery catalyzer discharge port of described thickener is arranged on the bottom of described thickener; The top of described thickener is provided with pressure regulating valve tank connected with nitrogen and the mouth of pipe be connected with vacuum pump; The pipeline be connected with the outlet at bottom of described thickener is sequentially set with a valve and an intermediate storage tank, and between described outlet at bottom and described valve, is also provided with an outlet branch with purging valve; Described catalyst recycle unit also comprises catalyst make up tank, static mixer; The outlet of described catalyst make up tank is connected with the entrance of described catalyst charge groove, and described static mixer is arranged between described catalyst charge groove and the entrance of described reactor; Described catalyst make up tank is provided with whipping appts, and described catalyst make up tank and described catalyst charge groove are provided with the chuck for catalyzer insulation; The heat-transfer medium being selected from hot water, hot steam or thermal oil is passed in described chuck; Described catalyst recycle unit also comprises discharging dashpot, and described discharging dashpot is arranged between described discharge port and described flash drum.
2. catalyst recycle unit according to claim 1, is characterized in that, described reactor is annular-pipe reactor, and described annular-pipe reactor is multistage annular-pipe reactor, and annular-pipe reactor at different levels connects all in turn; Annular-pipe reactor at different levels is provided with one or more entrance and one or more outlet, and an outlet of upper level annular-pipe reactor is connected by pipeline with an entrance of next stage annular-pipe reactor.
3. catalyst recycle unit according to claim 2, is characterized in that, described annular-pipe reactor arranged outside at different levels has temperature control chuck, and described temperature control chuck internal recycle has the medium that can carry out heat exchange; Between the entrance of multistage annular-pipe reactor described in the outlet of multistage annular-pipe reactor described in upper level and next stage, pressure regulating tank is set; A Matter Transfer pump and a described reaction mass water cooler are set between the outlet of described multistage annular-pipe reactor at different levels and the entrance of respective entrance or other grade of described multistage annular-pipe reactor in turn.
4. catalyst recycle unit according to claim 3, it is characterized in that, described discharge port is arranged between the outlet of multistage annular-pipe reactor described in each and the entrance of corresponding described reaction mass water cooler or is only arranged between the outlet of multistage annular-pipe reactor described in last step and the entrance of corresponding described reaction mass water cooler; Matter Transfer pump described in every one-level and between described reaction mass water cooler or only Matter Transfer pump described in last step and be provided with spent catalyst discharge port between described reaction mass water cooler, described spent catalyst discharge port is connected with spent catalyst storage tank.
5. catalyst recycle unit according to claim 1, is characterized in that, is provided with catalyst transport pump between described catalyst charge groove and described static mixer; Feed back outlet is set between described catalyst transport pump and described static mixer; Described catalyst charge groove upper end is provided with the feed back entrance exporting with described feed back and be connected.
6. catalyst recycle unit according to claim 1, is characterized in that, described discharging dashpot internal space is divided into gas phase zone and liquid phase region; The material inlet of described discharging dashpot is arranged on the position corresponding with gas phase zone.
7. the method utilizing the catalyst recycle unit according to claim 1-6 to carry out catalyst recirculation, said method comprising the steps of: the catalyzer in catalyst charge groove enters catalyst reaction circulation device, described catalyst reaction circulation device comprises reactor, reaction mass water cooler; Described catalyst charge groove is connected with the entrance of described reactor; Between the outlet that described reaction mass water cooler is arranged on described reactor and entrance, recycle stock is cooled; Component loops material, by being arranged on the discharge port on the pipeline between the outlet of described reactor and described reaction mass water cooler, enters catalyst recovery devices; The catalyzer reclaimed in described catalyst recovery devices enters reactor by reclaiming catalyst inlet, and described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor; The process reclaiming catalyzer in described catalyst recovery devices is as follows: after for some time is carried out in reaction, carry out the partial material of autoreactor through discharge hole for discharge, this strand of material enters flash drum and carries out flash distillation, light constituent exports through flash drum top, heavy constituent containing catalyzer exports through the bottom of flash drum, under the effect of material-handling pump, enter extraction tower; Complete extraction process under the effect of extraction agent after, at the bottom of the tower of extraction tower, discharging enters thickener, exports after carrying out concentrating and separating in a heated condition by bottom thickener, then directly or indirectly gets back to reactor and continues catalyzed reaction.
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| US20110288343A1 (en) * | 2010-05-18 | 2011-11-24 | Lanzhou Institute Of Chemical Physics, Chinese Academy Of Sciences | Method for synthesizing polyoxymethylene dimethyl ethers catalyzed by an ionic liquid |
| CN202808649U (en) * | 2012-06-11 | 2013-03-20 | 北京科尔帝美工程技术有限公司 | Systemic device for preparing polyoxymethylene dimethyl ether |
| CN202962442U (en) * | 2012-12-13 | 2013-06-05 | 北京东方红升新能源应用技术研究院有限公司 | Liquid phase reaction device for synthesizing polymethoxy dialkyl ether |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110288343A1 (en) * | 2010-05-18 | 2011-11-24 | Lanzhou Institute Of Chemical Physics, Chinese Academy Of Sciences | Method for synthesizing polyoxymethylene dimethyl ethers catalyzed by an ionic liquid |
| CN202808649U (en) * | 2012-06-11 | 2013-03-20 | 北京科尔帝美工程技术有限公司 | Systemic device for preparing polyoxymethylene dimethyl ether |
| CN202962442U (en) * | 2012-12-13 | 2013-06-05 | 北京东方红升新能源应用技术研究院有限公司 | Liquid phase reaction device for synthesizing polymethoxy dialkyl ether |
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