CN104177235A - Catalyst circulation system for preparing polyoxymethylene dimethyl ether, and method thereof - Google Patents
Catalyst circulation system for preparing polyoxymethylene dimethyl ether, and method thereof Download PDFInfo
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- CN104177235A CN104177235A CN201310613341.1A CN201310613341A CN104177235A CN 104177235 A CN104177235 A CN 104177235A CN 201310613341 A CN201310613341 A CN 201310613341A CN 104177235 A CN104177235 A CN 104177235A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
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Abstract
The invention relates to a catalyst circulation system for preparing polyoxymethylene dimethyl ether, and a method thereof. The catalyst circulation system comprises a catalyst feeding tank, a catalyst reaction circulation device and a catalyst recovering device; the catalyst reaction circulation device comprises a reactor and a reaction material cooler; the catalyst feeding tank is connected with the inlet of the reactor; the reaction material cooler is arranged between the outlet and the inlet of the reactor; a pipeline between the outlet of the reactor and the reaction material cooler is provided with a discharging hole, and the discharging hole is connected with the catalyst recovering device; and the recovered catalyst outlet of the catalyst recovering device is connected with a recovered catalyst inlet, and the recovered catalyst inlet is arranged on a pipeline in front of the inlet of the reactor. The catalyst circulation system and the method thereof effectively improve the catalyst recycling rate and avoid catalyst waste and environmental pollution caused by the catalyst waste.
Description
Technical field
The present invention relates to chemical field, in particular to a kind of catalyst recirculation system and method for preparing polymethoxy dimethyl ether.
Background technology
In prior art, for example, in the patent application that publication number is CN202808649, disclose a kind of system and device of preparing polymethoxy dimethyl ether, having comprised: 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 is made catalyzer with ionic liquid, adopts annular reactor to realize polymethoxy dimethyl ether and produces, and annular reactor outside is equipped with chuck, steam, hot water or cooling water circulationly in chuck, heat, constant temperature or remove heat, annular reactor outside is provided with circulation line and recirculation cooler simultaneously, the temperature in of the cooling water inflow gate ring tubular reactor by controlled circulation water cooler, described reactive system also comprises voltage-stabilizing system, voltage-stabilizing system comprises the compensator being communicated with tubular reactor, from the outlet of annular reactor, draw one material and by pipeline, deliver to the pressure of compensator gate ring tubular 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 a minute process control, 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, in annular reactor, be provided with hybrid element, the abundant mixing that keeps 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 recirculation system, so that efficient, also reclaims fully and recycle catalyzer, reduces the loss of catalyzer.
Summary of the invention
The application's object is to provide a kind of catalyst recirculation system of preparing polymethoxy dimethyl ether, one of to solve the above problems at least.
The application provides a kind of catalyst recirculation system of 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; The entrance of described catalyst charge groove and described reactor is connected; Described reaction mass water cooler is arranged between the outlet and entrance of described reactor, with refrigeration cycle material; On pipeline between the outlet of described reactor and described reaction mass water cooler, be provided with a discharge port, described discharge port is connected with described catalyst recovery devices; The recovery catalyst outlet of described catalyst recovery devices with reclaim catalyst inlet and be connected, 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, between described thickener and described recovery catalyst inlet, be provided with 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 and the tank connected pressure regulating valve of nitrogen and the mouth of pipe being connected with vacuum pump; On the pipeline being connected with the described outlet at bottom of described thickener, be sequentially set with a valve and an intermediate storage tank, and be also provided with one with the outlet branch of purging valve between described outlet at bottom and described valve.
Preferably, described reactor is annular-pipe reactor, and preferably, described annular-pipe reactor is multistage annular-pipe reactor, and annular-pipe reactors at different levels all connect in turn; More preferably, annular-pipe reactors at different levels are provided with one or more entrances 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 have temperature control chuck, and described temperature control chuck internal recycle has the medium that can carry out heat exchange; Described in upper level, described in the outlet of multistage annular-pipe reactor and next stage, between the entrance of multistage annular-pipe reactor, pressure regulating tank is set; A Matter Transfer pump and a described reaction mass water cooler are set between the entrance of the outlet of described multistage annular-pipe reactors at different levels and an entrance separately or other grade of described multistage annular-pipe reactor in turn.
Preferably, described discharge port can be arranged on described in each between the outlet of multistage annular-pipe reactor and the entrance of corresponding described reaction mass water cooler or only be arranged on described in last step between the outlet of multistage annular-pipe reactor and the entrance of corresponding described reaction mass water cooler; Described in every one-level, between Matter Transfer pump and described reaction mass water cooler or only between Matter Transfer pump and described reaction mass water cooler, be provided with spent catalyst discharge port described in last step, described spent catalyst discharge port is connected with spent catalyst storage tank.
Preferably, also comprise 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; In described chuck, pass into hot water, hot steam or heat conduction wet goods heat-transfer medium; Described catalyst recirculation system also comprises discharging dashpot, and described discharging dashpot is arranged between described discharge port and described flash drum.
Preferably, between described catalyst charge groove and described static mixer, be provided with catalyst transport pump; 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 being connected with described feed back outlet.
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 and utilizes above-mentioned catalyst recirculation system to carry out the method for 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; The entrance of described catalyst charge groove and described reactor is connected; Described reaction mass water cooler is arranged between the outlet and entrance of described reactor, to recycle stock, carries out cooling; Part recycle stock, by being arranged on the outlet of described reactor and the discharge port on the pipeline between described reaction mass water cooler, entering catalyst recovery devices and connects; The catalyzer reclaiming 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 that reclaims catalyzer in described catalyst recovery devices is as follows: reaction was carried out after for some time, come the partial material of autoreactor through discharge hole for discharge, this strand of material enters flash drum and carries out flash distillation, light constituent is exported through flash drum top, the heavy constituent that contains catalyzer, through the output of the bottom of flash drum, enters extraction tower under the effect of material-handling pump; Under the effect of extraction agent, complete after extraction process, from discharging at the bottom of the tower of extraction tower, enter thickener, under heating condition, carry out after concentrating and separating, by the output of thickener bottom, then directly or indirectly getting back to reactor and continuing catalyzed reaction.
A kind of catalyst recirculation system and method for preparing polymethoxy dimethyl ether providing by the application, can bring following beneficial effect:
Catalyzer enters into reaction unit by catalyst charge groove and static mixer after catalyst make up tank is through pre-treatment and preparation, and its state is conducive to catalyzed reaction more; Catalyzer in multistage catalyst reaction circulation device with raw material effect and recycle, directly do not follow product discharging from reactor, thereby reached the object that catalyst recirculation is used, improved utilization ratio and the catalytic efficiency of catalyzer, reduced production costs; After reaction for some time, partially catalyzed agent inactivation, can extraction from pipeline, is stored in spent catalyst storage tank; When reaction product discharging, partially catalyzed agent meeting is accompanied by product discharging, enters into catalyst recovery devices and carries out separating treatment, and the recovery catalyzer obtaining sends back in reaction unit, continues to recycle in catalyst reaction circulation device; Pressure regulating valve and broken negative pressure valve are set on thickener, can make the catalyzer extraction from thickener smoothly of thickness, improved organic efficiency, more than 95% at least percent catalyzer can be recycled.
Accompanying drawing explanation
A kind of schematic diagram of preparing the catalyst recirculation system of polymethoxy dimethyl ether that Fig. 1 provides for the embodiment of the present application;
A kind of schematic diagram (reclaiming catalyst inlet from different shown in Fig. 1) of preparing the catalyst recirculation system of polymethoxy dimethyl ether that Fig. 2 provides for the embodiment of the present application;
A kind of schematic diagram (reclaiming catalyst inlet from different shown in Fig. 1, Fig. 2) of preparing the catalyst recirculation system 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) of preparing the catalyst recirculation system of polymethoxy dimethyl ether that Fig. 4 provides for the embodiment of the present application;
The schematic diagram of the thickener in a kind of catalyst recirculation system of preparing 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) of preparing the catalyst recirculation system of polymethoxy dimethyl ether that Fig. 6 provides for the embodiment of the present application;
The schematic diagram of the catalyst reaction circulation device in a kind of catalyst recirculation system of preparing polymethoxy dimethyl ether that Fig. 7 provides for the embodiment of the present application;
The schematic diagram of the another kind of catalyst reaction circulation device in a kind of catalyst recirculation system of preparing 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 restriction to the application.
The application provides a kind of catalyst recirculation system of 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; The entrance of described catalyst charge groove and described reactor is connected; Described reaction mass water cooler is arranged between the outlet and entrance of described reactor, with refrigeration cycle material; On pipeline between the outlet of described reactor and described reaction mass water cooler, be provided with a discharge port, described discharge port is connected with described catalyst recovery devices; The recovery catalyst outlet of described catalyst recovery devices with reclaim catalyst inlet and be connected, 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, between described thickener and described recovery catalyst inlet, be provided with 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 and the tank connected pressure regulating valve of nitrogen and the mouth of pipe being connected with vacuum pump; On the pipeline being connected with the described outlet at bottom of described thickener, be sequentially set with a valve and an intermediate storage tank, and be also provided with one with the outlet branch of purging valve between described outlet at bottom and described valve.
Preferably, described reactor is annular-pipe reactor, and preferably, described annular-pipe reactor is multistage annular-pipe reactor, and annular-pipe reactors at different levels all connect in turn; More preferably, annular-pipe reactors at different levels are provided with one or more entrances 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 have temperature control chuck, and described temperature control chuck internal recycle has the medium that can carry out heat exchange; Described in upper level, described in the outlet of multistage annular-pipe reactor and next stage, between the entrance of multistage annular-pipe reactor, pressure regulating tank is set.
Preferably, a Matter Transfer pump and a described reaction mass water cooler are set in turn between the outlet of described multistage annular-pipe reactors at different levels and the entrance of an entrance separately or other grade of described multistage annular-pipe reactor.
Preferably, described discharge port can be arranged on described in each between the outlet of multistage annular-pipe reactor and the entrance of corresponding described reaction mass water cooler or only be arranged on described in last step between the outlet of multistage annular-pipe reactor and the entrance of corresponding described reaction mass water cooler; Described in every one-level, between Matter Transfer pump and described reaction mass water cooler or only between Matter Transfer pump and described reaction mass water cooler, be provided with spent catalyst discharge port described in last step, described spent catalyst discharge port is connected with spent catalyst storage tank.
Preferably, also comprise 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; In described chuck, pass into hot water, hot steam or heat conduction wet goods heat-transfer medium; Described catalyst recirculation system also comprises discharging dashpot, and described discharging dashpot is arranged between described discharge port and described flash drum.
Preferably, between described catalyst charge groove and described static mixer, be provided with catalyst transport pump; 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 being connected with described feed back outlet.
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 of preparing the catalyst recirculation system of polymethoxy dimethyl ether that Fig. 1 provides for the embodiment of the present application.
As shown in Figure 1, this catalyst recirculation system 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 of reactor 201 and the entrance of reaction mass water cooler 202, being provided with discharge port 203 is connected with catalyst recovery devices 300; Between the outlet of catalyst charge groove 100 and the entrance of reactor 201, be provided with 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 from different shown in Fig. 1) of preparing the catalyst recirculation system of polymethoxy dimethyl ether that Fig. 2 provides for the embodiment of the present application.As shown in Figure 2, in another embodiment, reclaim on the pipeline before the entrance that catalyst inlet 204 can be arranged on catalyst charge groove 100.
A kind of schematic diagram (reclaiming catalyst inlet from different shown in Fig. 1, Fig. 2) of preparing the catalyst recirculation system 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 and also can be arranged on catalyst charge groove 100.
In other embodiment, reclaim catalyst inlet 204 and can be arranged on the place that any one those skilled in that art on reactor 201 entrances pipeline before consider appropriate.
A kind of schematic diagram of preparing the catalyst recirculation system (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 recirculation system comprises catalyst charge groove 100, static mixer 102, reactor 201, reaction mass water cooler 202, flash drum 302, extraction tower 303 and thickener 304.
Between the entrance of the outlet of catalyst charge groove 100 and static mixer 102, be provided with catalyst transport pump 104; Between the entrance of the outlet of catalyst transport pump 104 and static mixer 102, be provided with feed back outlet 105, feed back outlet 105 is connected with the feed back entrance 106 that is arranged on catalyst charge groove 100 upper ends by pipeline; The outlet of static mixer 102 is connected with the entrance of reactor 201, between the outlet of static mixer 102 and the entrance of reactor 201, be provided with and reclaim catalyst inlet 204, in other embodiment, reclaim any possible position of the pipeline before the entrance that catalyst inlet 204 can be arranged on reactor 201.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 and fully mixes with unclassified stores under the effect of catalyst transport pump through catalyst charge groove 100, then enters into the interior reaction of reactor 201.The skin of catalyst charge groove is provided with the chuck (not shown) of insulation use, 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 in order to regulate the work output of catalyzer, the 2nd, and in order 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 catalyzer 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; Catalyzer is accompanied by raw material and after interior reaction for some time, under the effect of Matter Transfer pump 206, through the heat of removing of reaction mass water cooler 202, gets back to the interior continuation reaction of reactor 201 at reactor 201.
The setting of reaction cycle device, makes reaction unit itself form a circulation, effectively utilizes catalyzer, adds the carrying out of fast response, impels and reacts carry out more stable.
Between the outlet of reactor 201 and Matter Transfer pump 206, be provided with discharge port 203, discharge port 203 is connected with the entrance of flash drum, and the catalyst mix material outlet of flash drum 203 is arranged on cell body bottom and is connected with the material inlet that is arranged on the extraction tower of extraction tower 303 upper ends; Between the material inlet of the catalyst mix material outlet of flash drum 203 and the extraction tower of extraction tower 303 upper ends, be provided with material-handling pump 305; 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 is provided with and reclaims catalyst transport pump 306 between the recovery catalyzer discharge port of thickener 304 and recovery catalyst inlet 204.
Reaction was carried out after for some time, and reactor 201 is through discharge port 203 one materials of output.This strand of material enters flash drum 302 and carries out flash distillation, and light constituent is through flash drum 302 top outputs, and the heavy constituent that contains catalyzer, through the output of the bottom of flash drum 302, enters extraction tower 303 under the effect of material-handling pump 305; Under the effect of extraction agent, complete after extraction process, from discharging at the bottom of the tower of extraction tower 303, enter thickener 304, under heating condition, carry out by thickener 304 bottoms, being exported after concentrating and separating, under the effect of reclaiming catalyst transport pump 306, through reclaiming catalyst inlet 204, get back to reactor 201 continuation catalyzed reactions.Certainly the catalyzer after reclaiming can directly be got back to (as shown in the figure) in reaction system, also can be stored in and reclaim in catalyzer storage tank, then through reclaiming catalyst inlet 204, get back to reactor 201 continuation catalyzed reactions (this is indirect mode) from reclaiming catalyzer storage tank.
The schematic diagram of the thickener in a kind of catalyst recirculation system of preparing 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 and the tank connected pressure regulating valve of nitrogen 3041, the mouth of pipe being connected with vacuum pump 3044 and a thickener top discharge mouth (not label); On pipeline between thickener 304 and recovery catalyst transport pump 306, be sequentially set with a broken negative pressure valve 3042, after the branch of broken negative pressure valve 3042, a valve 3045 is set again, avoid like this thickener and device below to influence each other, be provided with thereafter an intermediate storage tank 3043.
After having concentrated, because the working pressure of thickener 304 is negative pressure, and larger owing to reclaiming catalyzer viscosity, be difficult for extraction from thickener 304, now open pressure regulating valve 3041 input nitrogen, increase the pressure of thickener 304, open brokenly negative pressure valve 3042 simultaneously, abolish up and down the negative pressure state (also can first break negative pressure below) of thickener 304 simultaneously, thereby make to reclaim catalyzer in normal pressure even (malleation) under the state higher than normal pressure, extraction from thickener 304 smoothly, enter in intermediate storage tank 3043, and then by reclaiming under the effect of catalyst transport pump 306, getting back to reaction wherein recycles.Can reduce the operating time like this, increase work efficiency.
A kind of schematic diagram (showing waste catalyst recovery device and catalyst make up tank) of preparing the catalyst recirculation system of polymethoxy dimethyl ether that Fig. 6 provides for the embodiment of the present application.
As shown in Figure 6, compare with the catalyst recirculation system shown in Fig. 4, the difference of this catalyst recirculation system is: first, before catalyst charge groove, added catalyst make up tank 101, catalyst make up tank 101 skins are provided with the chuck (not shown) of insulation use, in chuck, pass into hot water, hot steam or heat conduction wet goods heat-transfer medium, catalyst make up tank 101 inside are provided with whipping appts 103, for catalyzer is stirred; The second, between discharge port 203 and flash drum 302, be provided with a discharging dashpot 205, for cushioning from the material with certain pressure and temperature of reactor 201 outputs, and prevent that the material under emergency case from flowing backwards.
The ionic-liquid catalyst that this reaction is used presents solid-state or solid-liquid mixing at normal temperatures, and while reacting in reactor, unclassified stores is liquid state, when catalyzer is liquid, result of use is best, therefore, before using, need in catalyst make up tank, first to it, carry out necessary preparation, make it meet the needs of reaction.
The schematic diagram of the catalyst reaction circulation device in a kind of catalyst recirculation system of preparing polymethoxy dimethyl ether that Fig. 7 provides for the embodiment of the present application.
Catalyst reaction circulation device as shown in Figure 7, it is that from the difference of catalyst reaction circulation device in the catalyst recirculation system shown in Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 6 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 2011 of the first step and the second stage; Between the entrance of the multistage annular-pipe reactor 2012 of the outlet of the multistage annular-pipe reactor 2011 of the first step and the second stage, by pipeline, be connected; The outside of the multistage annular-pipe reactor 2011 of the first step and the multistage annular-pipe reactor 2012 in the second stage is provided with temperature control chuck 2013, and temperature control chuck 2013 internal recycle have 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 2011 of the first step, be also provided with the devices such as a pressure regulating tank 209 and attached pump thereof and valve.Between the outlet of the multistage annular-pipe reactor 2012 in the second stage and the entrance of Matter Transfer pump 2062, be provided with discharge port 203, discharge port 203 is connected with discharging dashpot.
The hybrid reaction material that contains catalyzer enters the multistage annular-pipe reactor 2011 of the first step through the entrance of the multistage annular-pipe reactor 2011 of the first step, and temperature control chuck 2013 is by the temperature that is used for guaranteeing reaction needed of heat exchange medium; 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 and removes heat under the effect of Matter Transfer pump 2061, then through the entrance of the multistage annular-pipe reactor 2011 of the first step, gets back in the multistage annular-pipe reactor 2011 of the first step and continues to react; When the reaction pressure of the multistage annular-pipe reactor 2011 of the first step and the multistage annular-pipe reactor 2012 in the second stage need to regulate, valve open on pressure regulating tank 209, regulate reacting system pressure, a little material that enters 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 being reacted to while to a certain degree needing extraction material, discharge port 203 is opened, and one material of extraction enters in discharging surge tank 205, then reclaims catalyzer work.Through laboratory test, reaction of high order system operation more than this two-stage is more steadily easier, quiet run for a long time.The control of single-stage annular-pipe reactor difficulty relatively, may occur the big ups and downs of 2-5 secondary response every day, and multistage annular-pipe reactor can reach continuous one week and not occur large fluctuation comparatively speaking.。
The schematic diagram of the another kind of catalyst reaction circulation device in a kind of catalyst recirculation system of preparing 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: increased the multistage annular-pipe reactor 2014 of the third stage, increased accordingly a pressure regulating tank 209 and one group of Matter Transfer pump 2063, reaction mass water cooler 2023.
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 all arranged between the outlet and entrance of this grade of annular-pipe reactor in turn; Between the multistage annular-pipe reactor of every two-stage neighboring, be provided with a pressure regulating tank; Discharge port is only arranged at the exit of the multistage annular-pipe reactor of last step.
In other embodiment, one group of Matter Transfer pump and reaction mass water cooler also can be arranged between the outlet of the multistage annular-pipe reactor of one-level and the entrance of other grade of multistage annular-pipe reactor; Discharge port 203 also can be arranged between the outlet and corresponding reaction mass water cooler of the multistage annular-pipe reactor of every one-level; The number of multistage annular-pipe reactor also can change, as three grades, Pyatyi, ten grades or more multistage number.If small, preferably two-stage is to Pyatyi.
Utilize catalyst recirculation system that the application provides to carry out the method for catalyst recirculation 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; The entrance of described catalyst charge groove and described reactor is connected; Described reaction mass water cooler is arranged between the outlet and entrance of described reactor, to recycle stock, carries out cooling; Part recycle stock, by being arranged on the outlet of described reactor and the discharge port on the pipeline between described reaction mass water cooler, enters catalyst recovery devices; The catalyzer reclaiming 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 that reclaims catalyzer in described catalyst recovery devices is roughly as follows: reaction was carried out after for some time, come the partial material of autoreactor through discharge hole for discharge, this strand of material enters flash drum and carries out flash distillation, light constituent is exported through flash drum top, the heavy constituent that contains catalyzer, through the output of the bottom of flash drum, enters extraction tower under the effect of material-handling pump; Under the effect of extraction agent, complete after extraction process, from discharging at the bottom of the tower of extraction tower, enter thickener, under heating condition, carry out after concentrating and separating, by the output of thickener bottom, then directly or indirectly getting back to reactor and continuing catalyzed reaction.
Utilize the application's device and method, more than 95% the catalyzer of (approximately 95%-99.8%, for example 96%, 98%, 99.5%) can recycle and reuse.
Use the method, can form two circulations of catalyzer.First circulation is reaction partial circulating, catalyzer reacts after for some time in reactor, with reaction raw materials extraction simultaneously, enter in reaction mass water cooler and remove heat, then get back in reactor and continue reaction, do not increasing under the prerequisite of reactor, lengthened the flow process of reaction, also can reduce the severe degree of reaction, effectively control the carrying out of reaction simultaneously; Second circulation reclaimed systemic circulation for reaction, and catalyzer after extraction, carries out separation through flash tank, extraction tower, thickener concentrated, by most of catalyst recovery utilization from reactor.
The preferred embodiment that the foregoing is only the application, is not limited to the application, and for a person skilled in the art, the application can have various modifications and variations.All within the application's spirit and principle, any modification of doing, be equal to replacement, improvement etc., within all should being included in the application's protection domain.
Claims (11)
1. a catalyst recirculation system of preparing polymethoxy dimethyl ether, 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; The entrance of described catalyst charge groove and described reactor is connected; Described reaction mass water cooler is arranged between the outlet and entrance of described reactor, with refrigeration cycle material; On pipeline between the outlet of described reactor and described reaction mass water cooler, be provided with a discharge port, described discharge port is connected with described catalyst recovery devices; The recovery catalyst outlet of described catalyst recovery devices with reclaim catalyst inlet and be connected, described recovery catalyst inlet is arranged on the pipeline before the entrance of described reactor.
2. catalyst recirculation system according to claim 1, is characterized in that, 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, between described thickener and described recovery catalyst inlet, be provided with and reclaim catalyst transport pump.
3. catalyst recirculation system according to claim 2, is characterized in that, 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.
4. catalyst recirculation system according to claim 2, is characterized in that, the top of described thickener is provided with and the tank connected pressure regulating valve of nitrogen and the mouth of pipe being connected with vacuum pump; On the pipeline being connected with the described outlet at bottom of described thickener, be sequentially set with a valve and an intermediate storage tank, and be also provided with one with the outlet branch of purging valve between described outlet at bottom and described valve.
5. catalyst recirculation system according to claim 1, is characterized in that, described reactor is annular-pipe reactor, and preferably, described annular-pipe reactor is multistage annular-pipe reactor, and annular-pipe reactors at different levels all connect in turn; More preferably, annular-pipe reactors at different levels are provided with one or more entrances 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.
6. catalyst recirculation system according to claim 5, is characterized in that, described annular-pipe reactor arranged outside at different levels have temperature control chuck, and described temperature control chuck internal recycle has the medium that can carry out heat exchange; Described in upper level, described in the outlet of multistage annular-pipe reactor and next stage, between the entrance of multistage annular-pipe reactor, pressure regulating tank is set; A Matter Transfer pump and a described reaction mass water cooler are set between the entrance of the outlet of described multistage annular-pipe reactors at different levels and an entrance separately or other grade of described multistage annular-pipe reactor in turn.
7. catalyst recirculation system according to claim 6, it is characterized in that, described discharge port can be arranged on described in each between the outlet of multistage annular-pipe reactor and the entrance of corresponding described reaction mass water cooler or only be arranged on described in last step between the outlet of multistage annular-pipe reactor and the entrance of corresponding described reaction mass water cooler; Described in every one-level, between Matter Transfer pump and described reaction mass water cooler or only between Matter Transfer pump and described reaction mass water cooler, be provided with spent catalyst discharge port described in last step, described spent catalyst discharge port is connected with spent catalyst storage tank.
8. catalyst recirculation system according to claim 2, is characterized in that, 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; In described chuck, pass into hot water, hot steam or heat conduction wet goods heat-transfer medium; Described catalyst recirculation system also comprises discharging dashpot, and described discharging dashpot is arranged between described discharge port and described flash drum.
9. catalyst recirculation system according to claim 8, is characterized in that, between described catalyst charge groove and described static mixer, is provided with catalyst transport pump; 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 being connected with described feed back outlet.
10. catalyst recirculation system according to claim 8, 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.
The method of catalyst recirculation is carried out in 11. 1 kinds of utilizations according to the catalyst recirculation system described in claim 1-8, 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; The entrance of described catalyst charge groove and described reactor is connected; Described reaction mass water cooler is arranged between the outlet and entrance of described reactor, to recycle stock, carries out cooling; Part recycle stock, by being arranged on the outlet of described reactor and the discharge port on the pipeline between described reaction mass water cooler, entering catalyst recovery devices and connects; The catalyzer reclaiming 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 that reclaims catalyzer in described catalyst recovery devices is as follows: reaction was carried out after for some time, come the partial material of autoreactor through discharge hole for discharge, this strand of material enters flash drum and carries out flash distillation, light constituent is exported through flash drum top, the heavy constituent that contains catalyzer, through the output of the bottom of flash drum, enters extraction tower under the effect of material-handling pump; Under the effect of extraction agent, complete after extraction process, from discharging at the bottom of the tower of extraction tower, enter thickener, under heating condition, carry out after concentrating and separating, by the output of thickener bottom, then directly or indirectly getting back to reactor and continuing catalyzed reaction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105694021A (en) * | 2016-03-30 | 2016-06-22 | 吉林欧科自动化设备有限公司 | Double-mode alkoxylation technique |
| CN110563753A (en) * | 2019-08-05 | 2019-12-13 | 潜江宜生新材料有限公司 | Photochlorination system of methyl trichlorosilane |
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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 |
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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 |
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| CN105694021A (en) * | 2016-03-30 | 2016-06-22 | 吉林欧科自动化设备有限公司 | Double-mode alkoxylation technique |
| CN110563753A (en) * | 2019-08-05 | 2019-12-13 | 潜江宜生新材料有限公司 | Photochlorination system of methyl trichlorosilane |
| CN110563753B (en) * | 2019-08-05 | 2022-04-26 | 潜江宜生新材料有限公司 | Photochlorination system of methyl trichlorosilane |
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| CN104177235B (en) | 2015-11-18 |
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