CN108889261B - Device for preparing Grignard reagent and control method - Google Patents
Device for preparing Grignard reagent and control method Download PDFInfo
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- CN108889261B CN108889261B CN201810909581.9A CN201810909581A CN108889261B CN 108889261 B CN108889261 B CN 108889261B CN 201810909581 A CN201810909581 A CN 201810909581A CN 108889261 B CN108889261 B CN 108889261B
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- 150000004795 grignard reagents Chemical class 0.000 title claims abstract description 24
- 239000007818 Grignard reagent Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 98
- 238000012544 monitoring process Methods 0.000 claims abstract description 32
- 238000003860 storage Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims description 33
- 239000000498 cooling water Substances 0.000 claims description 22
- 150000008282 halocarbons Chemical class 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 19
- 150000005826 halohydrocarbons Chemical class 0.000 claims description 15
- 230000002572 peristaltic effect Effects 0.000 claims description 4
- 238000004891 communication Methods 0.000 abstract description 6
- 238000003747 Grignard reaction Methods 0.000 abstract description 5
- 239000007810 chemical reaction solvent Substances 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 238000011010 flushing procedure Methods 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- QARVLSVVCXYDNA-UHFFFAOYSA-N bromobenzene Chemical compound BrC1=CC=CC=C1 QARVLSVVCXYDNA-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 description 1
- JNTPTNNCGDAGEJ-UHFFFAOYSA-N 6-chlorohexan-1-ol Chemical compound OCCCCCCCl JNTPTNNCGDAGEJ-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 125000002734 organomagnesium group Chemical group 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/02—Magnesium compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00103—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor in a heat exchanger separate from the reactor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to the field of Grignard reaction control, in particular to a device for preparing a Grignard reagent and a control method. The device for preparing the Grignard reagent comprises: the device comprises a storage container, a dripping rate controller, a reaction container, a condenser, a signal monitoring module, a receiving container, a first pipeline, a second pipeline and a connecting pipeline; the material storage container and the dripping rate controller are communicated through the first pipeline, the first pipeline is communicated with the second pipeline, and the reaction container is communicated with the upper end of the condenser through the second pipeline; the lower end of the condenser is communicated with the reaction vessel through the connecting pipeline, and a signal monitoring module is arranged on the connecting pipeline; the receiving vessel is located downstream of and in communication with the reaction vessel, and the receiving vessel is located downstream of and in communication with the condenser.
Description
Technical Field
The invention relates to the field of Grignard reaction control, in particular to a device for preparing a Grignard reagent and a control method.
Background
The grignard reaction is one of the most widely used reactions in organic chemistry, which is a reaction for preparing alcohol by reacting a grignard reagent (organomagnesium reagent) with ketone and aldehyde and then hydrolyzing, wherein the most important link in the reaction process is the preparation of the grignard reagent. The preparation of the Grignard reagent is a strong exothermic reaction, the Grignard reagent is extremely active, can react with water, oxygen and carbon dioxide and release heat, and is extremely easy to cause overpressure explosion venting once the conditions are out of control, so that dangerous accidents such as fire and explosion occur.
In chemical production, the main difficulty in preparing grignard reagents is that the temperature and reflux rate during the reaction cannot be monitored, and the optimal drop rate should be to keep the reaction in a slightly refluxed state. If the temperature is higher, the coupling reaction is easy to generate byproducts; too low a temperature, the reaction time becomes long and the reaction is not complete. On the other hand, if the dropping speed is too high, the reaction temperature can be rapidly increased, and the temperature difference between the solution and the whole reaction equipment can be generated; meanwhile, the solvent backflow phenomenon is obvious, the reaction is easy to run away, the instrument is overpressurized, and the safety problem occurs.
In the prior art, the production process is judged according to human experience.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a device for preparing a Grignard reagent and a control method.
According to an aspect of the present invention, there is provided an apparatus for preparing a grignard reagent, comprising:
The device comprises a storage container, a dripping rate controller, a reaction container, a condenser, a signal monitoring module, a receiving container, a first pipeline, a second pipeline and a connecting pipeline;
The material storage container and the dripping rate controller are communicated through the first pipeline, the first pipeline is communicated with the second pipeline, and the reaction container is communicated with the upper end of the condenser through the second pipeline; the lower end of the condenser is communicated with the reaction vessel through the connecting pipeline, and a signal monitoring module is arranged on the connecting pipeline; the receiving vessel is located downstream of and in communication with the reaction vessel, and the receiving vessel is located downstream of and in communication with the condenser.
According to one embodiment of the invention, the device for preparing grignard reagent further comprises a flushing buffer container connected with the condenser through a connecting pipeline and used for receiving the organic solvent from the condenser when the pressure of the organic solvent in the condenser exceeds a set value.
Under the condition of reaction out of control, the generated heat can not be cooled down in time, materials in the reaction system are boiled and flushed out of the reaction kettle, and the materials are flushed out of a pipeline connected with the flushing buffer container from the condenser, so that the safety of the reaction system can be ensured, and the loss of reaction materials can be reduced by arranging the flushing buffer container.
According to one embodiment of the invention, the signal monitoring module includes a temperature sensor and a flow meter. According to one embodiment of the invention, the signal monitoring module may further comprise a pressure sensor.
According to one embodiment of the invention, a liquid level meter can be arranged in the reaction container and the receiving container for immediately monitoring the liquid level change of the reaction and the intensity of the reaction.
According to one embodiment of the invention, the device for preparing the grignard reagent can further comprise a signal alarm to play a role of automatic early warning.
According to one embodiment of the invention, the dripping rate controller is selected from any one of a proportional valve, a peristaltic pump and a diaphragm pump.
According to one embodiment of the invention, the device further comprises one or both of a cooling assembly and a pressure relief assembly; the cooling assembly is used for reducing the reaction temperature and comprises a first cooling water pipeline arranged at the upper end of the reaction container, a cooling water outlet valve positioned on the first cooling water pipeline, a second cooling water pipeline arranged at the lower end of the reaction container and a cooling water inlet valve positioned on the second cooling water pipeline; the pressure relief assembly is used for reducing the pressure in the reaction device and comprises a pressure relief valve arranged at the lower end of the signal monitoring module.
According to one embodiment of the invention, the connecting pipeline comprises a third pipeline and a fourth pipeline, the third pipeline is provided with the temperature sensor and the first valve, the fourth pipeline is connected in parallel with two ends of the third pipeline, which are positioned at the first valve, and the fourth pipeline is provided with the flowmeter and the second valve.
According to another aspect of the present invention, there is provided a control method for preparing a grignard reagent, comprising the steps of:
S101: the temperature of the condensate and the flow rate of the condensate reflux are monitored,
S102: the dripping speed of the halohydrocarbon is adjusted according to the flow of the condensed reflux,
S103: depending on the temperature of the condensate, it is decided whether to perform the following three operations: 1) stopping dripping halogenated hydrocarbon, 2) cooling the reaction, and 3) decompressing the reaction.
According to one embodiment of the invention, the control method is performed with the device according to the invention, comprising the following steps:
S104: monitoring the temperature of condensate and the flow of condensate reflux by using a signal monitoring module;
S105: when the flow of the condensed reflux reaches a first preset value, the dripping speed of the halohydrocarbon is slowed down by a dripping speed controller; when the flow rate of the condensed reflux is lower than a first preset value, the dripping rate of the halohydrocarbon is accelerated by a dripping rate controller;
S106: when the temperature reaches a second preset value, the following operations are performed: a) Stopping dripping halogenated hydrocarbon; b) Cooling the reaction by using a cooling assembly; c) And carrying out pressure relief treatment on the reaction by utilizing a pressure relief assembly.
According to one embodiment of the invention, the second valve is always in an open state during the reaction, and when the flow rate of the condensed reflux reaches a third preset value, the first valve is opened to ensure that the condensed reaction solvent can still flow back into the reaction vessel rapidly under the condition of overlarge flow rate.
According to one embodiment of the invention, the second preset value is 10-15 ℃.
According to one embodiment of the invention, the signal monitoring module includes a temperature sensor and a flow meter. According to one embodiment of the invention, the signal monitoring module may further comprise a pressure sensor.
The invention has the following beneficial effects: when the device and the method are used for preparing the Grignard reagent, the signal monitoring module is used for monitoring the flow and the temperature on line in real time, and the operations such as dripping of the halogenated hydrocarbon, cooling and pressure relief treatment on the reaction are controlled according to the flow and the temperature, so that the reaction can be efficiently carried out under stable conditions, potential safety risks are avoided, and the purposes of automation and humanization of the Grignard reagent production are achieved.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a Grignard reagent according to the invention.
The device comprises a 101-storage container, a 102-dripping rate controller, a 103-reaction container, a 104-condenser, a 105-temperature sensor, a 106-flowmeter, a 107-first valve, a 108-second valve, a 109-receiving container, a 201-first pipeline, a 202-second pipeline, a 203-connecting pipeline, a 204-third pipeline, a 205-fourth pipeline, a 401-first cooling water pipeline, a 402-cooling water outlet valve, a 403-second cooling water pipeline, a 404-cooling water inlet valve and a 405-pressure relief valve.
Detailed Description
The present invention is described in detail in the following description, which is not to be construed as limiting the invention.
In the present invention, the storage container may be, for example, a head tank or the like for storing halogenated hydrocarbon; the dripping rate controller is selected from any one of adjustable equipment such as a proportional valve, a peristaltic pump, a diaphragm pump and the like, and the dripping rate is adjusted by rotating the size of the valve; the reaction vessel may be, for example, a reaction vessel or the like; the receiving container may be, for example, a receiving tank or the like.
In the present invention, the raw Mg is a solid and is added to the reaction vessel in its entirety before the reaction proceeds (for example, from a feed port located in the reaction vessel). The halide is stored in the storage vessel and the rate of its drop into the reaction vessel is controlled by a drop rate controller.
As shown in fig. 1, the apparatus for preparing a grignard reagent according to the present invention includes:
A storage vessel 101, a dropping rate controller 102, a reaction vessel 103, a condenser 104, a signal monitoring module, a receiving vessel 109, a first line 201, a second line 202, and a connecting line 203;
the material storage container 101 and the dripping rate controller 102 are communicated through the first pipeline 201, the first pipeline 201 is communicated with the second pipeline 202, and the reaction container 103 is communicated with the upper end of the condenser 104 through the second pipeline 202; the lower end of the condenser 104 is communicated with the reaction vessel 103 through the connecting pipeline 203, and a signal monitoring module is arranged on the connecting pipeline 203; the receiving vessel 109 is located downstream of the reaction vessel 103 and is in communication with the reaction vessel 103, and the receiving vessel 109 is located downstream of the condenser 104 and is in communication with the condenser 104.
According to one embodiment of the present invention, the apparatus for preparing a grignard reagent further comprises a flushing buffer vessel (not shown) connected to the condenser 104 through a connection line for receiving the organic solvent from the condenser 104 when the pressure of the organic solvent in the condenser 104 exceeds a set value.
Under the condition of reaction out of control, the generated heat can not be cooled down in time, materials in the reaction system are boiled and flushed out of the reaction kettle, and the materials are flushed out of a pipeline connected with the flushing buffer container from the condenser, so that the safety of the reaction system can be ensured, and the loss of reaction materials can be reduced by arranging the flushing buffer container.
The signal monitoring module includes a temperature sensor 105 and a flow meter 106. According to one embodiment of the invention, the signal monitoring module may further comprise a pressure sensor.
According to one embodiment of the invention, a liquid level meter can be arranged in the reaction container and the receiving container for immediately monitoring the liquid level change of the reaction and the intensity of the reaction.
According to one embodiment of the invention, the device for preparing the grignard reagent can further comprise a signal alarm to play a role of automatic early warning.
The drip rate controller 102 in fig. 1 may be any of a proportional valve, a peristaltic pump, and a diaphragm pump.
The apparatus of fig. 1 further includes a cooling assembly and a pressure relief assembly; the cooling assembly is used for reducing the reaction temperature and comprises a first cooling water pipeline 401 arranged at the upper end of the reaction vessel 103, a cooling water outlet valve 402 arranged on the first cooling water pipeline 401, a second cooling water pipeline 403 arranged at the lower end of the reaction vessel 103 and a cooling water inlet valve 404 arranged on the second cooling water pipeline 403; the pressure relief assembly is used for reducing the pressure in the reaction device and comprises a pressure relief valve 405 arranged at the lower end of the signal monitoring module.
The connecting pipeline 203 comprises a third pipeline 204 and a fourth pipeline 205, the third pipeline 204 is provided with a temperature sensor 105 and a first valve 107, the fourth pipeline 205 is connected in parallel with two ends of the third pipeline 204, which are positioned on the first valve 107, and the fourth pipeline 205 is provided with a flowmeter 106 and a second valve 108.
According to another aspect of the present invention, there is provided a control method for preparing a grignard reagent, comprising the steps of:
S101: the temperature of the condensate and the flow rate of the condensate reflux are monitored,
S102: the dripping speed of the halohydrocarbon is adjusted according to the flow of the condensed reflux,
S103: depending on the temperature of the condensate, it is decided whether to perform the following three operations: 1) stopping dripping halogenated hydrocarbon, 2) cooling the reaction, and 3) decompressing the reaction.
In the invention, the dripping rate of the halohydrocarbon is regulated according to the flow of the condensed reflux so as to ensure that the reaction is smoothly carried out within a set temperature range; and monitoring the reflux temperature of the reaction solvent, stopping dripping halogenated hydrocarbon when the reaction temperature is too high, and cooling and decompressing the reaction to prevent the safety risks of excessive temperature and overpressure caused by too high speed of adding the halogenated hydrocarbon.
In the invention, the dripping control mode of the halohydrocarbon is rough-fine control and can be divided into two stages:
the first stage: slowly increasing the condensing reflux flow rate by slowly adjusting the speed of dropwise adding halogenated hydrocarbon;
and a second stage: after reaching the fine control range, the fine dropwise adding of the halohydrocarbon is started, so that safety accidents caused by too fast dropwise adding or large fluctuation are avoided. Specifically, the method can be realized by the following three steps:
The first step:
firstly, a unitary linear regression equation of the halogenated hydrocarbon dropping rate and the condensation reflux flow rate is established through a pre-experiment, and a linear relation of the halogenated hydrocarbon dropping rate and the condensation reflux flow rate is established through a series of data.
And a second step of:
According to the linear relation between the two, the condensing reflux flow rate is slowly increased, and a certain time (for example, within 10 minutes) is increased to a preset value of refinement control; the drop rate of the halocarbon is adjusted by adjusting the value of the condensate reflux flow rate variable.
And a third step of:
After the condensation reflux flow rate reaches the refinement control range, starting refinement adjustment; and automatically adjusting the dripping rate of the halogenated hydrocarbon according to the flow rate.
And the first two steps of fuzzification control the condensation reflux flow rate, and after the condensation reflux flow rate preliminarily reaches a preset value of refinement control, the refinement control is started. The condensate reflux flow speed is stable, and the fluctuation is reduced as much as possible.
When the real-time flow rate of the condensation reflux is larger than a first preset value, reducing the dripping speed of the halohydrocarbon by one unit; and when the real-time flow rate of the condensed reflux is smaller than a first preset value, increasing the dropping speed of the halohydrocarbon by one unit. A unit herein may be, for example, 0.1ml/min or the like.
In one embodiment of the present invention, the preset value of the refinement control is generally set to be lower than the first preset value described herein. For example, the first preset value is 200ml/s, and the preset value for refinement control is set to 150ml/s. In the case of rough control, the program adjustment period is, for example, 20 s/time; in the case of the refinement control, the program adjustment period is, for example, 5 s/time.
According to one embodiment of the invention, the control method is performed with the device according to the invention, comprising the following steps:
S104: monitoring the temperature of condensate and the flow of condensate reflux by using a signal monitoring module;
S105: when the flow of the condensed reflux reaches a first preset value, the dripping speed of the halohydrocarbon is slowed down by a dripping speed controller; when the flow rate of the condensed reflux is lower than a first preset value, the dripping rate of the halohydrocarbon is accelerated by a dripping rate controller;
S106: when the temperature reaches a second preset value, the following operations are performed: a) Stopping dripping halogenated hydrocarbon; b) Cooling the reaction by using a cooling assembly; c) And carrying out pressure relief treatment on the reaction by utilizing a pressure relief assembly.
Monitoring the temperature and the flow rate, and when the flow rate reaches a first preset value, slowing down the dripping rate of the halogenated hydrocarbon to control the intensity of the reaction; when the temperature reaches a second preset value, the gas of the reaction solvent cannot be cooled sufficiently in time, and the reaction is partially out of control, at the moment, the reaction degree cannot be controlled effectively by only slowing down the dripping speed of the halogenated hydrocarbon, and three operations of a) stopping dripping the halogenated hydrocarbon, b) cooling the reaction by using a cooling component and c) decompressing the reaction by using a decompression component are needed to ensure that the reaction can be carried out safely. In the present invention, when the flow rate has reached the first preset value, the temperature has not reached the second preset value, but is lower than the second preset value.
The dripping rate of the halohydrocarbon is controlled by the dripping rate controller, so that the intensity of the reaction can be controlled, and meanwhile, the continuous addition of raw materials is ensured, and the smooth progress of the reaction is ensured.
In the present invention, the setting of the first preset value is affected by the volume of the reaction vessel, the kind and amount of the reaction solvent, the amount of the reaction raw material Mg, the kind and amount of the halogenated hydrocarbon, and the like, and thus the first preset value is not fixed for different reaction cases.
The solvent used in the Grignard reaction may be tetrahydrofuran, and the halogenated hydrocarbon may be bromobenzene, 1-chlorobutane, 6-chloro-1-hexanol, or the like.
In one embodiment, the halogenated hydrocarbon is bromobenzene using tetrahydrofuran as the reaction solvent, and the flow rate is set to, for example, 200 ml/min when the Grignard reaction is performed in a 100L reaction vessel.
According to one embodiment of the invention, the second valve is always in an open state during the reaction, and when the flow rate of the condensed reflux reaches a third preset value, the first valve is opened to ensure that the condensed reaction solvent can still flow back into the reaction vessel rapidly under the condition of overlarge flow rate.
In the invention, the third preset value and the first preset value are both values related to the flow, and the third preset value corresponds to the maximum flow value which can be born by the reaction system when the first valve is not opened. Typically, the first preset value is less than the third preset value, e.g., the first preset value is 70% -85%, e.g., 70%, 72%, 75%, 77%, 78%, 80%, 82%, 85%, etc., of the third preset value.
According to one embodiment of the invention, the second preset value is 10-15 ℃. According to one embodiment of the invention, the second preset value is, for example, 10 ℃, 10.5 ℃, 11 ℃, 12 ℃, 13 ℃, 14 ℃, 15 ℃, etc.
According to one embodiment of the invention, the signal monitoring module includes a temperature sensor and a flow meter. According to one embodiment of the invention, the signal monitoring module may further comprise a pressure sensor.
In the present invention, a temperature sensor is used to monitor the temperature of condensate, a flow meter is used to monitor the flow rate of condensate reflux, and a pressure sensor is used to monitor the pressure in, for example, a reaction vessel, a condenser, a receiving vessel, etc.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. An apparatus for preparing a grignard reagent, characterized in that: the device comprises a storage container, a dripping rate controller, a reaction container, a condenser, a signal monitoring module, a receiving container, a first pipeline, a second pipeline, a connecting pipeline, a cooling assembly and a pressure relief assembly;
The material storage container and the dripping rate controller are communicated through the first pipeline, the first pipeline is communicated with the second pipeline, and the reaction container is communicated with the upper end of the condenser through the second pipeline; the lower end of the condenser is communicated with the reaction vessel through the connecting pipeline, and a signal monitoring module is arranged on the connecting pipeline; the receiving container is positioned downstream of the reaction container and is communicated with the reaction container, and the receiving container is positioned downstream of the condenser and is communicated with the condenser; the signal monitoring module is used for monitoring the temperature of condensate and the flow of condensate reflux; when the flow rate of the condensed reflux reaches a first preset value, the dripping rate controller is used for controlling the dripping rate of the slow-down halohydrocarbon, and when the flow rate of the condensed reflux is lower than the first preset value, the dripping rate controller is used for controlling the dripping rate of the fast-up halohydrocarbon; when the temperature reaches a second preset value, the dripping speed controller is used for controlling stopping dripping halogenated hydrocarbon; when the temperature reaches a second preset value, the cooling component is used for cooling the reaction, and the pressure relief component is used for relieving the pressure of the reaction; when the flow reaches the first preset value, the temperature does not reach the second preset value yet, but is lower than the second preset value.
2. The apparatus according to claim 1, wherein: the signal monitoring module comprises a temperature sensor and a flowmeter.
3. The apparatus according to claim 1, wherein: the dripping rate controller is selected from any one of a proportional valve, a peristaltic pump and a diaphragm pump.
4. The apparatus according to claim 1, wherein:
The cooling assembly comprises a first cooling water pipeline arranged at the upper end of the reaction container, a cooling water outlet valve positioned on the first cooling water pipeline, a second cooling water pipeline arranged at the lower end of the reaction container and a cooling water inlet valve positioned on the second cooling water pipeline; the pressure relief assembly comprises a pressure relief valve arranged at the lower end of the signal monitoring module.
5. The device of claim 2, wherein the connecting pipeline comprises a third pipeline and a fourth pipeline, the third pipeline is provided with the temperature sensor and the first valve, the fourth pipeline is connected in parallel with two ends of the third pipeline, which are positioned at the first valve, and the fourth pipeline is provided with the flowmeter and the second valve.
6. A control method of an apparatus for preparing a Grignard reagent according to claim 5, wherein the method comprises the steps of:
S101: the temperature of the condensate and the flow rate of the condensate reflux are monitored,
S102: the dripping speed of the halohydrocarbon is adjusted according to the flow of the condensed reflux,
S103: depending on the temperature of the condensate, it is decided whether to perform the following three operations:
1) Stopping dripping halogenated hydrocarbon;
2) Cooling the reaction;
3) The reaction was depressurized.
7. The control method according to claim 6, wherein the second valve is always in an open state during the reaction, and the first valve is opened when the flow rate of the condensed reflux reaches a third preset value; the third preset value corresponds to a maximum flow value which can be born by the reaction system when the first valve is not opened, and the first preset value is smaller than the third preset value.
8. The control method according to claim 6, wherein the second preset value is 10-15 ℃.
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