Integrated high-safety mechanical-stirring-free Grignard reagent preparation device

Abstract

The utility model discloses an integrated high-safety non-mechanical stirring Grignard reagent preparation device which comprises a material feeding module, a Grignard reagent non-stirring preparation module and a Grignard reagent using module, aiming at the characteristics of a Grignard reagent preparation solid-liquid reaction, a tower type fixed bed reactor is used for replacing a traditional kettle type reactor, and the Grignard reagent using module is used for preparing the Grignard reagent. The problem that the service life of equipment is influenced by collision between stirring of the tank reactor and solid magnesium is solved; by arranging the detachable preloaded solid magnesium filler layer, the safety problem of solid magnesium feeding in a class A workshop is solved; a plurality of reactors are connected in parallel, and the whole feeding and discharging rate is not influenced by single disassembly and assembly, so that the continuity of the whole fine chemical reaction process is realized; through reasonable integration of the tower type fixed bed reactor, the circulating cooler and the circulating pump, integration of the Grignard reagent stirring-free preparation module and modularization of the device are realized, the occupied area is reduced, and the operation process is solidified.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the fine chemical safety technical field, concretely relates to an integrated high safety no mechanical stirring Grignard reagent preparation device. BACKGROUND

[0002] Grignard reagent is the organic magnesium compound that halogenated hydrocarbon is reacted with magnesium in anhydrous ether or tetrahydrofuran. At present, there are still some problems in the preparation process of Grignard reagent:

[0003] 1) The dosage and surface area of magnesium directly affect the reactivity, and if it cannot be effectively initiated, a large amount of unreacted material will accumulate, causing the material in the kettle to suddenly react to form high temperature and high pressure and explode under the condition of local overheating;

[0004] 2) Magnesium is one of the raw materials, and the dosage is large, and the hardness cannot be ignored. At present, the kettle type reactor is usually used for preparation, and the collision and friction of magnesium and stirring paddle are serious, which greatly reduces the service life of the stirring paddle;

[0005] 3) The process of preparing Grignard reagent is a strong exothermic reaction process. In the intermittent kettle type reactor, the preparation is not only low in efficiency, but also the consequences are often serious if the material is not careful and out of control due to large amount of material;

[0006] 4) The integration of the device for preparing Grignard reagent is low, and the floor area is large. UTILITY MODEL CONTENT

[0007] In view of the above problems, the purpose of the utility model is to provide an integrated high safety no mechanical stirring Grignard reagent preparation device.

[0008] The specific technical scheme is as follows:

[0009] An integrated high safety no mechanical stirring Grignard reagent preparation device, which comprises a material feeding module, a Grignard reagent non-stirring preparation module and a Grignard reagent use module. The Grignard reagent non-stirring preparation module comprises a plurality of parallel tower type fixed bed reaction systems, each tower type fixed bed reaction system comprises a tower type fixed bed reactor, a circulating cooler and a circulating pump, the top outlet pipeline of the tower type fixed bed reactor is connected with the circulating cooler, the bottom outlet pipeline of the circulating cooler is divided into two pipelines, one pipeline is connected with the bottom of the tower type fixed bed reactor through the circulating pump, and the other pipeline is connected with the Grignard reagent use module. The material feeding module is connected with the bottom of the tower type fixed bed reactor through the circulating pump. The upper part and the lower part of the tower type fixed bed reactor are respectively provided with detachable flanges, a metal magnesium filler layer is arranged in the middle part of the tower type fixed bed reactor between the detachable flanges, filter screens are arranged at the upper end and the lower end of the metal magnesium filler layer, a discharge filter layer is arranged in the top of the tower type fixed bed reactor, and a feed distributor is arranged in the bottom of the tower type fixed bed reactor and connected with the circulating pump through a pipeline.

[0010] Further, the material feeding module comprises a halogenated hydrocarbon / THF mixed solution feeding tank, a feeding tank liquid supplementing system, an initiator feeding system and a quenching agent feeding system, the feeding tank liquid supplementing system is connected with the halogenated hydrocarbon / THF mixed solution feeding tank, the discharge pipe of the halogenated hydrocarbon / THF mixed solution feeding tank is divided into multiple pipelines, each pipeline is connected with a group of tower type fixed bed reaction systems respectively, the discharge pipe of the initiator feeding system is divided into multiple pipelines, each pipeline is connected with a group of tower type fixed bed reaction systems respectively, and the discharge pipe of the quenching agent feeding system is divided into multiple pipelines, each pipeline is connected with a group of tower type fixed bed reaction systems respectively.

[0011] Further, the Grignard reagent using module comprises two groups of Grignard reagent collecting systems, each group of Grignard reagent collecting system comprises a Grignard reagent feeding control device and a Grignard reagent high tank, the Grignard reagent feeding control device is arranged at the top of the Grignard reagent high tank, the discharge pipes of the multiple groups of tower type fixed bed reaction systems are connected into one pipeline, the one pipeline is divided into two pipelines, and the two pipelines are connected with the Grignard reagent feeding control devices of the two groups of Grignard reagent collecting systems respectively, and the bottom discharge openings of the Grignard reagent high tanks of the two groups of Grignard reagent collecting systems are connected after being connected in series and then connected with a Grignard reaction safety control assembly.

[0012] Further, the Grignard reagent feeding control device comprises a remote liquid level meter arranged on the Grignard reagent high tank and a feeding start switch valve interlocked with the remote liquid level meter, and the Grignard reaction safety control assembly comprises a dropwise adding pneumatic regulating valve and a discharge pneumatic switch valve.

[0013] Further, nitrogen seals and tail gas pipes are arranged on the halogenated hydrocarbon / THF mixed solution feeding tank and the Grignard reagent high tank.

[0014] Further, the multiple groups of tower type fixed bed reaction systems are arranged on movable supports, the movable supports comprise multiple groups of mounting frames, the mounting frames are fixedly connected between the mounting frames, one group of tower type fixed bed reaction systems is arranged on one group of mounting frames, rotatable folding movable legs are arranged at the bottom of each group of mounting frames, limit grooves are arranged on the inner sides of the movable legs, sliding blocks are arranged at the bottom of the mounting frames, one end of the limit groove is an opening, and the other end of the limit groove is a limit structure, the sliding blocks slide from the opening to the limit structure, so that the movable legs are fixedly limited.

[0015] A Grignard reagent preparation process using an integrated high-safety mechanical stirring-free Grignard reagent preparation device, comprising the following steps:

[0016] 1) nitrogen replacement, open the circulating cooler, halogenated hydrocarbon / THF mixture through halogenated hydrocarbon / THF mixture feed tank buffer, halogenated hydrocarbon / THF mixture through circulating pump into the tower fixed bed reactor with magnesium filler layer contact, at the same time through initiator feed system to the tower fixed bed reactor inside the initiator to initiate Grignard reagent preparation reaction, after the reaction begins liquid full tower fixed bed reactor, under the action of circulating pump constantly through the tower fixed bed reactor and magnesium reaction exothermic Grignard reagent, then through the circulating cooler to the safe temperature control;

[0017] 2) the outlet of the circulating cooler detects the concentration of the product, when the product concentration reaches the requirement, the circulating reaction pipeline is closed, the Grignard reagent at the outlet of the tower fixed bed reactor is introduced into the Grignard reagent high tank;

[0018] 3) after the completion of step 2) discharge, switch back to the circulating reaction pipeline, the feed pipeline is switched to the quenching agent feed system to introduce the quenching agent into the tower fixed bed reactor, and the circulating quenching agent is switched to nitrogen after the feed, and the discharge is switched to the blowdown to blow clean the liquid phase material in the tower fixed bed reaction system;

[0019] 4) the magnesium filler layer of the cleaned tower fixed bed reaction system is disassembled by disassembling the detachable flange, and the new filler is replaced;

[0020] 5) the tower fixed bed reaction system with the replaced filler reenters the next reaction cycle, and a plurality of tower fixed bed reaction systems alternately react and replace to ensure the continuous reaction;

[0021] 6) one group of Grignard reagent collecting system Grignard reagent high tank is in the state of dropping discharge, and the other group of Grignard reagent collecting system Grignard reagent high tank is in the state of collecting, when the Grignard reagent high tank in the collecting state reaches the upper limit of the collecting, the Grignard reagent high tank in the dropping state has been dropped, the working state of the Grignard reagent high tank is switched by the Grignard reagent feed control device, so that continuous production is realized; the dropping state is that the feed start on-off valve is closed, the dropping pneumatic regulating valve and the discharge pneumatic on-off valve are opened, and the temperature signal of the receiving discharge port is adjusted to adjust the discharge opening degree; the collecting state is that the feed start on-off valve is opened, and the dropping pneumatic regulating valve and the discharge pneumatic on-off valve are closed.

[0022] Further, the coolant of the circulating cooler is a non-aqueous phase coolant selected from heat conducting oil, freon or ethanol.

[0023] The beneficial effects of the utility model lie in:

[0024] 1) The utility model discloses a tower type fixed bed reactor instead of traditional kettle type reactor according to the characteristics of solid-liquid reaction of Grignard reagent preparation, and solid-liquid contact efficiency is no longer ensured by stirring paddle, but solid-liquid phase is fully contacted by circulating pump and feed distributor, so that the problem of equipment life influenced by stirring and solid magnesium collision of kettle type reactor is solved.

[0025] 2) The utility model discloses that the hidden danger of burning and explosion of magnesium when contacting air and water or moisture is solved by setting detachable preloaded solid magnesium filler layer, and the dangerous magnesium filling process is transferred to outside the production workshop, so that secondary disaster caused by magnesium burning and explosion of type A and B medium in the workshop is avoided, the possibility of magnesium filling process accident in the workshop is eliminated, the possibility of magnesium filling process accident during Grignard reagent preparation is solved, and the safety problem of magnesium filling during Grignard reagent preparation is solved.

[0026] 3) The utility model discloses that a plurality of tower type fixed bed reaction systems are connected in parallel according to the problems existing in the preparation of Grignard reagent by kettle type process, and the whole feeding and discharging rate is not influenced by single disassembly and assembly, so that the continuousness of the whole process of fine chemical reaction is realized, the liquid holding capacity of the whole device is greatly reduced due to continuous production, the heat exchange effect is increased, and the severity of accident consequences is reduced.

[0027] 4) The utility model discloses that the tower type fixed reactor, circulating cooler and circulating pump are reasonably integrated into the tower type fixed bed reaction system and packaged in the frame, so that the integration of Grignard reagent non-stirring preparation module and the modularization of the device are realized, and the land occupation of the device is reduced. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1 It is the flowchart of the utility model;

[0029] Figure 2 It is the structure diagram of the tower type fixed bed reaction system;

[0030] Figure 3 It is the overhead view diagram of the material feeding module and Grignard reagent non-stirring preparation module after installation of the utility model;

[0031] Figure 4 It is the side view of the movable support;

[0032] Figure 5 It is the working mode diagram of the movable support leg;

[0033] Figure 6 It is the side view of the movable support leg.

[0034] In the figure: 1, tower type fixed bed reaction system; 11, tower type fixed bed reactor; 111, detachable flange; 112, magnesium metal filler layer; 113, filter screen; 114, discharge filter layer; 115, feed distributor; 12, circulating cooler; 13, circulating pump; 2, halogenated hydrocarbon / THF mixed solution feed tank; 3, feed tank liquid supplement system; 4, initiator feed system; 5, quenching agent feed system; 6, Grignard reagent collection system; 61, Grignard reagent feed control device; 62, Grignard reagent high tank; 7, Grignard reaction safety control assembly; 8, movable support; 81, mounting frame; 811, movable leg; 8111, limiting groove; 8112, sliding block. DETAILED DESCRIPTION

[0035] The utility model will be further explained below in combination with the drawings and examples of the specification, but the protection scope of the utility model is not limited to this.

[0036] As shown in Figure 1 and Figure 2 , an integrated high-safety mechanical-stirring-free Grignard reagent preparation device comprises a material feed module (A) in Figure 1 , a mechanical-stirring-free Grignard reagent preparation module (B) in Figure 1 , and a Grignard reagent use module (C) in Figure 1The C in the above formula is prepared by the no-stirring Grignard reagent preparation module, which comprises multiple groups of parallel tower fixed bed reaction systems 1, each group of tower fixed bed reaction systems 1 comprising a tower fixed bed reactor 11, a circulating cooler 12 and a circulating pump 13, the top outlet pipeline of the tower fixed bed reactor 11 being connected with the circulating cooler 12, the bottom outlet pipeline of the circulating cooler 12 being divided into two pipelines, one pipeline being connected with the bottom of the tower fixed bed reactor 11 through the circulating pump 13, and the other pipeline being connected with the Grignard reagent use module, the material feeding module being connected with the bottom of the tower fixed bed reactor 11 through the circulating pump 13, the upper part and the lower part of the tower fixed bed reactor 11 being respectively provided with detachable flanges 111, a metal magnesium filler layer 112 being arranged in the middle part of the tower fixed bed reactor 11 between the detachable flanges 111, the upper end and the lower end of the metal magnesium filler layer 112 being respectively provided with filter screens 113, a discharge filter layer 114 being arranged in the top of the tower fixed bed reactor 11, and a feed distributor 115 being arranged in the bottom of the tower fixed bed reactor 11 and connected with the circulating pump 13 through a pipeline, the material feeding module comprising a halogenated hydrocarbon / THF mixed liquid feeding tank 2, a feeding tank liquid supplementing system 3, an initiator feeding system 4 and a quenching agent feeding system 5, the feeding tank liquid supplementing system 3 being connected with the halogenated hydrocarbon / THF mixed liquid feeding tank 2, the discharge pipeline of the halogenated hydrocarbon / THF mixed liquid feeding tank 2 being divided into multiple pipelines, each pipeline being connected with one group of tower fixed bed reaction systems 1, the discharge pipeline of the initiator feeding system 4 being divided into multiple pipelines, each pipeline being connected with one group of tower fixed bed reaction systems 1, the discharge pipeline of the quenching agent feeding system 5 being divided into multiple pipelines, each pipeline being connected with one group of tower fixed bed reaction systems 1, the Grignard reagent use module comprising two groups of Grignard reagent collecting systems 6, each group of Grignard reagent collecting systems 6 comprising a Grignard reagent feeding control device 61 and a Grignard reagent high-level tank 62, the Grignard reagent feeding control device 61 being arranged at the top of the Grignard reagent high-level tank 62, the discharge pipelines of the multiple groups of tower fixed bed reaction systems 1 being connected into one pipeline, the one pipeline being divided into two pipelines and being connected with the Grignard reagent feeding control devices 61 of the two groups of Grignard reagent collecting systems 6, respectively, the bottom discharge openings of the Grignard reagent high-level tanks 62 of the two groups of Grignard reagent collecting systems 6 being connected after being combined, and being connected with a Grignard reaction safety control assembly 7. Nitrogen seals and tail gas pipelines are arranged on the halogenated hydrocarbon / THF mixed liquid feeding tank 2 and the Grignard reagent high-level tank 62, the Grignard reagent feeding control device 61 comprising a remote liquid level meter arranged on the Grignard reagent high-level tank 62 and a feeding start-on valve interlocked with the remote liquid level meter; the Grignard reaction safety control assembly 7 comprising a dropwise addition pneumatic regulating valve and a discharge pneumatic on-off valve.

[0037] As Figures 3 to 6As shown, the plurality of sets of tower type fixed bed reaction systems 1 are arranged on the movable support 8, the movable support 8 comprises a plurality of sets of mounting frames 81, the mounting frames 81 are fixedly connected between each other, one set of tower type fixed bed reaction system 1 is arranged on one set of mounting frame 81, the bottom of each set of mounting frame 81 is provided with a rotatable folding movable supporting leg 811, the inner side of the movable supporting leg 811 is provided with a limiting groove 8111, the bottom of the mounting frame 81 is provided with a sliding block 8112, the sliding block 8112 is in the shape of an I-beam, one end of the limiting groove 8111 is an open mouth, and the other end is a limiting structure, after the movable supporting leg 811 is folded, the sliding block 8112 slides from the open mouth to the limiting structure, so that the movable supporting leg 811 is limited and fixed, at this time, a large space is reserved at the bottom of the movable support 8, which can be used for placing the material feeding module.

[0038] A Grignard reagent preparation process using the above-mentioned integrated high-safety mechanical stirring-free Grignard reagent preparation device, comprising the following steps:

[0039] 1) Nitrogen replacement, open the circulating cooler 12, the halogenated hydrocarbon / THF mixed solution is buffered through the halogenated hydrocarbon / THF mixed solution feeding tank 2, the halogenated hydrocarbon / THF mixed solution enters the tower type fixed bed reactor 11 through the circulating pump 13 and contacts with the magnesium filler layer 112, at the same time, the initiator is introduced into the tower type fixed bed reactor 11 through the initiator feeding system 4 to initiate the Grignard reagent preparation reaction, after the reaction starts, the liquid phase fills the tower type fixed bed reactor 11, under the action of the circulating pump 13, continuously passes through the tower type fixed bed reactor 11 to react with magnesium to generate heat and generate Grignard reagent, and then passes through the circulating cooler 12 to control the temperature to a safe temperature;

[0040] 2) The product concentration is detected at the outlet of the circulating cooler 12, when the product concentration reaches the requirement, the circulating reaction pipeline is closed, and the Grignard reagent at the outlet of the tower type fixed bed reaction system 1 is introduced into the Grignard reagent high-level tank 62;

[0041] 3) After the completion of the discharging of step 2), the circulating reaction pipeline is switched back, the feeding pipeline is switched to the quenching agent feeding system 5 to introduce the quenching agent into the tower type fixed bed reactor 11, after the circulation quenching, the feeding is switched to nitrogen, and the discharging is switched to the blowdown to blow clean the liquid phase material in the tower type fixed bed reaction system 1;

[0042] 4) The magnesium filler layer 112 of the cleaned tower type fixed bed reaction system 1 is disassembled by disassembling the detachable flange 111, and the new filler is replaced;

[0043] 5) The tower type fixed bed reaction system 1 with the replaced filler reenters the next reaction period, and a plurality of sets of tower type fixed bed reaction systems 1 alternately perform reaction and replacement to ensure the continuous progress of the reaction;

[0044] 6) A group of Grignard reagent receiving system 6 Grignard reagent high tank 62 is in the state of dropping, the discharge speed is controlled by Grignard reaction safety control assembly 7, another group of Grignard reagent receiving system 6 Grignard reagent high tank 62 is in the state of receiving, when Grignard reagent high tank 62 in the state of receiving reaches the upper limit of receiving, Grignard reagent high tank 62 in the state of dropping has been dropped, the working state of Grignard reagent high tank 62 is switched by Grignard reagent feeding control device 61, so on and so forth, continuous production is realized, the dropping state is that the feeding start switch valve is closed, the dropping pneumatic regulating valve and the discharge pneumatic switch valve are opened, and the temperature signal of the discharge port is received to adjust the discharge opening degree, the receiving state is that the feeding start switch valve is opened, and the dropping pneumatic regulating valve and the discharge pneumatic switch valve are closed.

[0045] Example 1

[0046] The device and process are used for the production of a pesticide intermediate, the raw material of the Grignard reagent preparation process is chlorobutane, the raw material dosage is 60 kg / h, the initiator is bromobutane, the initiator dosage is 6 kg / h, the solvent is tetrahydrofuran, the solvent dosage is 348 kg / h, and the magnesium dosage is 15 kg / h; The reaction time required by the single tower fixed bed reaction system 1 is 6h, the number of the tower fixed bed reaction system 1 used is 6 sets, and the volume of the halogenated hydrocarbon / THF mixed liquid feeding tank 2 is 3000L; The coolant used is -15 DEG C heat conducting oil, the obtained reaction material flow is 429 kg / h, and the reaction product concentration is 18.88%.

[0047] Example 2

[0048] The device and process are used for the production of a raw material drug, the raw material of the Grignard reagent preparation process is bromoethane, the raw material dosage is 40 kg / h, the initiator is iodine, the initiator dosage is 4 kg / h, the solvent is tetrahydrofuran, the solvent dosage is 220 kg / h, and the magnesium dosage is 10 kg / h; The reaction time required by the single tower fixed bed reaction system 1 is 4h, the number of the tower fixed bed reaction system 1 used is 4 sets, and the volume of the feeding tank is 2000L; The coolant used is -25 DEG C heat conducting oil, the obtained reaction material flow is 274 kg / h, and the reaction product concentration is 19.71%.

[0049] Example 3

[0050] The device and process are used for producing certain health care products, the raw material of the Grignard reagent preparation process is chloropropane, the raw material dosage is 20kg / h, the initiator is potassium iodide, the initiator dosage is 2kg / h, the solvent is methyl tetrahydrofuran, the solvent dosage is 120kg / h, and the magnesium dosage is 5kg / h; the reaction time required by the single tower fixed bed reaction system 1 is 8h, the number of the tower fixed bed reaction system 1 used is 8 sets, and the volume of the feed tank is 4000L; the refrigerant used is -35 DEG C ethanol, the reaction product flow is 147kg / h, and the reaction product concentration is 18.37%.

[0051] Example 4

[0052] The device and process are used for producing certain food additives, the raw material of the Grignard reagent preparation process is chlorobutane, the raw material dosage is 25kg / h, the initiator is bromobutane, the initiator dosage is 2.5kg / h, the solvent is methyl tetrahydrofuran, the solvent dosage is 125kg / h, and the magnesium dosage is 6.25kg / h; the reaction time required by the single tower fixed bed reaction system 1 is 6h, the number of the tower fixed bed reaction system 1 used is 6 sets, and the volume of the feed tank is 3000L; the refrigerant used is freon, the reaction product flow is 158.75kg / h, and the reaction product concentration is 21.26%.

[0053] Example 5

[0054] The device and process are used for producing certain pesticide intermediates, the raw material of the Grignard reagent preparation process is bromoethane, the raw material dosage is 80kg / h, the initiator is iodine, the initiator dosage is 8kg / h, the solvent is diethyl ether, the solvent dosage is 465kg / h, and the magnesium dosage is 20kg / h; the reaction time required by the single tower fixed bed reaction system 1 is 4h, the number of the tower fixed bed reaction system 1 used is 4 sets, and the volume of the feed tank is 2000L; the refrigerant used is -15 DEG C heat conducting oil, the reaction product flow is 573kg / h, and the reaction product concentration is 18.85%.

[0055] Example 6

[0056] The device and process are used for producing certain raw pharmaceuticals, the raw material of the Grignard reagent preparation process is chloropropane, the raw material dosage is 100kg / h, the initiator is bromopropane, the initiator dosage is 10kg / h, the solvent is diethyl ether, the solvent dosage is 600kg / h, and the magnesium dosage is 25kg / h; the reaction time required by the single tower fixed bed reaction system 1 is 8h, the number of the tower fixed bed reaction system 1 used is 8 sets, and the volume of the feed tank is 4000L; the refrigerant used is -25 DEG C heat conducting oil, the reaction product flow is 735kg / h, and the reaction product concentration is 18.37%.

[0057] Example 7

[0058] The device and process are used for producing a certain health care product, the raw material of the Grignard reagent preparation process is chlorobutane, the raw material dosage is 80kg / h, the initiator is iodine, the initiator dosage is 8kg / h, the solvent is tetrahydrofuran, the solvent dosage is 450kg / h, and the magnesium dosage is 20kg / h; the reaction time required by a single tower type fixed bed reaction system 1 is 10h, the number of the tower type fixed bed reaction system 1 used is 10 sets, and the volume of the feed tank is 5000L; the refrigerant used is -35 DEG C ethanol, the obtained reaction product flow is 558kg / h, and the reaction product concentration is 19.35%.

[0059] Example 8

[0060] The device and process are used for producing a certain food additive, the raw material of the Grignard reagent preparation process is bromoethane, the raw material dosage is 25kg / h, the initiator is potassium iodide, the initiator dosage is 2.5kg / h, the solvent is tetrahydrofuran, the solvent dosage is 130kg / h, and the magnesium dosage is 6.25kg / h; the reaction time required by a single tower type fixed bed reaction system 1 is 12h, the number of the tower type fixed bed reaction system 1 used is 12 sets, the volume of the feed tank is 6000L; the refrigerant used is freon, the obtained reaction product flow is 163.75kg / h, and the reaction product concentration is 20.61%.

[0061] Example 9

[0062] The device and process are used for producing a certain pesticide intermediate, the raw material of the Grignard reagent preparation process is chloropropane, the raw material dosage is 60kg / h, the initiator is potassium iodide, the initiator dosage is 6kg / h, the solvent is methyl tetrahydrofuran, the solvent dosage is 320kg / h, and the magnesium dosage is 15kg / h; the reaction time required by a single tower type fixed bed reaction system 1 is 6h, the number of the tower type fixed bed reaction system 1 used is 6 sets, the volume of the feed tank is 3000L; the refrigerant used is -15 DEG C heat conducting oil, the obtained reaction product flow is 401kg / h, and the reaction product concentration is 20.20%.

[0063] Example 10

[0064] The device and process are used for producing a certain raw material medicine, the raw material of the Grignard reagent preparation process is chlorobutane, the raw material dosage is 40kg / h, the initiator is iodine, the initiator dosage is 4kg / h, the solvent is methyl tetrahydrofuran, the solvent dosage is 250kg / h, and the magnesium dosage is 10kg / h; the reaction time required by a single tower type fixed bed reaction system 1 is 4h, the number of the tower type fixed bed reaction system 1 used is 4 sets, the volume of the feed tank is 2000L; the refrigerant used is -25 DEG C heat conducting oil, the obtained reaction product flow is 304kg / h, and the reaction product concentration is 17.76%.

[0065] Example 11

[0066] The apparatus and process of this invention are used to produce a certain health product. In the Grignard reagent preparation process, the raw material is bromoethane at a rate of 50 kg / h, the initiator is iodine at a rate of 5 kg / h, the solvent is diethyl ether at a rate of 300 kg / h, and the amount of metallic magnesium is 12.5 kg / h. The reaction time required for a single tower-type fixed-bed reaction system 1 is 8 hours, and 8 sets of tower-type fixed-bed reaction systems 1 are used. The feed tank volume is 4000 L. The refrigerant used is -35℃ ethanol, the flow rate of the resulting reactants is 367.5 kg / h, and the concentration of the reaction product is 18.37%.

[0067] Example 12

[0068] The apparatus and process of this invention are used to produce a certain food additive. In the Grignard reagent preparation step, the raw material is chloropropane at a rate of 90 kg / h, the initiator is bromopropane at a rate of 9 kg / h, the solvent is diethyl ether at a rate of 500 kg / h, and the amount of metallic magnesium is 22.5 kg / h. The reaction time required for a single tower-type fixed-bed reaction system 1 is 10 hours, and 10 sets of tower-type fixed-bed reaction systems 1 are used, with a feed tank volume of 5000 L. The refrigerant used is Freon, the resulting reactant flow rate is 621.5 kg / h, and the concentration of the reaction product is 19.55%.

Claims

1. An integrated high safety Grignard reagent preparation device without mechanical stirring, characterized in that, The application relates to a preparation method of Grignard reagent, which comprises a material feeding module, a Grignard reagent preparation module without stirring and a Grignard reagent using module.

2. The integrated high safety no-mechanical stirring Grignard reagent preparation device according to claim 1, wherein, The material feeding module is connected with the bottom of the tower type fixed bed reactor (11) through the circulating pump (13), the upper part and the lower part of the tower type fixed bed reactor (11) are respectively provided with detachable flanges (111), a metal magnesium filler layer (112) is arranged in the middle part of the tower type fixed bed reactor (11) between the detachable flanges (111), the upper end and the lower end of the metal magnesium filler layer (112) are respectively provided with filter screens (113), a discharging filter layer (114) is arranged in the top of the tower type fixed bed reactor (11), and a feeding distributor (115) is arranged in the bottom of the tower type fixed bed reactor (11) and connected with the circulating pump (13) through a pipeline.

3. The integrated high safety no-mechanical stirring Grignard reagent preparation device according to claim 2, wherein, The material feeding module comprises a halogenated hydrocarbon / THF mixed liquid feeding tank (2), a feeding tank liquid supplementing system (3), an initiator feeding system (4) and a quenching agent feeding system (5), the feeding tank liquid supplementing system (3) is connected with the halogenated hydrocarbon / THF mixed liquid feeding tank (2), the discharging pipe of the halogenated hydrocarbon / THF mixed liquid feeding tank (2) is divided into multiple pipelines, each pipeline is connected with a group of tower type fixed bed reaction systems (1), the discharging pipe of the initiator feeding system (4) is divided into multiple pipelines, each pipeline is connected with a group of tower type fixed bed reaction systems (1), and the discharging pipe of the quenching agent feeding system (5) is divided into multiple pipelines, each pipeline is connected with a group of tower type fixed bed reaction systems (1).

4. The integrated high safety no-mechanical stirring Grignard reagent preparation device according to claim 3, characterized in that, The Grignard reagent using module comprises two groups of Grignard reagent collecting systems (6), each group of Grignard reagent collecting systems (6) comprises a Grignard reagent feeding control device (61) and a Grignard reagent high tank (62), the Grignard reagent feeding control device (61) is arranged at the top of the Grignard reagent high tank (62), the discharging pipes of the multiple groups of tower type fixed bed reaction systems (1) are connected into one pipeline, the one pipeline is divided into two pipelines, and the two pipelines are connected with the Grignard reagent feeding control devices (61) of the two groups of Grignard reagent collecting systems (6) respectively, and the bottom discharging openings of the Grignard reagent high tanks (62) of the two groups of Grignard reagent collecting systems (6) are connected with a Grignard reaction safety control assembly (7) after being connected.

5. The integrated high safety no-mechanical stirring Grignard reagent preparation device according to claim 4, wherein, The Grignard reagent feeding control device (61) comprises a remote liquid level meter arranged on the Grignard reagent high tank (62) and a feeding start switch valve interlocked with the remote liquid level meter, and the Grignard reaction safety control assembly (7) comprises a dropwise adding pneumatic regulating valve and a discharging pneumatic switch valve. Nitrogen seals and tail gas pipes are arranged on the halogenated hydrocarbon / THF mixed liquid feeding tank (2) and the Grignard reagent high tank (62).

6. The integrated high safety no-mechanical stirring Grignard reagent preparation device according to claim 5, wherein, The plurality of tower type fixed bed reaction systems (1) are arranged on the movable support (8), the movable support (8) comprises a plurality of mounting frames (81), the mounting frames (81) are fixedly connected between the mounting frames (81), a tower type fixed bed reaction system (1) is arranged on a mounting frame (81), and the bottom of each mounting frame (81) is provided with a rotatable folding movable supporting leg (811). The inner side of the movable supporting leg (811) is provided with a limiting groove (8111), the bottom of the mounting frame (81) is provided with a sliding block (8112), one end of the limiting groove (8111) is a through opening, the other end is a limiting structure, the sliding block (8112) slides from the through opening to the limiting structure, and the movable supporting leg (811) is limited and fixed.

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