CN216172300U

CN216172300U - Low-temperature ventilation device for synthesizing BOC anhydride

Info

Publication number: CN216172300U
Application number: CN202122479228.1U
Authority: CN
Inventors: 王晓伟; 张宝亮; 王艳艳; 郝光顺
Original assignee: Shandong Langheng Chemical Co ltd
Current assignee: Shandong Langheng Chemical Co ltd
Priority date: 2021-10-14
Filing date: 2021-10-14
Publication date: 2022-04-05
Anticipated expiration: 2031-10-14

Abstract

The utility model discloses a low-temperature ventilation device for synthesizing BOC anhydride, which comprises a reaction kettle, wherein the top of the reaction kettle is also provided with a ventilation main pipe with a ventilation valve, and the ventilation main pipe supplies air through a gas compressor; the stirring shaft ventilating pipe is communicated with the stirring paddle horizontal ventilating branch pipe; the main vent pipe is also communicated with an inner wall vent pipe arranged on the inner wall of the reaction kettle, and the inner wall vent pipe comprises a plurality of vertical vent branch pipes and horizontal vent branch pipes which are mutually crossed and communicated. The device can keep the reaction process at low temperature all the time, realize the control of ventilation volume and ventilation flow rate, ensure the uniform distribution of carbon dioxide in the solvent, be beneficial to the stable reaction, ensure the thorough conversion of the substrate, reduce the gas volume escaping from the liquid surface and reduce the energy consumption; meanwhile, the gas-liquid mixing effect is improved, the concentration of dissolved carbon dioxide in a reaction system is improved, and the reaction efficiency is improved.

Description

Low-temperature ventilation device for synthesizing BOC anhydride

Technical Field

The utility model belongs to the technical field of chemical equipment, relates to synthesis of BOC anhydride, and particularly relates to a low-temperature ventilation device for synthesizing BOC anhydride.

Background

BOC acid anhydride (i.e. di-tert-butyl dicarbonate) is an organic compound, is used for introducing a tert-butoxycarbonyl protecting group in organic synthesis, is particularly applied to amino protection of amino acid, and is widely applied to synthesis of various products such as medicines, protein and polypeptide synthesis, biochemistry, food, cosmetics and the like, thereby having wide market prospect. The first step of the synthesis needs to introduce carbon dioxide gas into an organic solvent of sodium tert-butoxide or potassium tert-butoxide at a low temperature, wherein the introduction mode of the carbon dioxide gas has great influence on the stirring operation and the material chemical process. The traditional method is to directly extend the vent pipe into the bottom of the reaction kettle or to use a single circle of vent pipe to enlarge the corresponding vent area, but the methods have the problems of difficult control of the uniformity of gas distribution, the size of bubbles and the stirring effect of gas on materials at the bottom of a container, uneven gas distribution, small contact area, dead angles of the reaction kettle and the like,

disclosure of Invention

Aiming at the defects in the prior art, the utility model aims to provide a low-temperature ventilation device for synthesizing BOC anhydride, and solve the technical problem that the ventilation uniformity of the device in the prior art needs to be further improved.

In order to solve the technical problems, the utility model adopts the following technical scheme:

a low-temperature ventilation device for synthesizing BOC anhydride comprises a reaction kettle, wherein the reaction kettle is provided with a stirring shaft, the stirring shaft is provided with a stirring paddle, and the stirring shaft is driven by a stirring motor; the top of the reaction kettle is provided with a feed inlet, and the bottom of the reaction kettle is provided with a discharge outlet;

the top of the reaction kettle is also provided with a main ventilation pipe with a ventilation valve, and the main ventilation pipe supplies air through a gas compressor; the top of the reaction kettle is also provided with an air outlet main pipe with an air outlet valve;

the stirring shaft is provided with a stirring shaft ventilating pipe, the stirring shaft ventilating pipe is communicated with a stirring paddle horizontal ventilating branch pipe, the stirring paddle horizontal ventilating branch pipe is positioned in the stirring paddle, and the stirring paddle horizontal ventilating branch pipe is provided with a plurality of first ventilating holes;

the inner wall breather pipe comprises a plurality of vertical breather branch pipes and a plurality of horizontal breather branch pipes which are mutually crossed and communicated, the vertical breather branch pipes are provided with a plurality of second breather holes, and the horizontal breather branch pipes are provided with a plurality of third breather holes;

the outer wall of the reaction kettle is provided with a heating jacket, and the outer wall of the reaction kettle in the heating jacket is provided with a cooling coil.

The utility model also has the following technical characteristics:

the reaction kettle is also provided with a thermometer and a pressure gauge.

The stirring paddle adopts a polytetrafluoroethylene multilayer turbine type stirring paddle.

And carbon dioxide concentration sensors are arranged at the end parts of the horizontal ventilating branch pipe and the vertical ventilating branch pipe of the stirring paddle.

Compared with the prior art, the utility model has the following technical effects:

the device can keep the reaction process at low temperature all the time, realize the control of ventilation volume and ventilation flow rate, ensure the uniform distribution of carbon dioxide in a solvent, be beneficial to the stable reaction, ensure the thorough conversion of a substrate, reduce the gas volume escaping from a liquid surface and reduce the energy consumption; meanwhile, the gas-liquid mixing effect is improved, the concentration of dissolved carbon dioxide in a reaction system is improved, and the reaction efficiency is improved.

The device can be used for automatically controlling the carbon dioxide ventilation quantity and enabling reaction gas-liquid mixing to be more uniform. Therefore, the problems of uneven gas ventilation, high energy consumption, waste of gas resources, high cost, poor product quality and low production efficiency in the traditional ventilation process are solved.

Drawings

FIG. 1 is a schematic diagram of the overall configuration of a low temperature vent for the synthesis of BOC anhydride.

Fig. 2 is a schematic structural diagram of a stirring paddle horizontal air branch pipe.

Fig. 3 is a schematic structural view of an inner wall breather pipe.

The meaning of the individual reference symbols in the figures is: 1-a reaction kettle, 2-a stirring shaft, 3-a stirring paddle, 4-a stirring motor, 5-a feeding port, 6-a discharging port, 7-a vent valve, 8-a vent header pipe, 9-a gas compressor, 10-a gas outlet valve, 11-a gas outlet header pipe, 12-a stirring shaft vent pipe, 13-a stirring paddle horizontal vent branch pipe, 14-a first vent hole, 15-an inner wall vent pipe, 1501-a vertical vent branch pipe, 1502-a horizontal vent branch pipe, 16-a second vent hole, 17-a third vent hole, 18-a heating jacket, 19-a cooling coil pipe, 20-a thermometer, 21-a pressure gauge, 22-a carbon dioxide concentration sensor and 23-a PLC (programmable logic controller).

The present invention will be explained in further detail with reference to examples.

Detailed Description

It is to be understood that all parts and devices of the present invention, unless otherwise specified, are intended to be covered by the present invention as if they were all known in the art.

The present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention fall within the protection scope of the present invention.

Example 1:

the embodiment provides a low-temperature ventilation device for synthesizing BOC anhydride, which comprises a reaction kettle 1, wherein the reaction kettle 1 is provided with a stirring shaft 2, the stirring shaft 2 is provided with a stirring paddle 3, and the stirring shaft 2 is driven by a stirring motor 4; the top of the reaction kettle 1 is provided with a feed inlet 5, the bottom of the reaction kettle 1 is provided with a discharge outlet 6,

the top of the reaction kettle 1 is also provided with a vent main pipe 8 with a vent valve 7, and the vent main pipe 8 supplies gas through a gas compressor 9; the top of the reaction kettle 1 is also provided with an air outlet main pipe 11 with an air outlet valve 10;

the main ventilation pipe 8 is communicated with a stirring shaft ventilation pipe 12 arranged inside the stirring shaft 2, the stirring shaft ventilation pipe 12 is communicated with a stirring paddle horizontal ventilation branch pipe 13, the stirring paddle horizontal ventilation branch pipe 13 is positioned in the stirring paddle 3, and a plurality of first ventilation holes 14 are formed in the stirring paddle horizontal ventilation branch pipe 13;

the air manifold 8 is also communicated with an inner wall air pipe 15 arranged on the inner wall of the reaction kettle 1, the inner wall air pipe 15 comprises a plurality of vertical air branch pipes 1501 and horizontal air branch pipes 1502 which are mutually crossed and communicated, a plurality of second air vents 16 are formed in the vertical air branch pipes 1501, and a plurality of third air vents 17 are formed in the horizontal air branch pipes 1502;

the outer wall of the reaction kettle 1 is provided with a heating jacket 18, and the outer wall of the reaction kettle 1 in the heating jacket 18 is provided with a cooling coil 19.

In this embodiment, the reactor body of the reaction kettle 1 is an acid and alkali resistant enamel reactor. The inner wall is stuck with a layer of anticorrosive coating.

In this embodiment, the vent valve 7 is a three-way vent valve capable of switching the introduction of two gases, such as nitrogen and carbon dioxide, at will.

In this embodiment, the distance between two adjacent vent holes is 50mm, and the diameter of the vent hole is about 20 mm.

In this embodiment, the reactor jacket 18 is a smooth jacket with a heat carrier therein, so as to achieve the purpose of rapid temperature rise.

In this embodiment, the recyclable low-temperature brine ice is introduced into the cooling coil 19 during cooling.

In a preferred embodiment of the present invention, the main gas pipe 8 is connected to the stirring shaft 2 by a known and commonly used connection method of a rotary ventilation shaft, so as to ensure that gas can stably and smoothly enter the stirring shaft ventilation pipe 12 from the main gas pipe 8.

As a preferable scheme of this embodiment, a thermometer 20 and a pressure gauge 21 are further disposed on the reaction kettle 1. The thermometer 20 is used for detecting the temperature of the inside of the reaction vessel 1, and its lower end is inserted into the reaction vessel 1 at a position 2/3. The pressure gauge 21 is used for displaying the pressure condition in the reaction kettle 1 in real time.

In a preferred embodiment of the present invention, a polytetrafluoroethylene multi-layer turbine type stirring blade is used as the stirring blade 3.

As a preferable scheme of this embodiment, the end of the stirring paddle horizontal aeration branch pipe 13 and the end of the vertical aeration branch pipe 1501 are both provided with carbon dioxide concentration sensors 22.

As a preferable scheme of this embodiment, the system further comprises a PLC controller 23, an input end of the PLC controller 23 is connected to the carbon dioxide concentration sensor 22, and an output end of the PLC controller 23 is connected to the gas compressor 9 to control the ventilation volume.

Taking potassium tert-butoxide to synthesize di-tert-butyl dicarbonate as an example, the specific working process of the device is illustrated:

11kg of potassium tert-butoxide is added from a feed inlet 5, 110L of cyclohexane is dried, a vent valve 7 and an air outlet valve 10 are opened, nitrogen is introduced to ensure that the reaction system is in a nitrogen atmosphere, a stirring motor 4 is started, and a stirring paddle 3 starts to stir. The temperature of the reaction system is reduced to 0 to 10 ℃ by introducing ice salt water through a temperature reduction coil 19. After the reaction starts, the nitrogen pipeline is switched to be a carbon dioxide pipeline, the introduced carbon dioxide gas passes through the ventilation main pipe 8, then the stirring shaft ventilation pipe 12, the stirring paddle horizontal ventilation branch pipe 13, the vertical ventilation branch pipe 1501 and the horizontal ventilation branch pipe 1502 are introduced, then the carbon dioxide gas is introduced into the reaction system through the first ventilation hole 14, the second ventilation hole 16 and the third ventilation hole 17, and the flow of the carbon dioxide is monitored through the carbon dioxide concentration sensor 22. About 2700L of carbon dioxide gas was blown in for a total of about 3 hours. Bubbles are evenly bubbled in the reaction kettle 1 until the reaction is detected to be finished by methyl red-bromophenol blue or other indicators. Closing the vent valve 7 and the gas outlet valve 10 and continuing the heat preservation reaction for about 1 to 2 hours under the low temperature condition to obtain a primary reaction product.

Claims

1. A low-temperature ventilation device for synthesizing BOC anhydride comprises a reaction kettle (1), wherein a stirring shaft (2) is arranged on the reaction kettle (1), a stirring paddle (3) is arranged on the stirring shaft (2), and the stirring shaft (2) is driven by a stirring motor (4); the top of reation kettle (1) seted up feed inlet (5), the bottom of reation kettle (1) seted up discharge gate (6), its characterized in that:

the top of the reaction kettle (1) is also provided with a vent main pipe (8) with a vent valve (7), and the vent main pipe (8) supplies air through a gas compressor (9); the top of the reaction kettle (1) is also provided with an air outlet main pipe (11) with an air outlet valve (10);

the air main pipe (8) is communicated with an air pipe (12) of the stirring shaft arranged in the stirring shaft (2), the air pipe (12) of the stirring shaft is communicated with a horizontal air branch pipe (13) of the stirring paddle, the horizontal air branch pipe (13) of the stirring paddle is positioned in the stirring paddle (3), and a plurality of first air holes (14) are formed in the horizontal air branch pipe (13) of the stirring paddle;

the aeration main pipe (8) is also communicated with an inner wall aeration pipe (15) arranged on the inner wall of the reaction kettle (1), the inner wall aeration pipe (15) comprises a plurality of vertical aeration branch pipes (1501) and horizontal aeration branch pipes (1502) which are mutually crossed and communicated, a plurality of second aeration holes (16) are formed in the vertical aeration branch pipes (1501), and a plurality of third aeration holes (17) are formed in the horizontal aeration branch pipes (1502);

the outer wall of the reaction kettle (1) is provided with a heating jacket (18), and the outer wall of the reaction kettle (1) in the heating jacket (18) is provided with a cooling coil (19).

2. The low-temperature aerator for synthesizing BOC anhydrides of claim 1, wherein the reaction kettle (1) is further provided with a thermometer (20) and a pressure gauge (21).

3. The cryogenic aeration device for synthesizing BOC anhydrides of claim 1, wherein the stirring blade (3) is a polytetrafluoroethylene multi-layer turbine type stirring blade.

4. The low-temperature aeration device for synthesizing BOC anhydride according to claim 1, wherein the carbon dioxide concentration sensors (22) are arranged at the end part of the stirring paddle horizontal aeration branch pipe (13) and the end part of the vertical aeration branch pipe (1501).