CN218609309U - Novel glass reaction kettle structure - Google Patents

Abstract

The utility model relates to a reation kettle equipment technical field, concretely relates to novel glass reation kettle structure, the reactor comprises a kettle body, the one-level coil pipe condenser, liquid seal bottle, second grade coil pipe condenser, dropwise add bottle and condensation distillation liquid receiving bottle, the steam that the internal reaction of cauldron produced enters into one-level coil pipe condenser condensation liquefaction, then accessible liquid seal bottle flows back to the cauldron internal, also can directly flow condensation distillation liquid receiving bottle through the glass pipeline, second grade coil pipe condenser can cool off a small amount of steam from one-level coil pipe condenser effusion, and guide condensation distillation liquid receiving bottle with the condensation distillation liquid after the cooling, the cauldron body is directly or indirectly adjusted through second grade coil pipe condenser to vacuum equipment, the atmospheric pressure of dropwise add bottle and condensation distillation liquid receiving bottle, thereby make the gas circuit and the liquid circuit separation of equipment.

Description

Novel glass reaction kettle structure

Technical Field

The utility model relates to a reation kettle equipment technical field, concretely relates to novel glass reation kettle structure.

Background

The reaction kettle structure commonly used at present comprises a glass kettle body interlayer, a glass kettle body inner part, a high-position dropping bottle, a glass coil condenser, a steam pipeline, a liquid reflux pipeline, a liquid separating ball bottle, a glass tetrafluoro valve and a condensed distilled liquid receiving bottle.

The glass kettle body interlayer is used for circulating heat-conducting liquid;

the glass kettle body is used for placing reaction materials, the heat-conducting liquid in the interlayer is conducted to the reaction materials, and the boiling point of solvent components in the reaction materials is reduced under the action of vacuum;

the high-level dropping bottle is used for dropping a catalytic solvent into the glass kettle body in the reaction process;

the glass coil condenser is characterized in that after reaction materials in the kettle body are heated, specific solvent components reach the boiling point, the reaction materials are converted into gas state to enter the coil condenser, meanwhile, cooling water is introduced into the coil condenser, and the gas state is condensed into liquid state again to flow downwards after being cooled;

the condensed and distilled liquid flows back to the kettle through the liquid separating ball bottle or is collected to a receiving bottle;

a glass tetrafluoro valve, which is opened, and the condensed distilled liquid flows into the receiving bottle;

the distilled liquid receiving flask was condensed.

The above structure has the following disadvantages: 1. after the kettle is vacuumized, the high-level dropping bottle and the vacuum state in the kettle cannot be synchronized, so that liquid materials in the high-level dropping bottle are sucked in the kettle in an accelerating manner under the vacuum action, the dropping speed cannot be accurately controlled, and the synthetic reaction fails; 2. after the kettle is vacuumized, the liquid flows back into the glass kettle body from time to time and is recycled to the condensed distilled liquid receiving bottle from time to time, and the glass tetrafluoro valve needs to be frequently opened or closed, so that the vacuum state of the receiving bottle and the kettle cannot be synchronous, and the liquid at the position of the liquid separating ball bottle cannot flow into the receiving bottle in the vacuum state; 3 the vapor pipeline and the liquid return pipeline are the same pipeline, so that a flooding phenomenon is generated. To the above problem, the utility model provides a novel glass reaction kettle structure.

SUMMERY OF THE UTILITY MODEL

In order to solve the problem, the utility model provides a novel glass reation kettle structure, the reactor comprises a kettle body, the one-level coil pipe condenser, liquid seal bottle, the second grade coil pipe condenser, dropwise add bottle and condensation distillation liquid receiving bottle, the steam that the internal reaction of cauldron produced enters into one-level coil pipe condenser condensation liquefaction, then accessible liquid seal bottle flows back to the cauldron internal, also can directly flow condensation distillation liquid receiving bottle through the glass pipeline, the second grade coil pipe condenser can cool off a small amount of steam from the effusion of one-level coil pipe condenser, and the condensation distillation liquid after will cooling leads condensation distillation liquid receiving bottle, the cauldron body is directly or indirectly adjusted through the second grade coil pipe condenser to vacuum equipment, the atmospheric pressure of dropwise add bottle and condensation distillation liquid receiving bottle, thereby make the gas circuit and the liquid circuit separation of equipment.

In order to solve the problems, the novel glass reaction kettle structure comprises

The kettle comprises a kettle body, wherein a kettle cover of the kettle body is provided with a dripping port, a steam interface and a return port;

the primary coil condenser is provided with an air inlet, a liquid outlet and a vacuum interface, the primary coil condenser is installed in a tilted horizontal mode, the air inlet is communicated with the steam interface of the kettle cover through a glass bent pipe, and the liquid port end of the primary coil condenser is communicated with the condensed distilled liquid receiving bottle through a glass pipeline;

the inlet end of the liquid seal bottle is communicated with the glass pipeline, and the outlet end of the liquid seal bottle is communicated with a reflux port on the kettle cover through a switch valve;

the secondary coil condenser is vertically arranged, the top end and the bottom end of the secondary coil condenser are respectively provided with an upper port and a lower port, the upper port is communicated with the dropping bottle and the vacuum interface of the primary coil condenser, the lower port is communicated with the condensed distilled liquid receiving bottle, the side surface of the secondary coil condenser is provided with a side interface, and the side interface is communicated with vacuum equipment;

the dropping bottle is communicated with a dropping port of the kettle cover through a constant-pressure dropping funnel;

the condensation distillation liquid receiving bottle is provided with an air pressure balancing port and a receiving valve, the air pressure balancing port is communicated with a lower port of the secondary coil condenser, and the receiving valve is communicated with the tail end of the glass pipeline.

Furthermore, a sampling valve is arranged at the bottom of the liquid seal bottle.

Further, the air inlet of the first-level coil condenser is higher than the liquid outlet and the vacuum interface, the vacuum interface is higher than the liquid outlet, and a condensation pipeline in the first-level coil condenser and a condensation pipeline in the second-level coil condenser are communicated with the temperature control equipment.

Furthermore, a continuous liquid adding pipeline is connected to the dropping bottle, and a liquid adding valve is installed at the tail end of the continuous liquid adding pipeline.

Furthermore, a three-way joint is arranged on the glass pipeline, and the liquid seal bottle is communicated with the glass pipeline through the three-way joint.

Furthermore, the two condensed distilled liquid receiving bottles are provided, the air pressure balance ports of the two condensed distilled liquid receiving bottles are communicated with the lower port of the secondary coil condenser, and the receiving valves of the two condensed distilled liquid receiving bottles are communicated with the tail end of the glass pipeline.

Further, the condensed distilled liquid receiving bottle is provided with a liquid discharge valve.

Furthermore, the center of the kettle cover is provided with a stirring port, and the kettle cover is also provided with an air exhaust port, a feeding port and a temperature measuring port.

Advantageous effects

1. The vacuum equipment is communicated with the dropping bottle through the secondary coil condenser, so that the air pressure in the dropping bottle can be adjusted, the vacuum equipment is communicated with the condensed distilled liquid receiving bottle through the secondary coil condenser, the condensed distilled liquid receiving bottle is pumped with negative pressure so that the condensed distilled liquid of the glass pipeline can flow into the vacuum equipment, and the vacuum equipment is communicated with the inside of the kettle body through the secondary coil condenser and the coil condenser so as to realize the operation of vacuumizing the inside of the kettle body;

2. when cooled condensed distilled liquid generated by the treatment of the primary coil condenser needs to flow back into the kettle body, a switch valve is opened and a receiving valve is closed, the condensed distilled liquid flows back into the kettle body through a glass pipeline, a liquid seal bottle, the switch valve and a return port in sequence, when the cooled condensed distilled liquid generated by the treatment of the primary coil condenser needs to be recovered into a condensed distilled liquid receiving bottle, the switch valve is closed and the receiving valve is opened, a vacuum device is used for generating a negative pressure environment in the condensed distilled liquid receiving bottle, and the condensed distilled liquid enters the condensed distilled liquid receiving bottle through the glass pipeline and the receiving valve;

3. the equipment adopts a design idea of separating a gas path and a liquid path, so that a vacuum gas path of the equipment reaches a balanced state, and the phenomenon of flooding in the reaction process is avoided.

Drawings

FIG. 1 is a schematic view of the structure of the apparatus;

FIG. 2 is a schematic top view of the kettle cover;

FIG. 3 is a schematic diagram of a primary coil condenser;

FIG. 4 is a schematic of the construction of a two-stage coil condenser;

FIG. 5 is a schematic view of the construction of a liquid-tight bottle;

in the figure: 1. the kettle body, 11, the dropwise add mouth, 12, the steam interface, 13, the backward flow mouth, 14, the kettle cover, 15, the switch valve, 16, the gas vent, 17, the charge door, 18, the temperature measurement mouth, 19, the stirring mouth, 2, one-level coil condenser, 21, the air inlet, 22, the liquid outlet, 23, the vacuum interface, 24, the glass pipeline, 25, the glass return bend, 3, the liquid seal bottle, 31, the entry end, 32, the exit end, 33, the sample valve, 4, the second level coil condenser, 41, the last port, 42, the bottom port, 43, the side interface, 5, the dropwise add bottle, 6, the bottle is received to the condensation distillation liquid.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.

In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description of the present invention and to simplify the description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless expressly specified otherwise.

In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

In the present application, unless expressly stated or limited otherwise, the first feature may be directly on or directly under the second feature or indirectly via intermediate members. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.

In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Moreover, various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art without being mutually inconsistent.

A novel glass reaction kettle structure comprises a kettle body 1, a primary coil condenser 2, a liquid seal bottle 3, a secondary coil condenser 4, a dropping bottle 5 and a condensed distilled liquid receiving bottle 6, and please refer to fig. 1 and fig. 2: the lateral wall of the kettle body 1 is provided with a heat exchange interlayer for heat-conducting fluid to pass through, a kettle cover 14 is installed at the top of the kettle body 1, a dropwise adding port 11, a steam interface 12, a reflux port 13, a stirring port 19, an exhaust port 16, a charging hole 17 and a temperature measuring port 18 are arranged on the kettle cover 14, the stirring port 19 is located at the center of the kettle cover 14, the dropwise adding port 11, the steam interface 12, the reflux port 13, the exhaust port 16, the charging hole 17 and the temperature measuring port 18 are all arranged along the circumferential direction by taking the kettle cover 14 as the center, the exhaust port 16 is used for discharging gas in the kettle body 1, the exhaust port 16 can be sealed, and the charging hole 17 and the steam interface 12 are inclined interfaces inclining towards the direction of the stirring port 19 away.

Referring to fig. 1 and 3, the primary coil condenser 2 is a customized condenser, a condensing pipeline is disposed inside the primary coil condenser 2, two ends of the condensing pipeline fixedly penetrate through an outer wall of the primary coil condenser 2 to be used for connecting a temperature control device, the primary coil condenser 2 is provided with an air inlet 21, an liquid outlet 22 and a vacuum interface 23, the air inlet 21 and the liquid outlet 22 are respectively located at two ends of the primary coil condenser 2, the primary coil condenser 2 is obliquely arranged to enable the air inlet 21 to be higher than the liquid outlet 22 and the vacuum interface 23, the vacuum interface 23 and the liquid outlet 22 are located at the same side of the primary coil condenser 2, and the vacuum interface 23 is higher than the liquid outlet 22 to prevent condensed distilled liquid in the primary coil condenser 2 from flowing into the vacuum interface 23 first. Air inlet 21 passes through glass return bend 25 and the 12 intercommunications of steam interface on the kettle cover 14, and in the steam accessible glass return bend 25 that the reaction produced in the kettle body 1 entered into one-level coil condenser 2, its liquid outlet 22 passed through glass pipeline 24 and condensed distillation liquid receiving bottle 6 intercommunications, install three way connection on the glass pipeline 24, liquid seal bottle 3 passes through three way interface and glass pipeline 24 intercommunication, and condensed distillation liquid of the liquid outlet 22 exhaust of one-level coil condenser 2 can enter into condensed distillation liquid receiving bottle 6 or liquid seal bottle 3 in through glass pipeline 24.

Referring to fig. 1 and 5, the liquid seal bottle 3 is provided with an inlet end 31 and an outlet end 32, the inlet end 31 of the liquid seal bottle 3 is opened on the side wall of the bottle body, an arc tube is arranged in the liquid seal bottle 3, one end of the arc tube is communicated with the inlet end 31, the other end of the arc tube is lower than the inlet end 31, the outlet end 32 is higher than the inlet end 31, the inlet end 31 of the liquid seal bottle 3 is communicated with a three-way connector to be connected to the glass pipeline 24, the outlet end 32 is provided with a switch valve 15, and the outlet end 32 is communicated with the return port 13 on the kettle cover 14 through the switch valve 15. When the switch valve 15 is opened, the condensation distillation liquid in the glass pipeline 24 can enter the liquid seal bottle 3 through the inlet end 31, then overflow from the outlet end 32, flow back to the kettle body 1 through the switch valve 15 and the return port 13, because the end of the arc-shaped pipe in the liquid seal bottle 3 is lower than the inlet end 31, the solution accumulated in the liquid seal bottle 3 seals the end of the arc-shaped pipe, even if the switch valve 15 is in the open state, the steam generated in the reaction kettle can not enter the glass pipeline 24 through the liquid seal bottle 3, the sampling valve 33 is installed at the bottom of the liquid seal bottle 3, and the liquid in the liquid seal bottle 3 can be sampled and detected through the sampling valve 33.

Referring to fig. 1 and 4, the secondary coil condenser 4 is vertically arranged, the secondary coil condenser 4 is a customized condenser, the top end and the bottom end of the customized condenser are respectively provided with an upper port 41 and a lower port 42, a condensing pipeline is arranged in the customized condenser, two ports of the condensing pipeline both fixedly penetrate through the outer wall of the secondary coil condenser 4 to be communicated with a temperature control device, the upper port 41 of the secondary coil condenser 4 is communicated with the dropping bottle 5 and the vacuum port 23 of the primary coil condenser 2 through a three-way joint, the lower port 42 of the secondary coil condenser 4 is communicated with the condensed distilled liquid receiving bottle 6, a side port 43 is arranged on the side surface of the secondary coil condenser 4, the side port 43 is located at the lower section of the secondary coil condenser 4, and the side port 43 is communicated with the vacuum device. A small amount of high temperature vapor escaping from the primary coil condenser 2 to the secondary coil condenser 4 is liquefied after passing through the secondary coil condenser 4, and then enters the condensed distillate receiver flask 6 from the lower port 42.

Referring to fig. 1, the dropping bottle 5 is communicated with a dropping port 11 on the kettle cover 14 through a constant pressure dropping funnel, the dropping bottle 5 is used for adding a catalytic solvent into the reaction kettle, the bottom end of the dropping bottle 5 is higher than the kettle cover 14, the top of the dropping bottle 5 is connected with a continuous liquid feeding pipeline, the continuous liquid feeding pipeline is used for feeding materials into the dropping bottle 5, and a liquid feeding valve is installed at the tail end of the continuous liquid feeding pipeline. The dropping bottle 5 is communicated with the three-way joint through a vacuum balance pipeline, so that the dropping bottle 5 is communicated with the upper port 41 of the secondary coil condenser 4, the air pressure in the dropping bottle 5 can be adjusted by vacuum equipment, and the amount and the speed of adding the catalytic solvent into the reaction kettle by the dropping bottle 5 can be realized.

Referring to fig. 1, the condensed distilled liquid receiving bottle 6 is provided with an air pressure balancing port and a receiving valve, the receiving valve is communicated with the tail end of the glass pipeline 24, the air pressure balancing port is communicated with the lower port 42 of the secondary coil condenser 4, the vacuum equipment can make the condensed distilled liquid in the glass pipeline 24 enter the condensed distilled liquid receiving bottle 6 by pumping negative pressure to the condensed distilled liquid receiving bottle 6, and the condensed distilled liquid receiving bottle 6 is provided with a liquid discharge valve. Preferably, there are two condensed distillation liquid receiving bottles 6, the two condensed distillation liquid receiving bottles 6 are arranged in parallel, the air pressure balance ports of the two condensed distillation liquid receiving bottles are both communicated with the lower port 42 of the secondary coil condenser 4, and the receiving valves of the two condensed distillation liquid receiving bottles are both communicated with the tail end of the glass pipeline 24.

Referring to fig. 1-5, the principle of the present device is as follows: reaction materials are put into a kettle body 1, a stirring device stirs the kettle body 1 through a stirring port 19 of a kettle cover 14 to enable the reaction materials to be fully and uniformly mixed, a dropping bottle 5 adds a catalytic solvent into the kettle body 1 through a constant-pressure dropping funnel, meanwhile, a temperature control device feeds heat-conducting fluid into a heat exchange interlayer of the kettle body 1 to enable the reaction materials to react at a set temperature, according to the progress stage of the reaction, a vacuum device is started to pump negative pressure to a primary coil condenser 2, the kettle body 1 and a condensate distillation liquid receiving bottle 6 through a secondary coil condenser 4 to enable the boiling point of a specific solvent in the kettle body 1 to be reduced, after the specific solvent reaches the boiling point, under the action of vacuum suction, steam enters the primary coil condenser 2 through a steam interface 12 and a glass bent pipe 25, the temperature control device feeds cooling liquid into a condensation pipeline of the primary coil condenser 2 in a circulating manner, most of the steam entering the primary coil condenser 2 can be pre-condensed into a liquid state, a part of escaped gas enters the secondary coil condenser 4, and the temperature control device feeds cooling liquid into the condensation pipeline of the secondary coil condenser 4 in a circulating manner, so that the steam entering the secondary coil condenser 4 is condensed into the condensate liquid receiving bottle 6 and is condensed into the condensate bottle 6. According to the reaction process stage, when the condensed distilled liquid needs to flow back into the kettle body 1, the switch valve 15 at the outlet end 32 of the liquid seal bottle 3 is opened, so that the condensed distilled liquid can flow back into the kettle body 1 through the liquid seal bottle 3, under the action of the liquid seal bottle 3, even if the switch valve 15 is in an open state, the steam in the kettle body 1 cannot enter the liquid seal bottle 3, and when the sampling valve 33 needs to be opened, the solution in the liquid seal bottle 3 can be sampled; when the condensed distilled liquid needs to be recovered to the condensed distilled liquid receiving bottle 6, the receiving valve on the condensed distilled liquid receiving bottle 6 is opened, so that the condensed distilled liquid can enter the condensed distilled liquid receiving bottle 6. In the use of the device, when the condensed distilled liquid is recovered and the catalytic solvent is dripped, the gas circuit and the liquid circuit are separated, so that the pipeline system reaches the vacuum gas circuit balance, and the generation of flooding images is avoided.

The above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above embodiments, and although the present invention has been disclosed with the preferred embodiments, it is not limited to the present invention, and any skilled person in the art can make some modifications or equivalent changes without departing from the technical scope of the present invention.

Claims (8)

1. The utility model provides a novel glass reation kettle structure which characterized in that: comprises that

The device comprises a kettle body (1), wherein a kettle cover (14) of the kettle body (1) is provided with a dripping port (11), a steam interface (12) and a return port (13);

the primary coil condenser (2) is provided with an air inlet (21), a liquid outlet (22) and a vacuum interface (23), the primary coil condenser (2) is installed in a tilted manner, the air inlet (21) is communicated with a steam interface (12) of the kettle cover (14) through a glass bent pipe (25), and the liquid outlet is communicated with a condensed distilled liquid receiving bottle (6) through a glass pipeline (24);

the inlet end (31) of the liquid seal bottle (3) is communicated with the glass pipeline (24), and the outlet end (32) of the liquid seal bottle (3) is communicated with the reflux port (13) on the kettle cover (14) through a switch valve (15);

the secondary coil condenser (4) is vertically arranged, an upper port (41) and a lower port (42) are respectively arranged at the top end and the bottom end of the secondary coil condenser (4), the upper port (41) is communicated with the dropping bottle (5) and the vacuum port (23) of the primary coil condenser (2), the lower port (42) is communicated with the condensed distilled liquid receiving bottle (6), a side port (43) is arranged on the side surface of the secondary coil condenser (4), and the side port (43) is communicated with vacuum equipment;

the dropping bottle (5) is communicated with a dropping port (11) of the kettle cover (14) through a constant-pressure dropping funnel;

the device comprises a condensation distilled liquid receiving bottle (6), wherein an air pressure balancing port and a receiving valve are arranged on the condensation distilled liquid receiving bottle (6), the air pressure balancing port is communicated with a lower port (42) of a secondary coil condenser, and the receiving valve is communicated with the tail end of a glass pipeline (24).

2. The novel glass reaction kettle structure according to claim 1, characterized in that: and a sampling valve (33) is arranged at the bottom of the liquid seal bottle (3).

3. The novel glass reaction kettle structure according to claim 1, characterized in that: air inlet (21) of one-level coil pipe condenser (2) are higher than liquid outlet (22) and vacuum interface (23), and vacuum interface (23) are higher than liquid outlet (22), and the condensation pipeline in one-level coil pipe condenser (2) and the condensation pipeline in the second grade coil pipe condenser all communicate with temperature control equipment.

4. The novel glass reaction kettle structure according to claim 1, characterized in that: the dripping bottle (5) is connected with a continuous liquid feeding pipeline, and the tail end of the continuous liquid feeding pipeline is provided with a liquid feeding valve.

5. The novel glass reaction kettle structure according to claim 1, characterized in that: the glass pipeline (24) is provided with a three-way joint, and the liquid seal bottle (3) is communicated with the glass pipeline (24) through the three-way joint.

6. The novel glass reaction kettle structure according to claim 1, characterized in that: the two condensed distillation liquid receiving bottles (6) are provided, the air pressure balance ports of the two condensed distillation liquid receiving bottles are communicated with the lower port (42) of the secondary coil condenser (4), and receiving valves of the two condensed distillation liquid receiving bottles are communicated with the tail end of the glass pipeline (24).

7. The novel glass reaction kettle structure according to claim 1 or 6, characterized in that: and the condensed distilled liquid receiving bottle (6) is provided with a liquid discharge valve.

8. The novel glass reaction kettle structure according to claim 1, characterized in that: the center of the kettle cover (14) is provided with a stirring port (19), and the kettle cover (14) is also provided with an exhaust port (16), a feeding port (17) and a temperature measuring port (18).

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