Purifying and recrystallizing system for m-bromobenzoic acid crude product

Abstract

The utility model provides a purification and recrystallization system for crude m-bromobenzoic acid. The purification and recrystallization system comprises a kettle body, a stirring assembly and a heat exchange jacket, the kettle body comprises a dissolving part, a filtering part and a recrystallization part from top to bottom; the dissolving part is provided with a feeding hole, a solvent inlet, an exhaust hole I and a pressurizing hole; a filtering component is arranged in the filtering part, and an exhaust port II is formed in the side wall; a discharge port is formed in the bottom of the recrystallization part, and a volatilization port is formed in the side wall; an inner cavity of the dissolving part is communicated with an inner cavity, positioned above the filtering assembly, of the filtering part through a feed liquid transfer pipe provided with a valve; an inner cavity, positioned below the filtering assembly, of the filtering part is communicated with an inner cavity of the recrystallization part through a filtrate outlet; the stirring assembly is used for stirring the m-bromobenzoic acid crude product purification and recrystallization system in the inner cavities of the dissolving part and the recrystallization part; heat exchange jackets are arranged on the outer wall of the dissolving part and the outer wall of the recrystallization part. The m-bromobenzoic acid crude product purification and recrystallization system disclosed by the utility model is reasonable in structural design, high in integration degree and small in occupied area.

Description

Technical Field

[0001] The utility model belongs to the technical field of meta-bromobenzoic acid purification, in particular to a meta-bromobenzoic acid crude product purification and recrystallization system. Background Art

[0002] Meta-bromobenzoic acid is a very important chemical intermediate. It is widely used in analytical testing, organic synthesis and pharmaceutical intermediates, curing accelerators and fire retardant additives in the plastics industry, and adhesives for photographic materials.

[0003] Synthesized meta-bromobenzoic acid is generally a crude product with low purity, and needs to be further purified by recrystallization. Recrystallization is the process of completely dissolving a substance in a solvent and then recrystallizing it from a clear solution. The process of recrystallization of crude meta-bromobenzoic acid is generally to add crude meta-bromobenzoic acid to a solvent, add an appropriate amount of activated carbon, heat and stir until completely dissolved, then filter, collect the filtrate, heat the filtrate to fully dissolve it, and then cool and recrystallize it to obtain a purified product. The existing recrystallization system has an unreasonable structural design, generally includes multiple devices, which are dispersed, have a low degree of integration, occupy a large area, need to be transferred between several devices during the working process, and have a large workload. Utility Model Content

[0004] In view of this, in order to solve the above technical problems, the utility model proposes a crude meta-bromobenzoic acid purification and recrystallization system with reasonable structural design, high degree of integration and small footprint.

[0005] In order to achieve the above object, the technical solution of the utility model is implemented as follows:

[0006] A crude meta-bromobenzoic acid purification and recrystallization system, comprising:

[0007] A kettle body, the kettle body comprising a dissolving part, a filtering part and a recrystallization part arranged concentrically from top to bottom; the top of the dissolving part is provided with a feed port, a solvent inlet, an exhaust port 1 and a pressurizing port connected to its inner cavity; the inner cavity of the filtering part is provided with a horizontally arranged filtering assembly, and the upper end of the side wall is provided with an exhaust port 2; the bottom of the recrystallization part is provided with a discharge port, and the upper end of the side wall is provided with a volatilization port; the inner cavity of the dissolving part is connected with the inner cavity of the filtering part located above the filtering assembly through a feed liquid transfer pipe provided with a valve; the inner cavity of the filtering part located below the filtering assembly is connected with the inner cavity of the recrystallization part through a filtrate discharge port;

[0008] A stirring component, the stirring component is used to stir the materials in the inner cavities of the dissolution part and the recrystallization part;

[0009] A heat exchange jacket is provided on the outer wall of the dissolution part and the outer wall of the recrystallization part.

[0010] The dissolution section, the filtration section and the recrystallization section are stacked in sequence, the crude meta-bromobenzoic acid and the solvent are added into the dissolution section, the stirring component is stirred, the heat exchange jacket heats up the dissolution section, after the crude meta-bromobenzoic acid is dissolved, the material-liquid transfer pipe is opened, the solution is transferred to the filtration section under the action of gravity, or the solution is transferred to the filtration section by pressurizing the pressure port, the solution is filtered through the filtration component, the filtrate falls into the recrystallization section, the stirring component is stirred, the heat exchange jacket heats up the recrystallization section, the filtrate is fully dissolved, the heat exchange jacket cools down the recrystallization section, the recrystallized meta-bromobenzoic acid is obtained and discharged through the discharge port; the dissolution, filtration and recrystallization processes are concentrated on the same equipment, which reduces the floor space and is more centralized, while reducing the frequency of material transfer between different equipment through pipelines or manual work, thereby reducing the workload.

[0011] Furthermore, the dissolving part, the filtering part and the recrystallization part are all connected detachably by means of ear plates provided with sealing gaskets and then locked and fixed by bolts.

[0012] In order to facilitate maintenance, the dissolution part, filtration part and recrystallization part are connected in a detachable manner.

[0013] Furthermore, a circle of mounting seats is provided on the inner side wall of the filter portion along the circumferential direction; the filter assembly includes an outer ring detachably mounted on the mounting seat and a filter layer fixed inside the outer ring.

[0014] Furthermore, one end of the liquid transfer pipe is connected to the inner cavity at the bottom end of the side wall of the dissolving part, and the other end is connected to the inner cavity of the filtering part located above the filtering component.

[0015] The liquid transfer tube can transfer the solution in the dissolving part to the filtering part. The solution can be transferred by gravity, or it can be connected to a pressurized gas supply device through the pressurizing port to pressurize the inner cavity of the dissolving part and pressurize the solution into the filtering part to speed up the solution transfer efficiency.

[0016] Furthermore, the stirring assembly includes a driving motor arranged on the outer top of the dissolution section, a stirring rod which sequentially passes through the dissolution section and the filtration section and extends into the recrystallization section, a stirring paddle 1 arranged on the stirring rod and located in the inner cavity of the dissolution section, and a stirring paddle 2 located in the inner cavity of the recrystallization section.

[0017] A driving motor is provided to drive the stirring paddle 1 and the stirring paddle 2 at the same time, thereby reducing the number of equipment settings and reducing investment costs without affecting the stirring effect.

[0018] Furthermore, a through hole is provided on the bottom plate of the dissolution section for the stirring rod to pass through, and the through hole is rotatably sealed and connected to the stirring rod via a rotating sealing bearing, so that the solution cannot flow into the filtration section from the through hole; a sleeve is provided on the filtration assembly for the stirring rod to pass through, and the sleeve is rotatably sealed and connected to the stirring rod via a rotating sealing bearing, so that the solution cannot flow into the recrystallization section from the sleeve.

[0019] Furthermore, the heat exchange jacket includes a jacket 1 arranged on the outer wall of the dissolution section and a jacket 2 arranged on the outer wall of the recrystallization section; the jacket 1 is provided with a heat medium inlet 1 and a heat medium outlet 1; the jacket 2 is provided with a heat medium inlet 2, a cold medium inlet, a heat medium outlet 2 and a cold medium outlet.

[0020] The dissolution section only involves temperature rise and dissolution, so the jacket is provided with a heat medium inlet 1 and a heat medium outlet 1; the recrystallization section involves temperature rise and temperature drop, so the jacket is provided with a heat medium inlet 2, a cold medium inlet, a heat medium outlet 2 and a cold medium outlet.

[0021] Compared with the prior art, the crude meta-bromobenzoic acid purification and recrystallization system described in the utility model has the following advantages:

[0022] The crude meta-bromobenzoic acid purification and recrystallization system of the utility model integrates the dissolution, filtration and recrystallization processes on the same equipment through reasonable structural design, realizes the centralization of the dissolution part, the filtration part and the recrystallization part, reduces the floor space, and has a high degree of integration. At the same time, during the recrystallization purification process, there is no need to transfer materials between different equipment through pipelines or manually, thereby reducing the workload. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The accompanying drawings constituting a part of the present invention are used to provide a further understanding of the present invention. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation on the present invention. In the accompanying drawings:

[0024] Figure 1 This is a schematic structural diagram of the crude meta-bromobenzoic acid purification and recrystallization system described in an embodiment of the utility model.

[0025] Description of reference numerals:

[0026] 1-dissolving part, 2-filtering part, 3-recrystallization part, 4-ear plate, 5-feeding port, 6-solvent inlet, 7-exhaust port one, 8-pressurization port, 9-filtering component, 10-exhaust port two, 11-mounting seat, 12-discharge port, 13-volatile port, 14-feed liquid transfer pipe, 15-filtrate discharge port, 16-driving motor, 17-stirring rod, 18-stirring paddle one, 19-stirring paddle two, 20-rotating sealing bearing, 21-sleeve, 22-jacket one, 23-jacket two, 24-heat medium inlet one, 25-heat medium outlet one, 26-heat medium inlet two, 27-refrigerant inlet, 28-heat medium outlet two, 29-refrigerant outlet. DETAILED DESCRIPTION

[0027] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.

[0028] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0029] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood by specific circumstances.

[0030] The present invention will be described in detail below with reference to the accompanying drawings and in combination with embodiments.

[0031] like Figure 1 As shown,

[0032] A system for purifying and recrystallizing crude meta-bromobenzoic acid comprises a kettle, a stirring assembly, and a heat exchange jacket;

[0033] The kettle body includes a dissolving part 1, a filtering part 2 and a recrystallization part 3 which are arranged concentrically from top to bottom; the dissolving part 1, the filtering part 2 and the recrystallization part 3 are connected by an ear plate 4 provided with a sealing gasket, and then are detachably connected by bolts for locking and fixing; the top of the dissolving part 1 is provided with a feed port 5, a solvent inlet 6, an exhaust port 7 and a pressurizing port 8 which are connected to its inner cavity; the inner cavity of the filtering part 2 is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with an exhaust port 10; the inner cavity of the filtering part 2 is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with an exhaust port 10; the inner cavity of the filtering part 2 is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with an exhaust port 10; the inner cavity of the filtering part 2 is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with a horizontally arranged filter assembly 9, and ... upper end of the side wall is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with a horizontally arranged filter assembly 9, and the upper end of the side wall is provided with a A circle of mounting seats 11 is provided on the side wall along the circumferential direction, and the filter assembly 9 includes an outer ring detachably mounted on the mounting seat 11 and a filter layer fixed in the outer ring; a discharge port 12 is provided at the bottom of the recrystallization part 3, and a volatilization port 13 is provided at the upper end of the side wall; the inner cavity at the bottom end of the side wall of the dissolution part 1 is connected with the inner cavity of the filter part 2 located above the filter assembly 9 through a feed liquid transfer pipe 14 provided with a valve; the inner cavity of the filter part 2 located below the filter assembly 9 is connected with the inner cavity of the recrystallization part 3 through a filtrate discharge port 15;

[0034] The stirring assembly includes a driving motor 16 arranged at the outer top of the dissolving part 1, a stirring rod 17 which sequentially penetrates the dissolving part 1 and the filtering part 2 and extends into the recrystallization part 3, a stirring paddle 18 arranged on the stirring rod 17 and located in the inner cavity of the dissolving part 1, and a stirring paddle 2 19 located in the inner cavity of the recrystallization part 3; a through hole for the stirring rod 17 to pass through is provided on the bottom plate of the dissolving part 1, and the through hole is rotatably sealed and connected to the stirring rod 17 through a rotating sealing bearing 20; a sleeve 21 for the stirring rod 17 to pass through is provided on the filtering assembly 9, and the sleeve 21 is rotatably sealed and connected to the stirring rod through a rotating sealing bearing 20;

[0035] The heat exchange jacket comprises a jacket 1 22 arranged on the outer wall of the dissolution part 1 and a jacket 2 23 arranged on the outer wall of the recrystallization part 3; the jacket 1 22 is provided with a heat medium inlet 1 24 and a heat medium outlet 1 25; the jacket 2 23 is provided with a heat medium inlet 26, a cold medium inlet 27, a heat medium outlet 28 and a cold medium outlet 29.

[0036] The working process of the crude meta-bromobenzoic acid purification and recrystallization system described in the utility model is as follows:

[0037] Add crude meta-bromobenzoic acid, solvent and activated carbon into the dissolution section, inject heat medium into jacket one to heat the material in the dissolution section, stir with stirring paddle one to dissolve the crude meta-bromobenzoic acid and obtain a solution; open the material-liquid transfer pipe, pressurize the dissolution section through the pressure port to transfer the solution to the filtration section, filter the solution through the filtration component, and let the filtrate fall into the recrystallization section; inject heat medium into jacket two to heat the material in the recrystallization section, stir with stirring paddle two to fully dissolve the meta-bromobenzoic acid; cool down after dissolution, pass cold medium into jacket two, cool down the recrystallization section, start crystallization, and after the crystallization is completed, discharge the material from the discharge port and send it to the next process.

[0038] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A system for purifying and recrystallizing crude meta-bromobenzoic acid, characterized in that: include: A kettle body, the kettle body comprising a dissolving part, a filtering part and a recrystallization part arranged concentrically from top to bottom; the top of the dissolving part is provided with a feed port, a solvent inlet, an exhaust port 1 and a pressurizing port connected to its inner cavity; the inner cavity of the filtering part is provided with a horizontally arranged filtering assembly, and the upper end of the side wall is provided with an exhaust port 2; the bottom of the recrystallization part is provided with a discharge port, and the upper end of the side wall is provided with a volatilization port; the inner cavity of the dissolving part is connected with the inner cavity of the filtering part located above the filtering assembly through a feed liquid transfer pipe provided with a valve; the inner cavity of the filtering part located below the filtering assembly is connected with the inner cavity of the recrystallization part through a filtrate discharge port; A stirring component, the stirring component is used to stir the materials in the inner cavities of the dissolution part and the recrystallization part; A heat exchange jacket is provided on the outer wall of the dissolution part and the outer wall of the recrystallization part.

2. The crude meta-bromobenzoic acid purification and recrystallization system according to claim 1, characterized in that: The dissolving part, the filtering part and the recrystallization part are all connected detachably by means of ear plates provided with sealing gaskets and then locked and fixed by bolts.

3. The crude meta-bromobenzoic acid purification and recrystallization system according to claim 2, characterized in that: A circle of mounting seats is arranged on the inner side wall of the filter part along the circumferential direction; the filter assembly comprises an outer ring detachably mounted on the mounting seat and a filter layer fixed inside the outer ring.

4. The crude meta-bromobenzoic acid purification and recrystallization system according to claim 1, characterized in that: One end of the liquid transfer pipe is connected to the inner cavity at the bottom end of the side wall of the dissolving part, and the other end is communicated with the inner cavity of the filtering part located above the filtering component.

5. The system for purifying and recrystallizing crude meta-bromobenzoic acid according to any one of claims 1 to 4, characterized in that: The stirring assembly includes a driving motor arranged at the outer top of the dissolution section, a stirring rod which sequentially passes through the dissolution section and the filtering section and extends into the recrystallization section, a stirring paddle 1 arranged on the stirring rod and located in the inner cavity of the dissolution section, and a stirring paddle 2 located in the inner cavity of the recrystallization section.

6. The crude meta-bromobenzoic acid purification and recrystallization system according to claim 5, characterized in that: A through hole is provided on the bottom plate of the dissolving part for the stirring rod to pass through, and the through hole is rotatably sealed and connected to the stirring rod via a rotating sealing bearing; a sleeve is provided on the filtering assembly for the stirring rod to pass through, and the sleeve is rotatably sealed and connected to the stirring rod via a rotating sealing bearing.

7. The system for purifying and recrystallizing crude meta-bromobenzoic acid according to any one of claims 1 to 4, characterized in that: The heat exchange jacket comprises a jacket 1 arranged on the outer wall of the dissolution part and a jacket 2 arranged on the outer wall of the recrystallization part; the jacket 1 is provided with a heat medium inlet 1 and a heat medium outlet 1; the jacket 2 is provided with a heat medium inlet 2, a cold medium inlet, a heat medium outlet 2 and a cold medium outlet.

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