Rectifying kettle-based ethyl alcohol recovery device for carbamazepine bromination process

Abstract

The utility model discloses a carbamazepine bromination process ethanol recovery device based on a rectifying still, and belongs to the technical field of chemical medicine recovery. The device comprises a preheating device, a rectification device, a steam temporary storage device and a heat exchange device, wherein the preheating device is arranged on a guide pipe on one side of the rectification device; the steam temporary storage device is arranged at the tail end of a steam pipe at the top end of the rectification device; the heat exchange device is connected to the lower portion of the steam temporary storage device through a guide pipe. On the basis that ethanol is obtained through rectification and purification of traditional equipment, heat brought by ethanol steam is guided into the preheating device again through the heat exchange device, ethanol mixed waste liquid is heated preliminarily, efficient recycling of the heat is achieved, and the operation cost of the whole equipment is reduced to a great extent.

Description

TECHNICAL FIELD

[0001] The utility model belongs to chemical medicine recovery technical field especially relates to a camphorated process ethanol recovery unit based on rectifying kettle. BACKGROUND

[0002] Camphorated process ethanol recovery unit based on rectifying kettle. + The mechanism of treating epilepsy is still unclear, which may be related to the increase of sodium channel inactivation efficiency, limiting the synaptic post-neuron and blocking the presynaptic Na 2+ channel, thereby limiting the firing of presynaptic and postsynaptic neuron action potential, blocking the release of excitatory neurotransmitters, reducing the excitability of nerve cells, and achieving the effect of anti-epilepsy; and the mechanism of anti-peripheral neuropathic pain may be related to Ca channel regulation. The chemical synthesis method of camphorated process in the prior art is from imino dibenzyl-gas (acyl chloride)-bromination-cyclization-gas-ammoniation to obtain camphorated process, which has many steps, complex process, large side effects, high cost and serious pollution.

[0003] Camphorated process ethanol recovery unit based on rectifying kettle.

[0004] Specifically, the refining process includes dissolving the crude camphorated process in ethanol, and then through the steps of reflux, pressure filtration, cooling crystallization, spin filtration, washing and drying, etc., to finally obtain pure camphorated process product. In this process, ethanol not only plays a role in dissolving the crude product, but also helps to remove impurities and improve the purity and quality of the product. Therefore, in the subsequent refining steps of camphorated process, ethanol is an important solvent and is widely used in the purification and refining process of camphorated process.

[0005] However, with the preparation of carbamazepine products, the ethanol mixture containing various impurities is often difficult to recycle, causing serious environmental pollution and increasing the cost of the entire process operation, and the existing technical means often uses ethanol rectification separation to separate and extract ethanol from the mixture. The basis of ethanol rectification separation is the difference in volatility of the components in the mixture, and the distillation is carried out in a distillation kettle. The essence of multi-tower distillation of ethanol is to repeat the single-tower operation on several complete or incomplete towers. In the ethanol-water two-component liquid mixture, after multiple partial vaporization and partial condensation, the ethanol with lower boiling point is obtained at the top of the tower, and the water with higher boiling point is obtained at the bottom of the tower. The more the number of separations, the higher the concentration of light components in the obtained gas phase product. Since ethanol and water can form azeotrope, the azeotrope point is 78.15℃, which ensures the feasibility of obtaining ethanol by rectification separation. Although the component purity of the extracted ethanol is greatly improved with the increase of the number of rectification, more heat is usually consumed, which will cause serious resource waste if not recycled, greatly increasing the operation cost of the process, and the investment and requirement of the equipment are also higher, which is difficult to realize industrial production.

[0006] Based on the fact that the existing technical means cannot effectively recycle ethanol in the carbamazepine bromination process waste liquid while reducing energy waste, an efficient and energy-saving ethanol recovery device is urgently needed. Practical new type content

[0007] The utility model discloses a kind of carbamazepine bromination process ethanol recovery devices based on rectification kettle, while improving ethanol recovery purity and efficiency, greatly reduce heat loss, reduce the cost of device operation.

[0008] To solve the above technical problems, the technical scheme adopted by the utility model is as follows:

[0009] A kind of carbamazepine bromination process ethanol recovery device based on rectification kettle, including preheating device, rectification device, steam temporary storage device and heat exchange device, the preheating device is placed on the guide pipe of the rectification device side;The steam temporary storage device is arranged at the end of the steam pipe at the top of the rectification device;The heat exchange device is connected below the steam temporary storage device by guide pipe.

[0010] Further, the preheating device upper end is connected with the cold water pipe of intercommunication heat exchange device, and the preheating device lower end is connected with the hot water pipe of intercommunication heat exchange device.

[0011] Further, the cold water pipe end close to heat exchange device is equipped with cold water pipe valve;The hot water pipe end close to heat exchange device is equipped with hot water pipe valve.

[0012] Further, the pre-heating device is arranged on the pipeline between the mixed liquid inlet and the rectifying device, and the mixed liquid inlet is provided with an inlet valve.

[0013] Further, the rectifying device is provided with a waste liquid outlet near the bottom, and the waste liquid outlet is provided with a waste liquid outlet valve.

[0014] Further, the heat exchange device comprises a condenser and a heat pump, and the heat pump is composed of an evaporator, a compressor and a heat pipe heat exchanger.

[0015] Further, the bottom of the heat exchange device is provided with a liquid outlet, and the liquid outlet is provided with a liquid outlet valve.

[0016] Compared with the prior art, the utility model has the following advantages:

[0017] (1) the utility model discloses a pre-heating device is arranged before the ethanol mixed waste liquid enters the rectifying device, can utilize the heat of subsequent ethanol steam liquefaction condensation heat exchange and carries out pre-heating treatment to ethanol mixed waste liquid, greatly reduces the supply and consumption of rectification process heat.

[0018] (2) the utility model discloses a steam temporary storage device, can buffer the ethanol steam evaporated by the rectifying device, balances the airflow, prevents the reflux of ethanol steam, causes the reduction of distillation efficiency.

[0019] (3) the utility model discloses a heat exchange device and carries out preliminary heating to ethanol mixed waste liquid by the heat brought by ethanol steam and re-lead into the pre-heating device, realizes the efficient recycling of heat.

[0020] (4) the utility model discloses the laying of special cold water pipe and hot water pipe, connects the heat exchange device and the pre-heating device, and adjusts the water flow while controlling the efficiency of heat exchange through the opening degree of corresponding valve. DRAWINGS

[0021] Figure 1 It is the whole structure schematic diagram of the utility model;

[0022] Figure 2 It is the pre-heating device sectional structure drawing of the utility model;

[0023] Figure 3 It is the device schematic drawing that the heat exchange device comprises.

[0024] The drawing mark is: 1, mixed liquid inlet;2, inlet valve;3, pre-heating device;4, cold water pipe;5, steam pipe;6, steam temporary storage device;7, cold water pipe valve;8, heat exchange device;9, liquid outlet valve;10, liquid outlet;11, hot water pipe valve;12, hot water pipe;13, rectifying device;14, waste liquid outlet valve;15, waste liquid outlet. DETAILED DESCRIPTION

[0025] The utility model will be further explained in connection with the drawings.

[0026] Please refer to Figure 1 and Figure 2 A kind of carbamazepine bromination process ethanol recovery device based on rectifying kettle, it mainly includes preheating device 3, rectifying device 13, steam temporary storage device 6 and heat exchange device 8.

[0027] Preheating device 3 is arranged on the pipeline between rectifying device 13 and mixed liquid inlet 1, and the upper and lower ends of preheating device 3 are connected with cold water pipe 4 and hot water pipe 12 respectively.The left side of rectifying device 13 is connected with pipeline, and the other end of the pipeline is mixed liquid inlet 1, and inlet valve 2 is arranged on mixed liquid inlet 1;Waste liquid outlet valve 14 is arranged on waste liquid outlet 15, which is arranged at the position close to the bottom of the right side of rectifying device 13;The upper end of rectifying device 13 is provided with steam pipe 5, and the structure of steam pipe 5 is wide at the bottom and narrow at the top, which is conducive to the conduction and collection of steam.Steam temporary storage device 6 is arranged at the end of steam pipe 5, which is used to buffer the ethanol steam evaporated by rectifying device 13, balance the airflow, prevent the reflux of ethanol steam, and cause the reduction of distillation efficiency;The bottom of steam temporary storage device 6 is provided with the guide pipe connected with heat exchange device 8, which can directly guide the buffered ethanol steam into heat exchange device 8 through the guide pipe for subsequent condensation collection and heat recovery.

[0028] As Figure 3As shown, the heat exchange device 8 includes a condenser, an evaporator, a compressor and a heat pipe heat exchanger. The upper end of the heat exchange device 8 is provided with a conduit connected to the steam temporary storage device 6 and a cold water pipe 4, one end of the cold water pipe 4 is connected to the heat exchange device 8, the other end is connected to the upper end of the preheating device 3, and the end of the cold water pipe 4 close to the heat exchange device 8 is provided with a cold water pipe valve 7. By opening and closing the cold water pipe valve 7 and the working of the evaporator and the compressor in the heat exchange device 8, the flow of condensed water from the preheating device 3 into the heat exchange device 8 can be adjusted, thereby realizing the rapid condensation of ethanol vapor; the lower end of the heat exchange device 8 is provided with a hot water pipe 12 and a liquid outlet 10, one end of the hot water pipe 12 is connected to the heat exchange device 8, the other end is connected to the lower end of the preheating device 3, and the end of the hot water pipe 12 close to the heat exchange device 8 is provided with a hot water pipe valve 11. By opening and closing the hot water pipe valve 11 and the working of the evaporator and the compressor in the heat exchange device 8, the flow of hot water from the heat exchange device 8 into the preheating device 3 can be adjusted. On the one hand, it can preliminarily heat the mixed liquid entering the rectification device 13 through the mixed liquid inlet 1, thereby reducing the energy input required for rectification; on the other hand, it can realize the dynamic circulation between the condensed water in the heat exchange device 8 and the hot water obtained by heat exchange, thereby greatly improving the heat recovery efficiency. The liquid outlet 10 is arranged at the bottom end of the heat exchange device 8, and the liquid outlet 10 is provided with a liquid outlet valve 9. By opening and closing the liquid outlet valve 9, the liquid ethanol can be recovered.

[0029] The device, the conduit and the material contact part of the device are all made of stainless steel SUS304 or SUS316L, the outer surface of the equipment is treated to be matte, meets the GMP pharmaceutical standard, has good chemical corrosion resistance, and has the advantages of energy saving, environmental protection, reduced production cost and improved efficiency.

[0030] As a preferred embodiment of the utility model, the rectification device 13 can be replaced by a rectification tower to further improve the rectification efficiency.

[0031] As a preferred embodiment of the utility model, a plurality of heat exchangers (by parallel connection or series-parallel connection, a plurality of condensers, evaporators, compressors and heat pipe heat exchangers are reasonably arranged) can be arranged in the heat exchange device 8 for rapid condensation of ethanol vapor and staged recovery of heat.

[0032] The working principle of the utility model is as follows: along with the carrying out of carbamazepine bromination process, the ethanol mixed solution containing various impurities is collected, at this time, only need to open the inlet valve 2 (the initial state is not explained, other valves are in the closed state by default), the ethanol mixed solution containing various impurities will be introduced into the rectification device 13 from the mixed solution inlet 1 along the pipe, in this process, because the preheating device 3 is arranged on the pipe between the mixed solution inlet 1 and the rectification device 13, so the ethanol mixed solution containing various impurities is preliminarily heated (generally can be heated to 45-55 DEG C), the initial temperature of the ethanol mixed solution in the rectification device 13 is greatly improved, which greatly reduces the heat supply and loss in the rectification stage. Along with the normal operation of the rectification device 13, the temperature of the ethanol mixed solution gradually rises, and the ethanol in the mixed solution is easy to volatilize from the mixed solution, the volatilized ethanol gas will pass through the steam pipe 5 to reach the steam temporary storage device 6, and then be transmitted to the heat exchange device 8 through the pipe at the lower end of the steam temporary storage device 6, when the temperature reaches 78.3 DEG C, the ethanol in the mixed solution will form ethanol steam, a large amount of ethanol steam will quickly enter the steam temporary storage device 6 through the steam pipe 5, and the ethanol steam will be transmitted to the heat exchange device 8 through the pipe at the lower end of the steam temporary storage device 6 after the buffering action of the steam temporary storage device 6, avoiding the liquefied reflux of most of the ethanol steam, which leads to the extension of the rectification time and the reduction of the efficiency. The mixed waste liquid after distillation of ethanol will be discharged from the waste liquid outlet 15 through the opening of the waste liquid outlet valve 14. The ethanol steam enters the heat exchange device 8, is quickly condensed by the condenser and the heat is recovered by the heat pump (evaporator, compressor and heat pipe heat exchanger) first, and then the ethanol steam is quickly liquefied to form ethanol solution, at this time, the liquid valve 9 is opened, and the liquefied ethanol solution finally flows out from the liquid outlet 10 and is collected. Along with the continuous reaction, the cold water pipe valve 7 and the hot water pipe valve 11 are opened, and the condensate water temperature after heat exchange rises to become hot water, in order to avoid excessive loss of the heat, the hot water obtained after heat exchange is introduced into the preheating device 3 from the hot water pipe 12 (that is, the heat is transferred from the heat exchange device 8 to the preheating device 3), which provides a heat source for the preheating device 3 and is used for the preliminary heating of the ethanol mixed solution. The cold water from the preheating device 3 is introduced into the heat exchange device 8 again along the cold water pipe 4 to condense and heat the ethanol steam again, so that the circulation of the condensate water-hot water-condensate water and the recycling of the heat are realized, and the heat recovery efficiency of the whole device is greatly improved.

[0033] The above only describes the preferred embodiments of the utility model and is not used to limit the utility model, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model should be included in the protection scope of the utility model.

Claims

1. A distillation kettle based carbamazepine bromination process ethanol recovery apparatus, characterized by, The pre-heating device (3) is arranged on the pipe on one side of the rectifying device (13); the steam temporary storage device (6) is arranged at the end of the steam pipe (5) at the top end of the rectifying device (13); the heat exchange device (8) is connected below the steam temporary storage device (6) through a pipe.

2. The ethanol recovery unit based on rectification kettle for the bromination process of carbamazepine according to claim 1, characterized in that, The upper end of the pre-heating device (3) is connected with the cold water pipe (4) communicating with the heat exchange device (8), and the lower end of the pre-heating device (3) is connected with the hot water pipe (12) communicating with the heat exchange device (8).

3. The ethanol recovery unit based on rectifier stills for the bromination process of carbamazepine according to claim 2, characterized in that, The cold water pipe (4) is provided with a cold water pipe valve (7) at one end close to the heat exchange device (8); the hot water pipe (12) is provided with a hot water pipe valve (11) at one end close to the heat exchange device (8).

4. The ethanol recovery unit based on rectifier stills for the bromination process of carbamazepine according to claim 1, characterized in that, The pre-heating device (3) is arranged on the pipe between the mixed liquid inlet (1) and the rectifying device (13), and the mixed liquid inlet (1) is provided with an inlet valve (2).

5. The ethanol recovery unit based on rectifier stills for the bromination process of carbamazepine according to claim 1, characterized in that, The rectifying device (13) is provided with a waste liquid outlet (15) close to the bottom on one side, and the waste liquid outlet (15) is provided with a waste liquid outlet valve (14).

6. The ethanol recovery unit based on rectifier stills for the bromination process of carbamazepine according to claim 1, characterized in that, The heat exchange device (8) comprises a condenser and a heat pump; the heat pump is composed of an evaporator, a compressor and a heat pipe heat exchanger.

7. The ethanol recovery unit based on rectifier kettle for the bromination process of carbamazepine according to claim 1, characterized in that, The bottom of the heat exchange device (8) is provided with a liquid outlet (10); the liquid outlet (10) is provided with a liquid outlet valve (9).

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