Device for recovering thionyl chloride by distillation method

Abstract

The utility model relates to the technical field of propionyl chloride preparation, in particular to a device for recovering thionyl chloride by a distillation method, which comprises a distillation kettle, a connecting pipe, a filter box, a filter screen filter, a deep filter, a head tank and a distillation recovery component. According to the utility model, through the arrangement of the filter box, the filter screen filter and the deep filter, a thionyl chloride solution containing impurities firstly passes through the filter screen filter to remove larger particles, and then passes through the deep filter to remove tiny solid impurities, so that the purity of raw materials entering the distillation kettle is ensured, and the interference of the impurities on the distillation effect is reduced; the material conveying is smoother, so that the distillation efficiency is improved and the energy consumption is reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to propionyl chloride preparation field technical field especially relates to a device of distillation method recovery of thionyl chloride. BACKGROUND

[0002] Thionyl chloride is a colorless or yellow liquid with a strong irritating odor, and has a certain toxicity. Its toxicity is greater than that of sulfur dioxide, and may irritate the eyes and respiratory system when in contact with the human body, and may cause edema and burns in severe cases. Therefore, in the preparation of propionyl chloride, in addition to providing necessary protective measures for workers, the leakage of thionyl chloride should also be reduced from the source.

[0003] The traditional thionyl chloride recovery process mostly uses distillation method, which aims to separate and purify thionyl chloride from the mixed system by utilizing the difference in boiling point of thionyl chloride and other substances, so as to realize the reuse of resources and reduce production cost. The existing distillation recovery device usually focuses on the design optimization of core components such as distillation column, condenser and receiver, so as to improve the distillation efficiency and product purity.

[0004] However, the device for adding thionyl chloride widely used at present has a significant defect, i.e. no filter assembly is provided. In the actual production process, the thionyl chloride to be recovered has complex sources, which not only contains unreacted raw materials and by-products, but also often contains solid impurities such as dust, metal scraps and polymer particles. When these thionyl chloride containing impurities directly enter the distillation system, it will cause the reduction of pipeline flow area and the increase of fluid resistance, so that the material transportation in the distillation system is not smooth, thereby reducing the distillation efficiency and increasing the energy consumption. UTILITY MODEL CONTENTS

[0005] The utility model aims at solving the defect that the existing device for adding thionyl chloride does not provide filter assembly, so that when the thionyl chloride containing impurities directly enters the distillation system, it will cause the reduction of pipeline flow area and the increase of fluid resistance, so that the material transportation in the distillation system is not smooth, thereby reducing the distillation efficiency and increasing the energy consumption, and proposes a device for recovering thionyl chloride by distillation method.

[0006] In order to achieve the above purpose, the utility model adopts the following technical scheme:

[0007] A device for recovering thionyl chloride by distillation method, comprising a distillation kettle placed on the ground, a connection pipe in symmetrical distribution is connected through the top end of the distillation kettle, a filter box is arranged at the top end of the connection pipe, a filter screen filter and a deep filter are arranged in the filter box from top to bottom, a high tank is arranged above the filter box, a valve is arranged on the connection pipe, and a distillation recovery assembly capable of distilling thionyl chloride is further arranged on the distillation kettle.

[0008] Preferably, mounting grooves are symmetrically arranged on the outer wall of the filter box, and the filter screen filter and the deep filter are both provided with sealing covers at the outward ends.

[0009] Preferably, the filter screen filter and the deep filter are both in sliding connection with the mounting grooves, and the sealing covers are in sliding connection with the mounting grooves.

[0010] Preferably, the distillation recovery assembly comprises a thermometer, a pressure gauge, a material conveying pipe, a vacuum pump, a flow meter, an extension strip, a circular arc groove, a steam recovery pipe, a shunt pipe, a condenser and a recovery bucket, the thermometer is arranged on the outer wall of the distillation kettle, and the pressure gauge is arranged at the top end of the distillation kettle.

[0011] Preferably, the material conveying pipe is in sealed connection with the connecting pipe, the vacuum pump is placed on the ground and connected with the material conveying pipe, and the flow meter is arranged on the vacuum pump.

[0012] Preferably, the extension strip is fixedly connected with the inner wall of the end cover of the distillation kettle, the circular arc groove is arranged at the top end of the extension strip, the steam recovery pipe is in through connection with the top end of the distillation kettle, one end of the shunt pipe is in through connection with the steam recovery pipe, the condenser is arranged on the outer wall of the distillation kettle, and the recovery bucket is placed on the ground and connected with the condenser through a water pipe.

[0013] Compared with the prior art, the distillation method for recovering thionyl chloride provided by the utility model has the advantages that:

[0014] 1. When the utility model is used, the filter box, the filter screen filter and the deep filter are arranged, so that the thionyl chloride solution containing impurities can first be removed of large particles by the filter screen filter and then be removed of small solid impurities by the deep filter, the purity of the raw material entering the distillation kettle is ensured, the interference of impurities on the distillation effect is reduced, the impurities are prevented from entering the distillation system, the material conveying is more smooth, the distillation efficiency is improved, and the energy consumption is reduced.

[0015] 2. When the utility model is used, a certain amount of diethylene glycol can be poured from the raw material tank into the reaction kettle by using the vacuum pump and the flow meter interlocking, the temperature in the reaction kettle can be kept in a proper interval, the thionyl chloride can be added dropwise into the reaction kettle through the high tank, the main method for recovering thionyl chloride is distillation, the thionyl chloride is recovered when the temperature in the reaction kettle is 79 DEG C by taking advantage of the low boiling point (79 DEG C) of the thionyl chloride, but the thionyl chloride is prone to disproportionation reaction or explosion when the temperature is too high, therefore, the key to recovering the thionyl chloride by using the distillation method lies in controlling the temperature between 79 DEG C and 90 DEG C. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 A perspective structural schematic view of the device for recovering thionyl chloride by using the distillation method is provided in the utility model.

[0017] Figure 2 The utility model provides a kind of back three-dimensional structure schematic diagram of device for recovering thionyl chloride by distillation is proposed in the utility model;

[0018] Figure 3 A kind of half cut three-dimensional structure schematic diagram of device for recovering thionyl chloride by distillation is proposed in the utility model

[0019] Figure 4 A kind of filter box internal three-dimensional structure schematic diagram of device for recovering thionyl chloride by distillation is proposed in the utility model.

[0020] In the drawing: 1, distillation kettle;2, connecting pipe;3, filter box;4, screen filter;5, deep filter;6, high tank;7, valve;8, distillation recovery component;9, mounting groove;10, sealing cover;11, thermometer;12, pressure gauge;13, feed pipe;14, vacuum pump;15, flowmeter;16, extension bar;17, circular arc groove;18, steam recovery pipe;19, shunt pipe;20, condenser;21, recovery bucket. DETAILED DESCRIPTION

[0021] The technical scheme in the embodiments of the utility model will be described clearly and completely below with reference to the drawings in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of the utility model.

[0022] Refer to Figures 1-4 A kind of device for recovering thionyl chloride by distillation, including the distillation kettle 1 placed on ground, the top end of the distillation kettle 1 is connected with the connecting pipe 2 being symmetrically distributed, the top end of the connecting pipe 2 is provided with the filter box 3, the inside of the filter box 3 is provided with screen filter 4 and deep filter 5 from top to bottom respectively, the top of the filter box 3 is provided with high tank 6, the connecting pipe 2 is provided with valve 7, the distillation kettle 1 is also provided with the distillation recovery component 8 capable of distilling thionyl chloride.

[0023] It should be noted that distillation kettle 1, thermometer 11, pressure gauge 12, vacuum pump 14, flowmeter 15, condenser 20 are prior art, and specific model specification needs to be selected and determined according to the actual specification of the device, and the specific selection calculation method adopts the prior art in the art, so it is not described in detail.

[0024] Further, mounting groove 9 is formed on the outer wall of filter box 3 in a symmetrical distribution, and the outward end of screen filter 4 and deep filter 5 is provided with sealing cover 10.

[0025] The deep filter 5 is made of polytetrafluoroethylene material, can resist the corrosion of thionyl chloride and various organic solvents, and will not react with raw materials during the filtering process, thereby ensuring the purity and effect of the filtering.

[0026] Further, the filter screen filter 4 and the deep filter 5 are in sliding connection with the mounting groove 9, and the sealing cover 10 is in sliding connection with the mounting groove 9.

[0027] The top end of the filter screen filter 4 and the deep filter 5 is provided with a downward groove, so that the impurities after filtering can be left in the groove, and when taking out for cleaning, the impurities will not be affected by the mounting groove 9, causing the impurities to remain in the filter box 3.

[0028] Further, the distillation recovery assembly 8 includes a thermometer 11, a pressure gauge 12, a feed pipe 13, a vacuum pump 14, a flow meter 15, an extension bar 16, a circular arc groove 17, a steam recovery pipe 18, a shunt pipe 19, a condenser 20, and a recovery barrel 21. The thermometer 11 is arranged on the outer wall of the distillation kettle 1, and the pressure gauge 12 is arranged at the top end of the distillation kettle 1.

[0029] The thermometer 11 is used to observe and record the temperature inside the distillation kettle 1, and the pressure gauge 12 is used to observe the pressure inside the distillation kettle 1, so that the distillation reaction can be carried out more safely.

[0030] Further, the feed pipe 13 is in sealed connection with the connecting pipe 2, the vacuum pump 14 is placed on the ground and connected with the feed pipe 13, and the flow meter 15 is arranged on the vacuum pump 14.

[0031] The vacuum pump 14 can extract the gas inside the distillation kettle 1 to create the conditions for reduced pressure distillation, and the flow meter 15 can clearly see the mass of the gas extracted by the vacuum pump 14, so as to control the pressure inside the distillation kettle 1.

[0032] Further, the extension bar 16 is fixedly connected with the inner wall of the end cover of the distillation kettle 1, the circular arc groove 17 is arranged at the top end of the extension bar 16, the steam recovery pipe 18 is in through connection with the top end of the distillation kettle 1, one end of the shunt pipe 19 is in through connection with the steam recovery pipe 18, the condenser 20 is arranged on the outer wall of the distillation kettle 1, and the recovery barrel 21 is placed on the ground and connected with the condenser 20 through a water pipe.

[0033] The steam recovery pipe 18 is connected with the condenser 20, when the thionyl chloride vaporizes and starts to be recovered, at this time, nitrogen is injected into the distillation kettle 1, the thionyl chloride gas can be protected from contacting with water molecules in the air by the nitrogen, the occurrence of the side reaction is avoided, the other end of the shunt pipe 19 is penetrated with the outer wall of the distillation kettle 1 and the lowest part of the circular arc groove 17, so that the thionyl chloride solution gathered in the circular arc groove 17 can be concentrated and discharged into the steam recovery pipe 18, the recovery efficiency is further improved.

[0034] Working principle: when the device is used, firstly, the thionyl chloride solution is added into the high tank 6, the thionyl chloride solution flows downwards into the filter box 3 under the influence of gravity, and is filtered through the filter screen filter 4 and the deep filter 5 in turn, then the valve 7 is opened to fall into the distillation kettle 1, the filter screen filter 4 and the deep filter 5 can be taken out for cleaning through the sealing cover 10; when distillation recovery is carried out, the temperature and pressure of the distillation kettle 1 can be accurately controlled through the thermometer 11 and the pressure gauge 12, when the thionyl chloride solution is vaporized into steam and floats upwards at 79 DEG C, the steam enters the condenser 20 through the steam recovery pipe 18, is condensed into liquid and is finally collected into the recovery barrel 21.

[0035] The above is only the preferred specific implementation of the present application, but the protection scope of the present application is not limited to this, any skilled person in the art can make equivalent replacement or change according to the technical scheme and the inventive concept of the present application within the technical range disclosed by the present application, which should be covered in the protection scope of the present application.

Claims

1. An apparatus for recovering thionyl chloride by distillation, comprising a distillation still (1) placed on the ground, characterized in that, The top of the distillation kettle (1) is connected with the connecting pipe (2) which is symmetrically distributed, the top of the connecting pipe (2) is provided with the filter box (3), the inside of the filter box (3) is provided with the filter screen filter (4) and the deep filter (5) from top to bottom respectively, the upper of the filter box (3) is provided with the high tank (6), the connecting pipe (2) is provided with the valve (7), the distillation kettle (1) is also provided with the distillation recovery assembly (8) which can distill thionyl chloride.

2. An apparatus for recovering thionyl chloride by distillation according to claim 1, characterized in that, The outer wall of the filter box (3) is provided with the mounting groove (9) which is symmetrically distributed, the outward end of the filter screen filter (4) and the deep filter (5) is provided with the sealing cover (10).

3. An apparatus for recovering thionyl chloride by distillation according to claim 2, characterized in that, The filter screen filter (4), the deep filter (5) are slidably connected with the mounting groove (9), the sealing cover (10) is slidably connected with the mounting groove (9).

4. An apparatus for recovering thionyl chloride by distillation according to claim 1, characterized in that, The distillation recovery assembly (8) comprises a thermometer (11), a pressure gauge (12), a material conveying pipe (13), a vacuum pump (14), a flowmeter (15), an extension bar (16), an arc groove (17), a steam recovery pipe (18), a shunt pipe (19), a condenser (20), a recovery bucket (21), the thermometer (11) is arranged on the outer wall of the distillation kettle (1), and the pressure gauge (12) is arranged at the top of the distillation kettle (1).

5. An apparatus for recovering thionyl chloride by distillation according to claim 4, characterized in that, The material conveying pipe (13) is sealingly connected with the connecting pipe (2), the vacuum pump (14) is placed on the ground and connected with the material conveying pipe (13), and the flowmeter (15) is arranged on the vacuum pump (14).

6. An apparatus for recovering thionyl chloride by distillation according to claim 4, characterized in that, The extension bar (16) is fixedly connected with the inner wall of the end cover of the distillation kettle (1), the arc groove (17) is arranged at the top of the extension bar (16), the steam recovery pipe (18) is penetratingly connected with the top of the distillation kettle (1), one end of the shunt pipe (19) is penetratingly connected with the steam recovery pipe (18), the condenser (20) is arranged on the outer wall of the distillation kettle (1), and the recovery bucket (21) is placed on the ground and connected with the condenser (20) through a water pipe.

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