Propylene sulfide crude product purification device

Abstract

The utility model discloses a crude product purifying device of propyl sulfide, which relates to the field of experimental facility, a liquid storage tank comprises a temperature control liquid tank, a liquid storage cavity and a liquid delivery pipe which are communicated with each other are sleeved in the temperature control liquid tank, the top of the liquid storage cavity is connected with a liquid injection pipe penetrating through the temperature control liquid tank, and a bottom outlet of the liquid storage cavity is connected with the liquid delivery pipe. A piston valve penetrating through the temperature control liquid tank is arranged at the lower middle part of the liquid conveying pipe; a lower outlet of the liquid conveying pipe is connected with the separation tank through a conveying pipe; the separation tank comprises a vacuum separation cavity, and a liquid inlet connected with the transmission pipe is formed in the upper part of the vacuum separation cavity; a drainage cylinder is fixed in the vacuum separation cavity, the exterior of the vacuum separation cavity is located below the liquid inlet, and a heating liquid cavity is formed above the upper edge of the drainage cylinder; the inner wall of the vacuum separation cavity above the lower edge of the drainage cylinder is connected with an impurity recovery tank through an impurity discharge pipe; a vacuum pipe is arranged at the lower part of the vacuum separation cavity and below the impurity discharge pipe; a cooling column penetrating from the bottom is arranged in the vacuum separation cavity; and the bottom of the vacuum separation cavity is connected with a propyl sulfide recovery tank.

Description

TECHNICAL FIELD

[0001] The utility model relates to experimental device field, especially a standard substance extraction device, specifically a propyl sulfide crude product purification device. BACKGROUND

[0002] Propyl sulfide is used as an organic synthesis intermediate, mainly used for replacing the performance evaluation of protective equipment of the corrosive chemical toxicant mustard gas, or used as a simulation agent in military training.

[0003] At present, the commercially available propyl sulfide is used as raw material in the evaluation of the performance of protective products such as protective clothing against corrosive chemical toxicants, and the content of the commercially available propyl sulfide is basically about 98%, wherein the substances such as ethyl propyl sulfide, sulfone and water affect the threshold of sulfur-containing alarm and sulfur-containing detection instrument, which can cause false alarm, therefore, in order to avoid this phenomenon, the raw material is usually purified to a certain purity, and the impurity content is as small as possible, so as to reduce or eliminate the influence of impurities on the alarm or detection instrument.

[0004] In the existing purification equipment, the United States has developed a permeation tube standard substance, by controlling certain temperature and pressure, a specific compound is allowed to permeate out through the tube wall, the equipment is complex in assembly, high in use cost, and improper use can easily cause leakage, pollute the experimental environment, and harm the health of experimental personnel, and there is no special equipment for purifying propyl sulfide at present. UTILITY MODEL CONTENT

[0005] The utility model discloses in order to solve the low purity of the commercially available propyl sulfide standard product needs to be purified, and there is no special equipment in the purification process, the existing purification equipment is complex in assembly, high in cost and high in risk coefficient, and provides a propyl sulfide crude product purification device.

[0006] The utility model discloses the following technical scheme is adopted: a kind of propyl sulfide crude product purification device, including liquid storage tank and lower than the separation tank of liquid storage tank, liquid storage tank includes temperature control liquid tank, temperature control liquid tank is sleeved with the liquid storage cavity and infusion tube of intercommunication, the top of liquid storage cavity is connected with the injection tube passing through temperature control liquid tank, the bottom outlet of liquid storage cavity is connected infusion tube, the lower part of infusion tube is equipped with the piston valve passing through temperature control liquid tank, and the lower part of infusion tube is connected separation tank by transmission pipe outlet;Separation tank includes vacuum separation cavity, and the upper portion of vacuum separation cavity is opened with the liquid inlet connected with transmission pipe;Vacuum separation cavity is fixed with drainage barrel, and the lower edge of drainage barrel is fixed with the inner wall of vacuum separation cavity middle lower part, and the outer portion of vacuum separation cavity is located below liquid inlet, and the upper edge of drainage barrel is located above heating liquid cavity;The inner wall of vacuum separation cavity is connected with impurity recovery tank by the impurity pipe above the lower edge of drainage barrel;Vacuum separation cavity is equipped with cooling column from bottom into in;The bottom of vacuum separation cavity is connected with propyl sulfide recovery tank.

[0007] In the implementation, the device comprises a liquid storage tank and a separation tank below the liquid storage tank. The liquid storage tank comprises a temperature control liquid tank. The top of the temperature control liquid tank is respectively provided with a temperature control liquid inlet and a temperature control liquid outlet, which are connected with constant temperature liquid, and are used for controlling the temperature of the crude propyl sulfide in the liquid storage tank. A storage cavity and a liquid delivery pipe are sleeved in the temperature control liquid tank. The top of the storage cavity is connected with a liquid injection pipe penetrating through the temperature control liquid tank, which is used for injecting the crude propyl sulfide for purification. The bottom outlet of the storage cavity is connected with the liquid delivery pipe, which controls the output speed of the propyl sulfide. A piston valve is arranged at the lower middle part of the liquid delivery pipe and penetrates through the temperature control liquid tank. The piston valve controls the flow rate and opening and closing of the liquid in the liquid delivery pipe. The lower outlet of the liquid delivery pipe is connected with the separation tank through a transmission pipe.

[0008] The separation tank comprises a vacuum separation cavity. The upper part of the vacuum separation cavity is provided with a liquid inlet connected with the transmission pipe, which is used for introducing the crude propyl sulfide into the separation tank, so that the propyl sulfide flows down along the inner wall of the vacuum separation cavity. A scraper is mounted on the top of the vacuum separation cavity through a bearing. The rotating speed of the scraper is 100-300 r / min. The output end of the scraper is provided with a scraper plate abutting against the inner wall of the vacuum separation cavity. The scraper plate uniformly coats the crude propyl sulfide on the hot inner wall of the vacuum separation cavity.

[0009] A drainage cylinder is fixed in the vacuum separation cavity. The lower edge of the drainage cylinder is fixed to the lower inner wall of the middle part of the vacuum separation cavity. The inner wall of the vacuum separation cavity and the drainage cylinder form a receiving interlayer, which receives the impurity-containing solution flowing down along the inner wall of the vacuum separation cavity. A heating liquid cavity is arranged outside the vacuum separation cavity and above the upper edge of the drainage cylinder below the liquid inlet. The upper part and the lower part of the heating liquid cavity are respectively provided with a heating liquid inlet and a heating liquid outlet. The heating liquid cavity heats the cavity wall of the vacuum separation cavity, so that the propyl sulfide thinly coated on the inner wall of the vacuum separation cavity escapes in the vacuum separation cavity under the condition of low pressure and high temperature.

[0010] The inner wall of the vacuum separation cavity above the lower edge of the drainage cylinder is connected with an impurity recovery tank through a discharge pipe.

[0011] The lower part of the vacuum separation cavity below the discharge pipe is provided with a vacuum pipe, which draws the pressure in the vacuum separation cavity to 10-50 Pa.

[0012] A cooling column penetrating from the bottom is arranged in the vacuum separation cavity. The cooling column is a spiral cooling pipe of circulating cooling liquid. The liquid inlet and the liquid outlet of the cooling column both penetrate from the bottom of the vacuum separation cavity. The height of the cooling column is flush with the upper edge of the heating liquid cavity, so as to increase the area of the cooling liquid.

[0013] The bottom of the vacuum separation cavity is connected with a propyl sulfide recovery tank.

[0014] In use, the device is placed in a fume hood for separation, commercially available propyl sulfide is selected as the crude propyl sulfide raw material, the raw material is poured into the storage cavity from the liquid injection pipe, the propyl sulfide flows to the upper side of the piston valve through the liquid delivery pipe, after the feeding is completed, the piston valve is opened, the propyl sulfide material passes through the transmission pipe into the separation tank, enters the vacuum separation cavity through the liquid inlet, and flows down from the inner wall of the vacuum separation cavity; under the rotation of the film scraper, the propyl sulfide is uniformly scraped on the inner wall of the hot vacuum separation cavity, at the same time, the heating liquid circulates through the heating liquid inlet and the heating liquid outlet, so that the temperature of the inner wall of the vacuum separation cavity is increased, the vacuum pipe is used to draw the vacuum separation cavity to a low pressure, and the propyl sulfide is arranged in a molecular thickness to form a liquid film through the film scraper; the surface temperature of the cooling column in the vacuum separation cavity is 10-20 DEG C, in the vacuum separation cavity with cold and hot alternation, due to the different molecular mass and free path, the propyl sulfide molecules evaporate from the inner wall of the separation tank before the impurity molecules, the light phase escapes to condense into liquid on the built-in cooling column, and flows down along the outer wall of the cooling column into the propyl sulfide recovery tank, so that the separation and purification of propyl sulfide are realized, and the heavy phase continues to flow along the inner wall of the vacuum separation cavity, enters the interlayer of the vacuum separation cavity and the flow guide cylinder, and reaches the impurity recovery tank from the impurity discharge pipe.

[0015] Compared with the prior art, the propyl sulfide crude product purification device has the following beneficial effects:

[0016] The propyl sulfide crude product purification device has the following beneficial effects:

[0017] The propyl sulfide standard substance collected by the device is recovered separately, so that the impurities are not mixed in the unpurified propyl sulfide raw material, the content of propyl sulfide in the propyl sulfide raw material is reduced, the purification efficiency is reduced, the purification efficiency is effectively improved, the purification time is reduced, and the production efficiency is improved. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 The utility model discloses a kind of propyl sulfide crude product purification devices, including storage tank, vacuum separation cavity, cooling column, vacuum pipe, liquid injection pipe, transmission pipe, liquid inlet, film scraper, flow guide cylinder, heating liquid cavity, heating liquid inlet, heating liquid outlet, impurity recovery tank and propyl sulfide recovery tank.

[0019] Figure 2 It is the side view of the upper portion of storage tank.

[0020] In the drawing, 1-temperature control liquid tank, 2-temperature control liquid inlet, 3-temperature control liquid outlet, 4-storage cavity, 5-liquid delivery pipe, 6-liquid injection pipe, 7-piston valve, 8-transmission pipe, 9-vacuum separation cavity, 10-liquid inlet, 11-film scraper, 1101-scraping plate, 12-flow guide cylinder, 13-heating liquid cavity, 14-heating liquid inlet, 15-heating liquid outlet, 16-impurity discharge pipe, 17-impurity recovery tank, 18-vacuum pipe, 19-cooling column, 20-propyl sulfide recovery tank. DETAILED DESCRIPTION

[0021] The utility model discloses a specific embodiment of the utility model is specifically illustrated in connection with the drawings.

[0022] A kind of crude propyl sulfide purification device, as shown in Figure 1 、 2 Including liquid storage tank and lower separation tank of liquid storage tank, liquid storage tank includes temperature control liquid tank 1, the top of temperature control liquid tank 1 is respectively opened temperature control liquid inlet 2 and temperature control liquid outlet 3, connect constant temperature liquid, for controlling the temperature of crude product propyl sulfide in liquid storage tank;Temperature control liquid tank 1 is sleeved with the liquid storage cavity 4 and liquid transfer pipe 5 of intercommunication, the top of liquid storage cavity 4 is connected with the liquid injection pipe 6 passing through temperature control liquid tank 1, for injecting propyl sulfide crude product and purifying, the bottom outlet of liquid storage cavity 4 is connected with liquid transfer pipe 5, and the speed of propyl sulfide output is controlled, the lower part of the middle of liquid transfer pipe 5 is equipped with piston valve 7 passing through temperature control liquid tank 1, and piston valve 7 controls the liquid flow rate in liquid transfer pipe 5 and opens and closes, and the lower part outlet of liquid transfer pipe 5 is connected with separation tank through transmission pipe 8.

[0023] Separation tank includes vacuum separation cavity 9, and the upper portion of vacuum separation cavity 9 is opened with liquid inlet 10 connected with transmission pipe 8, and crude product propyl sulfide is introduced into the separation tank, so that propyl sulfide flows down along the inner wall of vacuum separation cavity 9;Vacuum separation cavity 9 is installed with scraper 11 on the top through bearing, and the rotating speed of scraper 11 is 100-300r / min, and the output end of scraper 11 is installed with scraper plate 1101 abutting on the inner wall of vacuum separation cavity 9, and the crude product propyl sulfide is evenly scraped on the inner wall of hot vacuum separation cavity 9 by scraper plate 1101.

[0024] Vacuum separation cavity 9 is fixed with drainage cylinder 12, and the lower edge of drainage cylinder 12 is fixed with the inner wall of the lower middle part of vacuum separation cavity 9, and the inner wall of vacuum separation cavity 9 forms a receiving interlayer with drainage cylinder 12, and the impurity-containing solution flowing down along the inner wall of vacuum separation cavity 9 is received, and the outer portion of vacuum separation cavity 9 is located below liquid inlet 10, and the upper edge of drainage cylinder 12 is located above heating liquid cavity 13;The upper portion and the lower portion of heating liquid cavity 13 are respectively provided with heating liquid inlet 14 and heating liquid outlet 15, and the cavity wall of vacuum separation cavity 9 is heated by heating liquid cavity 13, so that propyl sulfide thinly coated on the inner wall of vacuum separation cavity 9 escapes in vacuum separation cavity 9 under low pressure and high temperature.

[0025] The inner wall of vacuum separation cavity 9 is connected with impurity recovery tank 17 through impurity discharge pipe 16 above the lower edge of drainage cylinder 12;

[0026] The lower portion of vacuum separation cavity 9 is located below impurity discharge pipe 16 and is provided with vacuum pipe 18, and the pressure in vacuum separation cavity 9 is extracted to 10-50Pa;

[0027] The cooling column 19 is a spiral cooling pipe of circulating cooling liquid, the liquid inlet and liquid outlet of the cooling column 19 are both penetrated from the bottom of the vacuum separation cavity 9, the height of the cooling column 19 is flush with the upper edge of the heating liquid cavity 13, and the area of the cooling liquid is increased;

[0028] The bottom of the vacuum separation cavity 9 is connected with a propyl sulfide recovery tank 20.

[0029] In use, the device is placed in a fume hood for separation, commercially available propyl sulfide is selected as the raw material of the crude propyl sulfide, the raw material is poured into the liquid storage cavity 4 from the liquid pouring pipe 6, the propyl sulfide flows to the upper side of the piston valve 7 along the liquid conveying pipe 5, after the feeding is completed, the piston valve 7 is opened, the propyl sulfide material enters the separation tank through the transmission pipe 8, enters the vacuum separation cavity 9 through the liquid inlet 10 and flows down from the inner wall of the vacuum separation cavity 9; under the rotation of the film scraper 11, the propyl sulfide is uniformly scraped and coated on the inner wall of the hot vacuum separation cavity 9, at the same time, the heating liquid circulates along the heating liquid inlet 14 and the heating liquid outlet 15, so that the temperature of the inner wall of the vacuum separation cavity is increased, the vacuum pipe 18 draws the vacuum separation cavity 9 to a low pressure, the propyl sulfide is arranged in a molecular thickness to form a liquid film through the film scraper 11; the surface temperature of the cooling column in the vacuum separation cavity 9 is 10-20 DEG C, in the vacuum separation cavity 9 with alternating cold and hot, because the molecular mass is different, the free path is different, the propyl sulfide molecules evaporate from the inner wall of the separation tank before the impurity molecules, the light phase escapes and condenses into liquid on the built-in cooling column 19, and flows down along the outer wall of the cooling column 19 and enters the propyl sulfide recovery tank 20, so that the separation and purification of the propyl sulfide are realized, and the heavy phase continues to flow along the inner wall of the vacuum separation cavity 9, enters the interlayer of the vacuum separation cavity 9 and the flow guide cylinder 12, and reaches the impurity recovery tank 17 from the impurity discharge pipe 16.

[0030] The scope of the utility model is not limited to the above specific embodiments, and for those skilled in the art, the utility model can have various modifications and alterations, and any modification, improvement and equivalent replacement within the concept and principle of the utility model should be included in the protection scope of the utility model.

Claims

1. A device for purifying crude propyl sulfide, characterized by: The application relates to a liquid storage tank and a separation tank below the liquid storage tank, wherein the liquid storage tank comprises a temperature-controlled liquid tank (1), a liquid storage cavity (4) and a liquid delivery pipe (5) are sleeved in the temperature-controlled liquid tank (1) and are communicated, a liquid injection pipe (6) penetrating through the temperature-controlled liquid tank (1) is connected to the top of the liquid storage cavity (4), the bottom outlet of the liquid storage cavity (4) is connected to the liquid delivery pipe (5), a piston valve (7) penetrating through the temperature-controlled liquid tank (1) is arranged at the lower middle part of the liquid delivery pipe (5), and the lower outlet of the liquid delivery pipe (5) is connected to the separation tank through a transmission pipe (8); The separation tank comprises a vacuum separation cavity (9), and a liquid inlet (10) connected to the transmission pipe (8) is formed in the upper part of the vacuum separation cavity (9); A drainage cylinder (12) is fixed in the vacuum separation cavity (9), the lower edge of the drainage cylinder (12) is fixed to the inner wall of the lower middle part of the vacuum separation cavity (9), and a heating liquid cavity (13) is arranged outside the vacuum separation cavity (9) and above the upper edge of the drainage cylinder (12) below the liquid inlet (10); The inner wall of the vacuum separation cavity (9) above the lower edge of the drainage cylinder (12) is connected to an impurity recovery tank (17) through a purifying pipe (16); A vacuum pipe (18) is arranged below the purifying pipe (16) at the lower part of the vacuum separation cavity (9); A cooling column (19) penetrating from the bottom is arranged in the vacuum separation cavity (9); The bottom of the vacuum separation cavity (9) is connected to a propyl sulfide recovery tank (20).

2. A device for purifying crude propyl sulfide according to claim 1, characterized in that: A scraper (11) is installed on the top of the vacuum separation cavity (9) through a bearing, and a scraper plate (1101) abutting against the inner wall of the vacuum separation cavity (9) is arranged on the output end of the scraper (11).

3. A device for purifying crude propyl sulfide according to claim 1, characterized in that: The top of the temperature-controlled liquid tank (1) is respectively provided with a temperature-controlled liquid inlet (2) and a temperature-controlled liquid outlet (3).

4. A device for purifying crude propyl sulfide according to claim 1, characterized in that: The upper part and the lower part of the heating liquid cavity (13) are respectively provided with a heating liquid inlet (14) and a heating liquid outlet (15).

5. A device for purifying crude propyl sulfide according to claim 1, characterized in that: The liquid inlet and the liquid outlet of the cooling column (19) both penetrate from the bottom of the vacuum separation cavity (9), and the height of the cooling column (19) is flush with the upper edge of the heating liquid cavity (13).

6. A device for purifying crude propyl sulfide according to claim 5, characterized in that: The cooling column (19) is a spiral cooling pipe.

7. A device for purifying crude propyl sulfide according to claim 1, characterized in that: The piston valve (7) controls the liquid flow in the liquid delivery pipe (5).

8. A device for purifying crude propyl sulfide according to claim 2, characterized in that: The rotating speed of the scraper (11) is 100-300 r / min.

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