Purification equipment and purification method for organic solvent n-heptane

Abstract

The purification equipment comprises a distillation barrel, the lower portion of a steam conveying pipe is connected with the distillation barrel, the lower portion of a supporting rod is connected with the distillation barrel, the upper portion of the supporting rod is connected with a condensation barrel, the side face of the condensation barrel is connected with a discharge pipe, the discharge pipe is connected with a valve, and the upper portion of the steam conveying pipe is inserted into the condensation barrel; an inner baffle filtering membrane cloth outer frame is arranged on the outer side of the filtering membrane cloth, an organic solvent n-heptane solution is poured into the distillation barrel, a proper amount of distilled persimmon frost is added, distillation is conducted in an oil bath heating mode, heating is conducted gradually to the hot bath temperature in the process, distillation is conducted continuously under the ventilation condition of a laboratory till the volume collection rate of petroleum ether is basically unchanged, and the petroleum ether is obtained. Through the steps, ethyl acetate and other impurities in n-heptane can be removed, the purity of an n-heptane sample can be improved, and in actual operation, the distillation temperature and the amount of distilled persimmon frost are generally required to be adjusted according to different characteristics and requirements of the sample so as to achieve the optimal distillation and purification effect.

Description

Technical Field

[0001] The invention relates to the field of n-heptane purification equipment, and in particular to a purification equipment and a purification method for an organic solvent n-heptane. Background Art

[0002] The existing patent (Announcement No.: CN103723719B) proposes a purification device, including a feed system, a purification furnace and a discharge system arranged in sequence along the vertical direction, and the purification furnace includes a muffle for purification heating and a resistance heating device arranged around the muffle. Purification work is carried out in the vertical direction, the feed system feeds the material at the top of the purification furnace, the purification work is carried out in the purification furnace, and the material is discharged by the discharge system at the bottom of the purification furnace. The material is purified inside the muffle, and the resistance heating device ensures the processing temperature inside the muffle to achieve high temperature heating. The discharge pipe of this device is connected to the bottom of the sealed aggregate bin, but there is no filtering device between the discharge pipe and the sealed aggregate bin, which easily causes the discharged material to contain impurities when used. Summary of the invention

[0003] In view of the above-mentioned deficiencies in the prior art, the present invention provides a purification device and method for an organic solvent n-heptane, in which a filter membrane cloth is installed between an arc partition and a condensation barrel through an inner baffle plate and an outer frame of the filter membrane cloth. The filter membrane cloth filters the condensed organic solvent n-heptane and impurities can be removed.

[0004] The purpose of the present invention is to be achieved through the following technical solutions: A purification device and a purification method for an organic solvent n-heptane, comprising a distillation barrel, a steam delivery pipe, a condensation barrel, a discharge pipe, a support rod, a reactant barrel, a rotating door, an arc-shaped partition, an inner baffle filter membrane cloth outer frame, a filter membrane cloth, and a rotating baffle, wherein the lower portion of the steam delivery pipe is connected to the distillation barrel, the lower portion of the support rod is connected to the distillation barrel, the upper portion of the support rod is connected to the condensation barrel, the side of the condensation barrel is connected to the discharge pipe, the discharge pipe is connected to the valve, the upper portion of the steam delivery pipe is inserted into the condensation barrel, the arc-shaped partition is connected to the condensation barrel, the outer side of the filter membrane cloth has an inner baffle filter membrane cloth outer frame, the condensation barrel has a condensation barrel side hole, the right side of the inner baffle filter membrane cloth outer frame is fitted with the arc-shaped partition, the lower right surface of the inner baffle filter membrane cloth outer frame is fitted with the arc-shaped partition, the left side of the inner baffle filter membrane cloth outer frame is fitted with the inner side of the condensation barrel, and the lower portion of the inner baffle filter membrane cloth outer frame has an outer frame convex plate.

[0005] The rotating door is adapted to the side hole of the condensation barrel, the rotating door is inserted into the side hole of the condensation barrel, the lower part of the rotating door is provided with a rotating door lower sleeve, the side connecting ears are connected to the condensation barrel, the two ends of the rotating door lower sleeve are fitted with a group of side connecting ears, the rotating door lower sleeve is connected to the side connecting ear axis, the inner baffle filter membrane cloth outer frame is connected to the condensation barrel, the inner side surface of the rotating door is fitted with the inner baffle filter membrane cloth outer frame, and a group of inner baffle filter membrane cloth outer frames are distributed in the condensation barrel.

[0006] The upper part of the rotating door is provided with an upper giving way notch, the upper part of the rotating door is provided with a plastic card board, the upper part of the side hole of the condensation barrel is provided with a limiting card slot, the upper part of the plastic card board is inserted into the limiting card slot, the side of the plastic card board is provided with a plastic card board side plate, the lower part of the reactant barrel is provided with a reactant barrel lower tube, and the lower part of the reactant barrel lower tube is connected to the upper part of the distillation barrel.

[0007] The rotating baffle is adapted to the lower tube of the reactant barrel, the rotating baffle is inserted into the lower tube of the reactant barrel, the rotating baffle rotates in the lower tube of the reactant barrel, the outer side of the rotating baffle is connected to the rubber outer ring, the outer side of the rubber outer ring is in contact with the inner wall of the lower tube of the reactant barrel, the rotating rod passes through the lower tube of the reactant barrel to connect the rotating baffle, and the rotating rod rotates in the lower tube of the reactant barrel. Beneficial Effects

[0008] 1. The distillation barrel of the present invention contains diluted organic solvent n-heptane, a heating structure is installed in the distillation barrel to heat the organic solvent n-heptane in the distillation barrel, the lower part of the steam delivery pipe is connected to the distillation barrel, and the vapor volatilized when the organic solvent n-heptane in the distillation barrel is heated moves upward into the steam delivery pipe, the bottom of the condensation barrel is installed on the upper part of the distillation barrel through a support rod, the steam delivery pipe is inserted into the condensation barrel, so that the organic solvent n-heptane vapor in the steam delivery pipe enters the condensation barrel for condensation, and the condensation is carried out in the condensation barrel, the arc partition is connected to the condensation barrel, and the organic solvent n-heptane entering the condensation barrel is placed in the area surrounded by the condensation barrel and the arc partition, the filter membrane cloth is installed between the arc partition and the condensation barrel through the inner baffle plate and the outer frame of the filter membrane cloth, the filter membrane cloth filters the condensed organic solvent n-heptane to remove impurities, 2. The lower sleeve of the rotating door of the present invention is connected to the side connecting ear shaft, so that the rotating door is installed on the side of the condensation barrel, and the plastic card plate is inserted into the limit card slot. The limit card slot limits the rotating door to prevent the rotating door from rotating and opening. A group of inner baffles and the outer frame of the filter membrane cloth limit the inside of the rotating door to prevent the rotating door from rotating inward. When there are many impurities in the filter membrane cloth, the side plate of the plastic card plate can be pressed downward so that the plastic card plate can be rotated out of the limit card slot to open the rotating door. After the rotating door is opened, the filter membrane cloth can be taken out for cleaning, and the organic solvent n-heptane liquid falling from the filter membrane cloth can flow out from the discharge pipe. This device purifies the organic solvent n-heptane according to the different boiling points of the distillation of the n-heptane solution containing impurities such as ethyl acetate, and controls the rotation of the rotating baffle in the lower tube of the reactant barrel by rotating the rotating rod to control the amount of reactant entering the distillation barrel from the reactant barrel. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] Figure 1 This is a left axonometric view of a purification device and a purification method for an organic solvent n-heptane according to the present invention.

[0010] Figure 2 This is a right-view axonometric diagram of an organic solvent n-heptane purification device and purification method described in the present invention.

[0011] Figure 3 This is the first cross-sectional view of the purification equipment and purification method of the organic solvent n-heptane described in the present invention.

[0012] Figure 4 This is the second cross-sectional view of the purification equipment and purification method of the organic solvent n-heptane described in the present invention.

[0013] Figure 5 This is an axonometric view of the distillation barrel and condensation barrel described in the present invention.

[0014] Figure 6 This is an axonometric view of the revolving door described in the present invention.

[0015] Figure 7 This is an axonometric view of the filter membrane cloth described in the present invention.

[0016] Figure 8 This is a top view of the cross-sectional view of the lower tube of the reactant barrel and the rotating baffle of the present invention. DETAILED DESCRIPTION

[0017] The present invention is further described in detail below according to the accompanying drawings and embodiments: Embodiment 1: A purification device and method for an organic solvent n-heptane, comprising a distillation barrel 01, a steam delivery pipe 02, a condensation barrel 03, a discharge pipe 04, a support rod 05, a reactant barrel 06, a rotating door 09, an arc-shaped partition 15, an inner baffle filter membrane cloth outer frame 17, a filter membrane cloth 18, and a rotating baffle 20. The lower portion of the steam delivery pipe 02 is connected to the distillation barrel 01, in which a diluted organic solvent n-heptane is placed, a heating structure is installed in the distillation barrel 01 to heat the organic solvent n-heptane in the distillation barrel 01, and the vapor volatilized when the organic solvent n-heptane in the distillation barrel 01 is heated moves upward into the steam delivery pipe 02, the lower portion of the support rod 05 is connected to the distillation barrel 01, the upper portion of the support rod 05 is connected to the condensation barrel 03, the bottom of the condensation barrel 03 is installed on the upper portion of the distillation barrel 01 through the support rod 05, the side of the condensation barrel 03 is connected to the discharge pipe 04, the discharge pipe 04 is connected to the valve, and the upper portion of the steam delivery pipe 02 is inserted into the condensation barrel 03, the organic solvent n-heptane vapor in the steam delivery pipe 02 enters the condensation barrel 03 for condensation in the condensation barrel 03, the arc-shaped partition 15 connects the condensation barrel 03, and the organic solvent n-heptane entering the condensation barrel 03 is placed in the area surrounded by the condensation barrel 03 and the arc-shaped partition 15. The outer side of the filter membrane cloth 18 has an inner baffle filter membrane cloth outer frame 17, and the condensation barrel 03 has a condensation barrel side hole 08. The right side of the inner baffle filter membrane cloth outer frame 17 is in contact with the arc-shaped partition 15, and the lower surface of the right side of the inner baffle filter membrane cloth outer frame 17 is in contact with the arc-shaped partition 15. The left side of the inner baffle filter membrane cloth outer frame 17 is in contact with the inner side of the condensation barrel 03. The lower part of the inner baffle filter membrane cloth outer frame 17 has an outer frame convex plate 19. The filter membrane cloth 18 is installed between the arc-shaped partition 15 and the condensation barrel 03 through the inner baffle filter membrane cloth outer frame 17. The filter membrane cloth 18 filters the condensed organic solvent n-heptane to remove impurities.

[0018] Embodiment 2: The revolving door 09 of the present invention is adapted to the side hole 08 of the condensing barrel, the revolving door 09 is inserted into the side hole 08 of the condensing barrel, the lower part of the revolving door 09 is provided with a revolving door lower sleeve 11, the side connecting ear 10 is connected to the condensing barrel 03, the two ends of the revolving door lower sleeve 11 are fitted with a group of side connecting ears 10, the revolving door lower sleeve 11 is axially connected with the side connecting ear 10, so that the revolving door 09 is installed on the side of the condensing barrel 03, the inner baffle filter membrane cloth outer frame 17 is connected to the condensing barrel 03, and the inner side surface of the revolving door 09 is fitted with the inner baffle filter membrane cloth outer frame 17 A group of inner baffle filter membrane cloth outer frames 17 are distributed in the condensation barrel 03, and a group of inner baffle filter membrane cloth outer frames 17 limit the inside of the rotating door 09 to prevent the rotating door 09 from rotating inward. When there are many impurities in the filter membrane cloth 18, the plastic pallet side plate 13 can be pressed downward to allow the plastic pallet 12 to be rotated out of the limiting slot 16, and the rotating door 09 can be opened. After the rotating door 09 is opened, the filter membrane cloth 18 can be taken out for cleaning, and the organic solvent n-heptane liquid falling from the filter membrane cloth 18 can flow out from the discharge pipe 04.

[0019] Embodiment 3: The rotating door 09 of the present invention has an upper clearance notch 14 on the upper part, a plastic card board 12 on the upper part of the rotating door 09, a limiting card slot 16 on the upper part of the condensation barrel side hole 08, the upper part of the plastic card board 12 is inserted into the limiting card slot 16, the limiting card slot 16 limits the rotating door 09 to prevent the rotating door 09 from rotating and opening, the side of the plastic card board 12 has a plastic card board side plate 13, the lower part of the reactant barrel 06 has a reactant barrel lower tube 07, and the lower part of the reactant barrel lower tube 07 is connected to the upper part of the distillation barrel 01.

[0020] Embodiment 4: The rotating baffle 20 of the present invention is adapted to the lower tube 07 of the reactant barrel, the rotating baffle 20 is inserted into the lower tube 07 of the reactant barrel, the rotating baffle 20 rotates in the lower tube 07 of the reactant barrel, the outer side of the rotating baffle 20 is connected to the rubber outer ring 21, the outer side of the rubber outer ring 21 is in contact with the inner wall of the lower tube 07 of the reactant barrel, the rotating rod 22 passes through the lower tube 07 of the reactant barrel to connect the rotating baffle 20, the rotating rod 22 rotates in the lower tube 07 of the reactant barrel, and the rotating baffle 20 is controlled to rotate in the lower tube 07 of the reactant barrel by rotating the rotating rod 22, so as to control the amount of reactant from the reactant barrel 06 entering the distillation barrel 01. The method for purifying the organic solvent n-heptane comprises the following steps: firstly taking the raw material n-heptane, sequentially adding a sulfuric acid solution with a volume concentration of 12% and a nitric acid solution with a volume concentration of 38%, wherein the volume ratio of sulfuric acid to nitric acid is 2:5, shaking and standing for stratification, discarding the acid layer and retaining the organic layer; adding activated carbon to the organic layer, stirring for 3 hours, adding potassium permanganate for oxidation, and refluxing for 2 hours before rapidly distilling out the n-heptane. Then, the obtained n-heptane is passed through an adsorbent column equipped with modified activated carbon to further remove the benzene ring-containing substances formed during the oxidation process. The n-heptane is passed through an adsorbent column of silica gel. The obtained n-heptane is rectified to obtain the high-purity organic solvent n-heptane.

[0021] Embodiment 5: The installation steps of the present invention are as follows: first, connect the lower part of the steam delivery pipe 02 to the distillation barrel 01, connect the arc partition 15 to the condensation barrel 03, insert the filter membrane cloth 18 between the arc partition 15 and the condensation barrel 03, connect the rotating door lower sleeve 11 to the side connecting ear 10 axis, connect the inner baffle filter membrane cloth outer frame 17 to the condensation barrel 03, connect the upper and lower ends of the support rod 05 to the condensation barrel 03 and the distillation barrel 01 respectively, insert the upper part of the steam delivery pipe 02 through the upper cover of the condensation barrel 03 into the condensation barrel 03, connect the outer side of the rotating baffle 20 to the rubber outer ring 21, insert the rotating baffle 20 into the lower tube 07 of the reactant barrel, pass the rotating rod 22 through the lower tube 07 of the reactant barrel to connect the rotating baffle 20, and connect the lower part of the lower tube 07 of the reactant barrel to the distillation barrel 01.

[0022] A purification method for an organic solvent n-heptane purification device: when the device is in use, the organic solvent n-heptane solution is poured into a distillation barrel 01 and an appropriate amount of distilled persimmon frost is added, and distillation is performed by heating with an oil bath, and gradually heated to the temperature of a hot water bath during the process, and the volume collection rate of petroleum ether is continuously distilled under laboratory ventilation conditions until it remains substantially unchanged. Through the above steps, impurities such as ethyl acetate in n-heptane can be removed, and the purity of the n-heptane sample can be improved. In actual operation, it is usually necessary to adjust the distillation temperature and the amount of distilled persimmon frost according to the different characteristics and requirements of the sample to achieve the best distillation and purification effect.

[0023] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. It should be pointed out that a person skilled in the art can make several improvements and modifications without departing from the technical principles of the present invention, and these improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A purification device and a purification method for an organic solvent n-heptane, Its characteristics are : It comprises a distillation barrel (01), a steam delivery pipe (02), a condensation barrel (03), a discharge pipe (04), a support rod (05), a reactant barrel (06), a rotating door (09), an arc-shaped partition (15), an inner baffle filter membrane cloth outer frame (17), a filter membrane cloth (18), and a rotating baffle (20), wherein the lower part of the steam delivery pipe (02) is connected to the distillation barrel (01), the lower part of the support rod (05) is connected to the distillation barrel (01), the upper part of the support rod (05) is connected to the condensation barrel (03), the side of the condensation barrel (03) is connected to the discharge pipe (04), the discharge pipe (04) is connected to the valve, and the steam delivery pipe (02) is connected to the distillation barrel (01). The upper part of the tube (02) is inserted into the condensation barrel (03), the arc-shaped partition (15) is connected to the condensation barrel (03), the outer side of the filter membrane cloth (18) is provided with an inner baffle filter membrane cloth outer frame (17), the condensation barrel (03) has a condensation barrel side hole (08), the right side of the inner baffle filter membrane cloth outer frame (17) is in contact with the arc-shaped partition (15), the right lower surface of the inner baffle filter membrane cloth outer frame (17) is in contact with the arc-shaped partition (15), the left side of the inner baffle filter membrane cloth outer frame (17) is in contact with the inner side of the condensation barrel (03), and the lower part of the inner baffle filter membrane cloth outer frame (17) is provided with an outer frame convex plate (19).

2. The purification device and method of an organic solvent n-heptane according to claim 1, Its characteristics are The rotating door (09) is adapted to the side hole (08) of the condensation barrel, the rotating door (09) is inserted into the side hole (08) of the condensation barrel, the lower part of the rotating door (09) is provided with a rotating door lower sleeve (11), the side connecting ears (10) are connected to the condensation barrel (03), the two ends of the rotating door lower sleeve (11) are fitted with a group of side connecting ears (10), the rotating door lower sleeve (11) is axially connected with the side connecting ears (10), the inner baffle plate filter membrane cloth outer frame (17) is connected to the condensation barrel (03), the inner side surface of the rotating door (09) is fitted with the inner baffle plate filter membrane cloth outer frame (17), and a group of inner baffle plate filter membrane cloth outer frames (17) are distributed in the condensation barrel (03).

3. The purification device and method of an organic solvent n-heptane according to claim 2, Its characteristics are The upper part of the rotating door (09) is provided with an upper clearance notch (14), the upper part of the rotating door (09) is provided with a plastic cardboard (12), the upper part of the condensation barrel side hole (08) is provided with a limit card slot (16), the upper part of the plastic cardboard (12) is inserted into the limit card slot (16), the side of the plastic cardboard (12) is provided with a plastic cardboard side plate (13), the lower part of the reactant barrel (06) is provided with a reactant barrel lower tube (07), and the lower part of the reactant barrel lower tube (07) is connected to the upper part of the distillation barrel (01).

4. The purification device and method for the organic solvent n-heptane according to claim 3, Its characteristics are The rotating baffle (20) is adapted to the lower tube (07) of the reactant barrel. The rotating baffle (20) is inserted into the lower tube (07) of the reactant barrel. The rotating baffle (20) rotates in the lower tube (07) of the reactant barrel. The outer side of the rotating baffle (20) is connected to a rubber outer ring (21).

5. The purification device and method for the organic solvent n-heptane according to claim 4, Its characteristics are The outer side surface of the rubber outer ring (21) is in contact with the inner wall of the lower tube (07) of the reactant barrel, the rotating rod (22) passes through the lower tube (07) of the reactant barrel and is connected to the rotating baffle (20), and the rotating rod (22) rotates in the lower tube (07) of the reactant barrel.

6. A method for purifying an organic solvent, n-heptane, Its characteristics are : Pour the organic solvent n-heptane solution into the distillation barrel and add an appropriate amount of distilled persimmon frost, and distill it by heating in an oil bath. Gradually heat it to the temperature of a hot water bath during the process, and continue to distill under ventilation conditions in the laboratory until the volume collection rate of petroleum ether remains basically unchanged. Through the above steps, impurities such as ethyl acetate in n-heptane can be removed and the purity of the n-heptane sample can be improved. In actual operation, it is usually necessary to adjust the distillation temperature and the amount of distilled persimmon frost according to the different characteristics and requirements of the samples to achieve the best distillation and purification effect.

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