CN217340110U

CN217340110U - High vacuum distillation purification device

Info

Publication number: CN217340110U
Application number: CN202221288771.1U
Authority: CN
Inventors: 张博申
Original assignee: Individual
Current assignee: Individual
Priority date: 2022-05-27
Filing date: 2022-05-27
Publication date: 2022-09-02
Anticipated expiration: 2032-05-27

Abstract

The utility model discloses a high vacuum distillation purification device is applicable to the separation of high boiling point, heat sensitive material. The device at least comprises a distillation kettle with a stirring shaft, wherein a feed inlet is arranged on a distillation kettle shell, a column is directly welded with the distillation kettle at 90 degrees, and the distillation kettle shell except for the feed inlet, the stirring shaft and the welding place of the column and the distillation kettle is completely wrapped by a jacketed heating layer; the front end of the condenser is welded with the top end of the column and inclines downwards, and the tail end of the condenser is connected with the receiving tank through a flange; the upper part of the receiving tank is provided with a vacuum pipeline, the vacuum unit is connected with the receiving tank through the vacuum pipeline, and the vacuum pipeline is provided with a vacuum valve for controlling the opening of the vacuum unit. The utility model has the characteristics of vacuum height, distillation temperature are low, evaporation rate is fast to device easy operation, equipment low price.

Description

High vacuum distillation purification device

Technical Field

The utility model relates to a separation device, which can be applied to the distillation, purification and separation of high boiling point and heat-sensitive substances in chemical production.

Background

At present, the widely applied high vacuum distillation technology in the market is molecular distillation technology, and a plurality of products are also purified by high vacuum reduced pressure distillation by using the technology. However, the molecular distillation technique has some disadvantages as described below. Firstly, the molecular distillation technology has good decolorization effect, but the primary separation degree is not high, so that the product purity is often improved by carrying out multiple times of molecular distillation on materials needing to be improved, the processing capacity is not high, the time is long, and the efficiency is low; secondly, molecular distillation equipment is expensive and high in maintenance cost; finally, the molecular distillation cannot remove light components in stages well, a pre-treatment pre-stage distillation system is needed, and multi-stage distillation is added to remove the light components. This not only increases the time for processing the material, but also reduces the yield of each stage, directly affecting the yield and efficiency of the final product.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a high vacuum distillation purification device to overcome the heat transfer efficiency that current high vacuum distillation device exists low, throughput is little, the material easily takes place oxidation, condenses, polymerization or schizolysis and product light component and gets rid of unclean, the yield is low, and the problem that finished product content is low, be applicable to the separation of high boiling point, heat-sensitive material.

The utility model discloses a solve the technical scheme that above-mentioned problem adopted: a high vacuum distillation purification device is characterized by comprising a distillation kettle with a stirring shaft, wherein a feed inlet is arranged on a distillation kettle shell, a column is directly welded with the distillation kettle at 90 degrees, and the distillation kettle shell except for the feed inlet, the stirring shaft and the position where the column is welded with the distillation kettle is completely wrapped by a jacketed heating layer; the front end of the condenser is welded with the top end of the column and inclines downwards, and the tail end of the condenser is connected with the receiving tank through a flange; the upper part of the receiving tank is provided with a vacuum pipeline, the vacuum unit is connected with the receiving tank through the vacuum pipeline, and the vacuum pipeline is provided with a vacuum valve for controlling the opening of the vacuum unit.

Further, the maximum width of the condenser is consistent with the diameter of the upper end of the column.

Further, the cross-sectional area of the column is equivalent to the longitudinal section of the distillation still.

Furthermore, the column is filled with filler.

The utility model discloses a first advantage utilizes the agitator to make the material be heated evenly, the uneven condition of being heated can not appear. The second advantage is that the evaporation area in the evaporation kettle is large. The third advantage is that the diameter of the column is large and is equivalent to the longitudinal section of the evaporation kettle. A fourth advantage is that the condenser has a large cross-sectional area and a width comparable to the column diameter.

The utility model discloses profitable effect is: the evaporation capacity is increased through a large evaporation area, the heat-sensitive substances are evaporated under high vacuum condition and at lower temperature, and the filler is added into the column to avoid the influence of spray on the product quality. Has the characteristics of high vacuum degree, low distillation temperature and high evaporation speed, and has simple device operation and low equipment price.

Drawings

Fig. 1 is a schematic view of the structure of the device of the present invention.

Fig. 2 is a top view of fig. 1.

The reference numbers illustrate: the device comprises a distillation still 1, a feed inlet 2, a jacketed heating layer 3, a stirring shaft 4, a column 5, a filler 6, a condenser 7, a receiving tank 8, a vacuum unit 9 and a vacuum valve 10.

Detailed Description

As shown in fig. 1 and fig. 2, the high vacuum distillation purification apparatus provided in this embodiment at least includes a feed inlet 2 for facilitating direct feeding, a distillation still 1 with a stirring shaft 4, a fully-wrapped jacketed heating layer 3, a large-caliber column 5 with packing 6, a condenser 7, a receiving tank 8 connected by a flange, and a vacuum unit 9.

The shell of the distillation kettle 1 except the welding position of the feed inlet 2, the stirring shaft 4 and the column 5 with the distillation kettle 1 is completely wrapped by a jacket type heating layer 3, and firstly, the jacket is heated to completely wrap the distillation kettle. The advantage is that the material in the distillation still is heated uniformly under the condition of stirring, and different heat sources are conveniently used by jacket heating, so that the distillation still can be heated by using water vapor or heat transfer oil, and different heating modes can be conveniently adopted according to different material distillation temperatures.

The distillation still 1 is composed of a cylinder which lies horizontally and a seal head, the evaporation area is larger than that of a vertical cylindrical distillation still, the cross-sectional area is enlarged, and the evaporation area is greatly increased. The filler 6 is used for preventing the spray from entering the product and preventing the spray from influencing the quality of the product.

The front end of the condenser 7 is welded with the top end of the column 5 and inclines downwards, the condenser 7 has the width same as the diameter of the top of the column 5, and a large outlet is beneficial to the rapid steam entering the condenser 7.

Receiving

tank

8 and 7 lower extremes of condenser pass through flange joint, because through flange joint, be convenient for change different receiving tank 8, collect the adjustment that can carry out the flexibility to segmentation distillation and easy solidified product.

The utility model discloses an integrated device all adopts but not limited to 304 stainless steel, metal materials such as titanium, makes through the welding.

The operation is briefly described as follows:

adding the materials through a feed inlet 2; sealing the container and opening the container for stirring; starting the vacuum unit 9; opening the vacuum valve 10; adjusting the temperature of the jacketed heating layer 3; the material is changed into steam and enters a condenser 7 through a column 5 to be condensed into liquid; collected collectively in the receiving tank 8. Example (b):

example of the isolation of a mixture of PCA menthyl esters (64519-44-4) using the apparatus of the present invention:

adding a mixture containing 80% of pca menthyl ester and 18% of menthol into a distillation kettle, distilling out the menthol at the vacuum degree of 50Pa and the kettle temperature of 70-90 ℃, and recovering; the residual volume is about 2/3 volume of the distillation kettle, and the finished product is directly distilled out when the temperature is raised to 114 ℃ and 115 ℃ under the condition of the vacuum degree of 50 Pa. The content of the finished product is more than 99.5 percent, and the menthol content is less than 100 ppm.

The above description is only for the specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are all covered by the protection scope of the present invention.

Claims

1. A high vacuum distillation purification device is characterized by comprising a distillation kettle (1) with a stirring shaft (4), wherein a feed inlet (2) is arranged on a shell of the distillation kettle (1), a column (5) is directly welded with the distillation kettle (1) at an angle of 90 degrees, and the shell of the distillation kettle (1) except the feed inlet (2), the stirring shaft (4) and the welding position of the column (5) and the distillation kettle (1) is completely wrapped by a jacket type heating layer (3); the front end of the condenser (7) is welded with the top end of the column (5) and inclines downwards, and the tail end of the condenser (7) is connected with the receiving tank (8) through a flange; the upper part of the receiving tank (8) is provided with a vacuum pipeline, the vacuum unit (9) is connected with the receiving tank (8) through the vacuum pipeline, and the vacuum pipeline is provided with a vacuum valve (10) for controlling the opening of the vacuum unit (9).

2. A high vacuum distillation purification apparatus according to claim 1, wherein the maximum width of said condenser (7) is consistent with the diameter of the upper end of said column (5).

3. A high vacuum distillation purification apparatus according to claim 2, wherein the cross-sectional area of said column (5) is equivalent to the longitudinal section of the still.

4. A high vacuum distillation purification apparatus according to claim 3, wherein said column (5) is packed with packing (6).