JPS59209605A - Refluxing and slide flowing-down membrane type distillation apparatus - Google Patents

Abstract

PURPOSE:To contrive to enhance the purity and recovery rate of a product, by forcibly refluxing a condensate by mounting reflux pipes to a large number of sections formed by dividing a condensing surface. CONSTITUTION:A raw liquid is supplied from a raw liquid feed pipe 19 to enter the liquid dispersing pipe 20 integrally rotated along with a rotary arm 17 and evaporated while scattered to an evaporation surface heated by a heating jacket 11. The generated steam is condensed in an uppermost stage recovery part S-1 and the condensate is collected by a receiver 21 to be taken out from a withdrawing pipe 23. The condensed liquids in the next recovery parts S-2, S-3 enter rotary receivers 26 from condensate receiving nozzles 25 and pass reflux pipes 27 by centrifugal force and refluxed to the liquid dispersing pipe 20 to be repeatedly subjected to evaporation. By this mechanism, the purity and recovery rate of a product are remarkably enhanced.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sliding flow type Kurobe device.

Conventionally, rectification using a vacuum cap distillation device has been carried out using plate columns, packed columns, etc., but when used in high vacuum regions, the vacuum level and residence time are different at the top and bottom of the column. Because of its large size, it could not be applied to substances that require a high vacuum black space, heat-sensitive substances, or low vapor pressure. In addition, high-vacuum distillation equipment is so-called molecular distillation equipment, which mainly uses half-covered distillation equipment, but uses the pot steel method.

Both the falling film method and the centrifugal method have complicated structures and have problems such as pressure loss and inconvenience in disassembling and cleaning even during use, so there was a need for an advantageous precision measuring device.

The present invention has been made in view of the above points, and it is an object of the present invention to provide an apparatus that increases the purity and recovery rate of lid products, improves the rectification effect, has a simple and convenient structure, and is easy to disassemble and clean. It is a purpose.

The first invention to achieve this object divides the condensation surface into a large number of sections, and each section is provided with a liquid dispersion tube that disperses the liquid evenly through the rotation of the section. A reflux sliding falling film type Kurobe device characterized in that a reflux pipe is provided between each section for forcibly refluxing liquid from a rotating receiver to a liquid dispersion tube by centrifugal force,
In addition, the second invention divides the condensation surface into a large number of sections, and each section is provided with a liquid dispersion tube that disperses the liquid evenly through rotation of the section, and the condensate is transferred from the rotating receiver to the liquid dispersion tube through the elution receiving nozzle. A reflux sliding falling membrane, characterized in that a reflux pipe for forcibly refluxing by centrifugal force is provided between each section, and the elution receiving nozzle 1 &: is pivotally supported on a partial receiving getter so as to be rotatable to the vertical position. This is related to the Shiki Kurobe device.

The device of the present invention will be described below based on the illustrated embodiment. The device of the present invention is composed of a body 1, its fins 2, 3, and a lid 4.5, and is made airtight by an O-ring 6. The upper part of the main body has a bearing section having a rotating shaft 7, and a bearing 9 in the shaft housing 8 and a mechanical seal 10IC form a rotating airtight seal.

The inner wall of the shell 1 forms an evaporation surface, and a heating jacket 11 is attached to the outer wall. There is a condenser 12 in the center of the body, and an exhaust port 13 is connected to a vacuum device at the bottom of the inner cylinder of the condenser to create a vacuum inside the main body.

Drive motor 14. The motor side pulley 152 and the main rotating shaft side pulley 16 rotate by decelerating the rotating shaft 7 via the V-pel If, and the sliding brush 18 is integrally connected to the rotating arm 17.
is rotated and slid on the evaporation surface to form a uniform thin film.

In the example of implementation, the first stage of the recovery section (S-1 section), the second stage of the concentration section (S-2 section), and the third stage (S-3 section) are configured. A vacuum device is connected to keep the inside of the main body in a vacuum state, and a heating medium or high temperature steam is introduced into the heating jacket 11 to heat the steam □□□□□□ surface. At this time, the heating temperature of each section is set to a desired value as necessary, cooling water is circulated in the condenser 12, and an evaporation division buckle 24 is attached to the rotary arm 17 to divide the inside of the hot melting chamber into stages. ing.

The stock solution is supplied through the raw material feed pipe 19, enters the liquid dispersion tube 20 that rotates simultaneously with the rotary arm 17, is spread on the evaporation surface, and is heated to form a uniform thin film by the sliding brush 18. The liquid is evaporated, collected in the condenser of the top recovery section (S-1 section) with a high degree of vacuum, and then sequentially collected in a receiver 21, passed through a pipe 22, and taken out through an extraction pipe 23. There is. 8-2 of condenser. The condensed material in the S-3 section enters the rotary receiver 26 through the elution receiver nozzle 25 provided for each section of the condenser, passes through the reflux pipe 27 by centrifugal force, and enters the liquid dispersion tube 20. It is refluxed and sprayed on the evaporation surface to reverse evaporation. The final portion accumulates at the bottom of the device and is removed from the residue pipe 28 after the end of the operation.

The liquid dispersion tube 20 is constructed in detail as shown in FIGS. 2 and 3, and has a gutter-like cross section installed in an annular manner to receive both the stock solution and the reflux solution.

A roof-shaped cover is formed on the upper part to prevent the hot solution from turning into a mist and to improve the accuracy of the black part, and a large number of small holes 29 with a suitable diameter are formed at regular intervals or evenly spaced in several stages on the evaporation surface side. The centrifugal force generated during rotation makes it possible to spray liquid uniformly over the evaporation surface without creating mist. Reflux pipe 27i1
Although it protrudes into the liquid dispersion tube 20, a small cover 30 is fixedly installed directly above the tip of the tube in order to completely prevent sudden injection of reflux liquid. With this configuration, the liquid sprayed onto the evaporation surface from the liquid dispersion tube 20 is made into a uniform thin film by the sliding brush.

Next, details of the partial receiving nozzles 25 provided in each section of the condenser will be described with reference to FIG.

The eluate is condensed on the surface of the condenser (S-2, S=3 parts), passes through a partial receiver getter 31, passes through an elution receiver nozzle 25, and is injected into a rotating receiver 26. However, if the elution receiver nozzle 25 is fixed in this state, the rotary receiver 26 cannot be pulled out upwardly when the hot melting device is disassembled.

In order to eliminate the above-mentioned drawbacks and make it easy to disassemble and clean the device, the elution receiver nozzle 25 is placed in a vertical position by moving the rotary receiver 26 upward during disassembly. Partial receiving nozzle 2
The boss 34 of No. 5 engages the upper part of the partial receiver getter 31, allowing the rotary receiver 26 to move upward.

During assembly, the guide 33 attached to the inner periphery of the rotating receiver 26 comes into contact with the bottom surface of the elution receiving nozzle 25 that has been rotated to the vertical position and rotates the nozzle counterclockwise in FIG. return to position.

Next, to describe the operation of the above device, the temperature of the evaporation surface of each section is adjusted so that evaporation occurs continuously while maintaining an appropriate steady state, and the stock solution is initially fed to the uppermost stage S-1. Supply through pipe 19. The stock solution passes through the liquid dispersion tube 20, forms a uniform thin film on the evaporation surface, and evaporation begins. Further 8-2. Evaporation begins in the S-3 section as well, and once the p11 portion is sufficiently refluxed into the liquid dispersion tube 20 through the reflux pipe 27, the stock solution is supplied from the feed pipe of the S-1 section to the ps-2 portion. Switched to feed pipe. A flow sheet in this state is shown in FIG. While dropping the raw material F (composition) in a constant flow from the upper part of 8-2 parts, add S-1 part Om part C (fil composition Vl
, Yl i )] and 8-3 parts of the residue part (composition L
3. X31) is extracted while being constantly separated. At this time, the part of the s-3 part [(condensate of composition Va, Yai)] and the part of part S-2 [(condensate of composition V2゜Y21)] pass through the reflux pipe 27 and go up one stage. The light fraction is refluxed to the evaporation surface of sections S-2 and S-1, and the light fraction with a higher concentration can be condensed in the upper section.

Using a two-component stock solution of di-2-ethylhexyl phthalate (low-boiling component) and di-2-ethylhexyl sebacate (high-boiling component) as a sample, the effects of the vaporization example performed using the above apparatus were evaluated. Shown below.

Raw material supply rate 50 Ky/H Composition of stock solution 50 mo1% Distillate elution 24 Ky/H Residue liquid amount 26 K51/H Low boiling fraction composition in distillate B 5 Low boiling fraction composition in mo1% residue liquid 15 mol 1% recovery rate of low boiling components 82 mol
On the other hand, the results of a conventional non-reflux, sliding flow lowering film type apparatus, in which the same elution rate as above was obtained, are as follows.

Composition of low-boiling components in the eluate 71 mol Composition of low-boiling components in the residual solution 31 mol % recovery rate of low-boiling components
(As shown in 38 mol or more, the invention is to continuously and continuously perform mist-free uniform feeding by repeating reflux dispersion in an I-type hot melting device under sliding flow, and It has a structure with low pressure loss, and has the effect of significantly improving product purity and recovery rate compared to conventional single-heat melting type products.

Furthermore, since the elution receiving nozzle is rotatably supported in the partial receiving book at the vertical position 1, disassembly and assembly of the device is facilitated, and cleaning and maintenance are further improved.

[Brief explanation of the drawing]

The drawings show one embodiment; Figures 1 to 3 are cross-sectional views of the entire device, Figures 2 and 3 are detailed views of the liquid dispersion tube, and Figure 4 is detailed views of the rotating receiver and elution receiver. , FIG. 5 is a flow sheet. 1 is the body, 2 and 3 are flanges, 4 and 5 are lids, 6 is O-ring, 7 is rotating shaft, 8 is shaft)/Using, 9 is bearing, 10 is mechanical seal, 11 is heating jacket,
12 is a condenser, 13 is an exhaust port, 14 is a drive motor, 15
16 is a pulley on the motor side, 16 is a pulley on the rotating shaft side of the main body, 17 is a rotating arm, 18 is a sliding brush, 19 is a raw material foot nozzle, 20 is a liquid dispersion tube, 21 is a receiver, 22 is a nozzle tube, 23 is a nozzle Extraction vibe, 24 is the evaporation section nokuru, 25
2 is an elution receiving nozzle, 26 is a rotating receiver, 27 is a reflux pipe, 28 is a residue vibe, 29 is a small hole, and 30 is a small cup (-
131 is a partial getter, 32 is a fulcrum, 33 is a guide, 3
4 is the boss. Figure 1 Figure 2 Figure 3

Claims (1)

[Claims] 1. The condensation surface is divided into a large number of sections, each section is provided with a liquid dispersion tube that distributes the liquid evenly through rotation, and the condensate is transferred from the rotating receiver to the elution receiving nozzle. A reflux sliding flow lowering film type Kurobe device, characterized in that a reflux pipe is provided between each section to force reflux into a dispersion tube by centrifugal force. 2 Divide the condensation surface into a large number of sections, and each section is provided with a liquid dispersion tube that distributes the liquid evenly through its rotation, and the condensate from the elution receiving nozzle is transferred from the rotating receiver to the liquid dispersion tube by centrifugal force. A reflux sliding falling film type black part device, characterized in that a reflux pipe for forcibly refluxing is provided between each section, and the elution receiving nozzle is pivotally supported on a partial receiving getter so as to be rotatable to a vertical position.