WO1992009352A1

WO1992009352A1 - Method of and device for counter-flow separation of mixture

Info

Publication number: WO1992009352A1
Application number: PCT/JP1991/001663
Authority: WO
Inventors: Terukatsu Miyauchi
Original assignee: Terukatsu Miyauchi
Priority date: 1990-11-29
Filing date: 1991-11-29
Publication date: 1992-06-11
Also published as: JPH04197402A; GB2255916A; DE4193006T; GB9216071D0

Abstract

An improved method of and device for separating at least one kind of objective constituent from solution or solid particles containing at least kind of said objective constituents. The method of this invention is characterized in that: a multi-shaft rotary blade type tower, in which respective screw blades provided on the respective outer peripheral surfaces of at least two revolving shafts in parallel with each other are adapted to be directionally opposite to each other and to overlap partly, is used so that, when said revolving shafts revolve in the directions reverse to each other respectively, solid particles continuously fed onto the bottom of the tower are continuously fed upward; and continuous upward feeding of solid particles from the bottom of said tower toward the top thereof and continuous downward flowing of solution into the tower in counter-flow manner against said solid particles give rise to uniform and effective counter-flow contact between upward fed solid particles and downward flowing solution which are stirred with the rotation of said screw blades, whereby objective constituents in the mixture contained in the solution are distributed to solid particles so as to be separated from the solution or, on the contrary, objective ones of constituents contained in solid particles are distributed to the solution so as to be separated from solid particles. The device of this invention is a counter-flow separator including multi-shaft rotary blade type tower for performing the above-described method.

Description

Description Method and apparatus for countercurrent separation of mixture (Technical field)

The present invention relates to an improved method and apparatus for separating at least one or more eye components from a solution or a solid particle containing at least one or more eye components. .

[Background technology]

Conventionally, in order to separate at least one or more specific components from a solution containing at least one or more specific components, a solute adsorption equilibrium, exchange equilibrium, and solute between a solution and particles have been used. The continuous separation method using the distribution equilibrium and the like includes the continuous annular mouth mat graph method and the simulated moving bed type method in which the solution is intermittently switched [Higgins method and Or the Sobex method (S 0 rbe∑) method) and the fluidized-bed method, but each has its advantages, features, and disadvantages. In addition, it was usually a batch type, and the efficiency was not always good.

[Disclosure of the invention]

The present invention has solved the difficulties and drawbacks of the continuous and steady solid-liquid countercurrent method, which was conventionally considered to be difficult as a solution separation device.

This makes it more efficient and easier to operate than conventional devices, and contains at least one or more eye-catching components. A method and an apparatus for separating and purifying at least one or more components of interest using functional particles, or at least one or more components of solid particles It is an object of the present invention to provide a method and an apparatus for distributing and separating components in a solution.

According to the present invention, the screw wings attached to the outer peripheral surface of at least two parallel rotating shafts are opposite to each other in direction and partially overlap each other. In this case, the rotary shafts rotate in opposite directions, so that the solid particles continuously supplied to the bottom of the column are continuously pumped upward. Using a rotary shaft tower, solid particles are continuously pumped from the bottom of the multi-axial rotary tower toward the top of the column, and at the same time, the solution is continuously flowed down the column in a countercurrent to the solid particles. The uniform and effective countercurrent contact between the pumped solid particles and the flowing solution is achieved by the rotation of the screw blade. In other words, the component of interest in the mixture contained in the solution is distributed to solid particles and separated from the solution, or conversely, contained in the solid particles. Another object of the present invention is to provide a countercurrent separation method for a mixture, which is characterized in that a target component of the component is distributed to a solution side and separated from solid particles.

In the method of the present invention, when at least one or more components of interest are contained in the solution, solid particles having a separation function for the components of interest are used, and the solution is supplied to the top of the column. To contact the solid particles rising from the top with the countercurrent. To separate the components from the solution into the particles. When the solid particles contain at least one or more eye contact components, a solution having a separating function for the eye contact components is used, and the solution is placed at the top of the column. The supplied solid particles are brought into contact with the solid particles ascending from the bottom of the tower in a countercurrent to distribute and separate the permeated components from the solid particles into the solution.

Also, when the solution contains two kinds of eye components, a combination of solid particles and an eluent which gives different resolutions to the two eye components should be used. By feeding the solid particles from the bottom of the column, supplying the eluent to the top of the column, and supplying the solution containing the component to be separated to the middle of the column. One of the two components is separated into solid particles and the other is separated into a solution, which is removed from the top and bottom of the column and separated.

The present invention also provides that the screw wings attached to the outer peripheral surface of at least two parallel rotating shafts have opposite directions and a part of them. Solid particles continuously supplied to the bottom of the column are continuously lifted upward by the rotation shafts rotating in opposite directions. A multi-spindle rotating tower having an action of feeding the solution, and a supply port for a solution containing at least one or more eye-catching components in any part of the multi-spindle rotating tower. A solid particle supply port near the lower part of the shaft rotor tower is provided with an outlet for solid particles with at least one or more of the joint components attached near the upper part of the multi-axis rotor tower. In addition, A separation liquid extraction chamber following a solid-liquid separation plate provided with a plurality of small holes or meshes near the lower end of the shaft rotor tower, and, if necessary, a side wall of the multi-shaft rotor tower, Separated liquid discharge chamber followed by solid-liquid separation plate with multiple small holes or mesh plate provided on the part where clear wings approach each other, or both or either chamber Means to allow this or these chambers to be at normal or reduced pressure, or to force the separated liquid to be assembled by pumps Another object of the present invention is to provide a countercurrent separation device having the following features.

According to the invention, the screw wings provided on the outer peripheral surface of at least two parallel rotating shafts are opposite in direction to each other, and some of them overlap. The rotating shafts rotate in opposite directions to each other, so that the solid particles continuously supplied to the lower part of the tower are continuously pumped upward. A multi-axial rotary tower, a supply port for a solution containing at least one or more components of interest in any part of the multi-axial rotary tower, and solid particles near a lower portion of the multi-axial rotary tower. A supply port for solid particles near the lower part of the multi-shaft impeller, a flood port for eluent and / or washing liquid near the top of the multi-shaft impeller, An outlet for solid particles having at least one or more notable components is provided near the upper part, and near the lower end of the multi-spindle impeller. The screw blades are separated from each other at the separated liquid discharge chamber following the solid-liquid separation plate provided with a number of small holes or mesh plates, and, if necessary, at the side wall of the multi-axial rotary blade tower. Approach In the part on the other side, a plurality of small holes, or a solid-liquid separation plate with a net plate, followed by a separated liquid discharge chamber and / or a separated liquid extraction chamber are installed. Or means to allow these chambers to be at normal pressure or reduced pressure, or to force the pump to assemble the separated liquid. The purpose of the present invention is to provide a countercurrent separator characterized by having a countercurrent separator.

[Brief description of drawings]

FIG. 1 is a schematic longitudinal sectional view of one embodiment of the separation apparatus of the present invention, and FIG. 2 is a schematic cross-sectional view taken along the line Π of the apparatus of FIG. 1 or FIG. FIG. 3 is a schematic longitudinal sectional view of another example of the separation apparatus of the present invention.

[Best mode for carrying out the invention]

The method and apparatus of the present invention will be described with reference to FIGS. 1 to 3 which show examples thereof.

First, the apparatus shown in FIGS. 1 and 2 is used in a method for separating at least one or more eye components from a solution containing at least one or more eye components. In the case described, the multi-axis rotary wing tower 1 is composed of a cylindrical body having a combination of at least two vertically long cylinders (for example, a cocoon cross section). The screw wings 4, 4 ′ attached to the outer peripheral surface of the parallel rotating shafts 3, 3 ′ driven by the device 2 have the opposite directions to each other. A part of the towers overlaps and extends almost the entire height of the tower, and the rotation axes are opposite to each other, preferably at a constant speed. To rotate with The solid particles in the solid-liquid mixture are removed from the bottom of the multi-rotor impeller 1 from the bottom to the top of the tower, where at least one or more attached components are attached.7 It is configured to be transported to The screw blades may be continuous as shown in the drawing, or may be partially notched. The screw wings 4 and 4 ′ installed in the inside are parts that are separated from each other by rotation, and are located above the solid-liquid separation plate 5, but in many cases. A port 6 for supplying solid particles is provided on the side wall near the lower part of the rotary blade tower 1.

In addition, the screw blades 4 and 4 ′ are portions on the side closer to each other due to rotation, and at least near the upper part of the multi-axial rotary wing tower 1, at least in the raw material solution. It has an outlet 7 for the solid particles to which one or more eye components are attached.

The solid particle feed port 6 and discharge port 7 are preferably fitted with a single or doubles screw extruder.

Here, a suitable position between the supply of solid particles 6 and the outlet 7 of the solid particles to which the eye-grain component separated from the raw material solution is attached, for example, near the center thereof The position has a supply port 8 for a raw material solution to be separated, which is a solution containing at least one or more components of interest.

In the example shown in Fig. 1, an inlet 15 for the eluent and / or washing liquid is provided near the top of the multi-spindle rotor tower 1. Elute the solid particles on which the rising component is attached and / or purify by washing.

Further, a plurality of small holes or mesh plates are provided in the solid-liquid separation plate 5 at the lower portion of the multi-spindle impeller 1, and the separated liquid is provided in the solid-liquid separation plate 5. The discharge chamber 9 is connected, and is connected to the pump 11 for forcibly sending out the separated liquid through the pipe 10 from the discharge chamber 9.

The multi-spindle rotor tower 1 may be provided with a heating or cooling device as necessary.

At this time, at least one or more eye-catching components in the raw material solution have been transferred, and the attached solid particles are purified by an eluent or a washing solution, and the solid particles are removed. It is removed from the room 7. The purified adhered solid particles are sent to one end of the separation device 13, for example, the lower portion thereof by the transfer means 12 from the outlet 7, and adhered thereto. It is sent to a process that separates and collects at least one or more eye-catching components.

Here, the step of separating and recovering at least one or more adhering components adhered to the solid particles and the type of the raw material solution to be separated and the difference in the recovery mechanism. Various methods can be adopted, but in any case, the solid particles are regenerated using the eluent to recover the target component of interest. .

In addition, outside the solid-liquid separation plate 5 and the separation liquid discharge chamber 6 provided at the bottom of the tower, or in place of them, the side wall of the multi-axis rotary blade In the part where the screw blades approach each other, i.e., on the same horizontal plane or slightly below it on the side opposite to the solid particle introduction port 6, a plurality of small holes or mesh plates were used. A solid-liquid separation plate and a separated liquid discharge chamber (not shown) following the plate may be provided.

The separated liquid discharge chamber may be provided with a means (not shown) capable of increasing or decreasing the pressure.

The solid particles that have completed the recovery process are taken out from the other end of the separation device 13, for example, near the upper part thereof, subjected to other processing if necessary, and again multi-axised by the transfer means 14. It is sent to the supply port 6 of the solid particles of the rotary wing tower 1 and can be used again as solid particles for separating the component of interest in the raw material solution.

At least one or more components of interest separated in the separation device 13 may be recirculated through the supply port 15 together with an eluent and / or a washing solution, if necessary. <Next, the separated liquid from which at least one or more components of interest have been removed is removed from the solid-liquid separation plate 5 near the lower end of the multi-axial rotary tower 1. The separated liquid is taken out through the chamber 10 and sent to the next step by the pump 11.

This separated liquid can be continuously sent to another separation device as needed to perform an appropriate treatment to separate and remove the remaining other components of interest.

Next, FIG. 3 shows that at least one component of interest is included without providing the eluent and / or washing solution inlet 15 in FIG. An example is shown in which an inlet 8 for a raw material solution, which is a solution to be removed, is provided at the upper side of the multi-axis rotary wing tower 1 but on the side wall slightly lower than the lower side of the extraction chamber 7.

This device can be used as a means for separation when the solution to be separated is a simple component.

Although the above description has been made for the case where the eye component is present in the solution, similar separation is possible when the eye component is present in the solid particles.

The following can be exemplified as the objects that can be used in the present invention.

Examples of solid particles

a) Various adsorbent particles

Shi Li Ca particles, A Le Mi Na particles, C a C 0 ₃ powder, activated carbon particles of the seed s, Ze O La wells particles, molecular sieving carbon, a throat molecular adsorbent particles that have a sieving action, the species' s Hydroxypatite particles, activated clay particles, ion-exchange resin particles, particles with adsorption capacity, etc.

b) Particles capable of ion exchange.

Strong and weakly acidic ion exchange resin particles, strong and weakly basic ion exchange resin particles, balm chip particles, activated clay particles, inorganic ion exchange ability particle.

c) Various chelating resin particles capable of chelating. Organic and inorganic particles impregnated with a chelating agent (diluted with an organic solvent if necessary). . d) Porous organic or inorganic particles impregnated with an organic solvent or an aqueous solution capable of selective extraction.

e) Porous organic or inorganic particles impregnated and immobilized with gels that have a separation sieving effect, such as polystyrene gel particles.

f) Particles having affinity ability modified with a substrate having a particular affinity ability for a specific component, for example, an enzyme (eg, agarose particles) ), Particles having an affinity function utilizing an antigen-antibody reaction, particles having an affinity function by modifying pores such as porous silica, and particles having an affinity function. A swellable gel component having a fining ability immobilized in porous fine particles.

g) Particles containing various useful components or components to be removed.

The range of the average particle size of the solid particles is preferably

The tower can be operated as long as it is not more than about 5 mm and up to 5; / m, but the average particle size is preferably about 1 mm to 20 πι.

Next, the solutions containing various at least one or more components of interest to be separated are very widespread, but examples include the following: is there .

a) Separation of metal ions from aqueous solutions containing various metal ions.

b) Biochemistry from aqueous solutions containing various biochemicals Separation of substances. For example, amino acids, enzymes, proteins, nucleic acids, and antibiotics.

c) Separation of active ingredient from natural product extract.

d) Decolorization, deodorization and purification of chemicals and foods.

e) Separation of components of interest from aqueous or organic solvent solutions containing various chemicals.

f) A solution that has the function of selectively distributing the spotting component from solid particles containing various useful components or components to be removed. For example, selective solvents or eluents.

The function of the separation device used in the present invention is to separate at least one or more eye components contained in a solution containing at least one or more eye components. For example, a multi-axis rotary tower may be used to separate a solution containing at least one or more components of interest, which is a raw material to be separated, for separation. Supply from supply port 8 of 1.

Next, the solid particle supply port 6 is located above the solid-liquid separation plate 5 in the multi-spindle impeller 1 but near the lower part of the multi-spindle impeller 1. Supply solid particles.

In the multi-axis rotary wing tower 1, the screw wings attached to the outer peripheral surface of the parallel rotary shaft are opposite to each other in direction, and a part thereof overlaps. And a slurry state in which the raw material solution to be separated from the solid particles by the rotation axes rotating in opposite directions is mixed. Therefore, there is not enough horizontal space on the side where the screw wings overlap each other. The liquid is squeezed out by being stirred and mixed and pressurized, and the slurry is depressurized on the side where the screw wings are away from each other. In other words, it absorbs the liquid flowing down by relaxation and promotes solid-liquid contact.

At that time, adsorption equilibrium, exchange equilibrium, partition equilibrium, solubility, affinity, etc., between the solid particles and at least one or more of the components to be separated in the raw material solution. Due to differences in exclusion function due to differences in molecular size, differences in physical and chemical properties such as chemical structure, etc. One or more of the components of interest are rapidly absorbed, adsorbed, dissolved, bonded, etc., to the solid particles and adhere to them.

The solid particles to which at least one or more of the eye components to be separated are attached are sufficiently stirred horizontally with the solution to be separated, mixed and squeezed. Solids with at least one or more eye contact components due to the rotation of the screw wings due to the release of the slurry generated and the liquid flowing down. The particles are sent upward.

Next, on the side where the screw blades move away from each other, the slurry relaxes and absorbs the liquid flowing down from above, causing it to swell. It becomes Lee. The swollen slurry is then sent to the side where the screw wings approach each other and are overlapped with each other, where they are pressurized. The liquid is discharged, and the discharged liquid flows downward. As a result, the solid particles come into countercurrent contact with the raw material solution. The solid particles to which at least one or more eye-catching components should be separated in the raw material solution rise as the screw blades rotate, and finally multi-rotor blades The solid particles near the upper part of 1 are discharged from the outlet 7.

At this time, the eluent is used to elute the solid particles to which the eluting components rising from the inlet 15 of the eluent and / or the washing liquid placed near the top of the multi-axis rotary blade tower 1 are attached. And, by flowing down the washing solution, it is possible to purify the eye-grain component attached to the solid particles.

Elution of solid particles to which the multi-spindle rotor tower 1 adheres depending on the type and amount of at least one or more of the components to be separated in the raw material solution. And / or in some cases the washing operation is unnecessary. In that case, you can use the equipment shown in Fig. 3.

Next, it is sent to a device 13 for separating and recovering at least one or more kinds of eye components adhering to the solid particles by the transfer step 12.

Now, when the solution to be separated contains two components (referred to as “A + B”) as the eye-catching component, A and B are separated. When each of them is to be separately taken out, the raw material solution 中 Α + Β containing intermediate feed solution ”is supplied from the supply port 8 at the approximate center of the multi-spindle impeller 1 shown in Fig. 1. Supply.

One of the two components, A, is selectively distributed to the solid particles, adheres to the solid particles, and ascends in the multi-axis rotary blade tower 1. If another combination of the component B and the solution and the solid particles is selected so that the component B is distributed by the liquid and flows down the column, the component B starts from the top of the multi-axis rotating blade tower 1. A is attached to the solid particles and discharged from the solid particle outlet 7, and B is discharged from the separated outlet chamber 10 at the bottom of the column along with the separated liquid. , A and B are separated. '

The principle of separation is as described above, but in some cases, in order to achieve sufficient separation and concentration, the solid particles adhering mainly to the discharged A component are regenerated. Then, a part of the separated A component is added to the eluent entering from the top of the tower, and returned to the column together with the liquid (this is called “top reflux”), and the A component is separated. , Purification and concentration.

Similarly, B is recovered from the separated liquid mainly containing B component discharged from the bottom of the tower, and a part of the recovered B is distributed to regenerated solid particles. It can also be returned to. (This is called "bottom reflux.")

The effectiveness of the top and bottom reflux depends on the separation mechanism.

Second, if the solution contains many components (A + B + C +…) that must be separated.

In general, a solution contains two or more n components, and it is necessary to use (η — 1) multi-axis rotating blade towers to separate each component. There is, but in principle,

(A + B) → (A) + (B) This is a repetition of the separation of the two-component system described above.

Next, if the solution contains only one component (referred to as “A”), the solution containing A is, for example, near the top of the tower in Figure 3. The raw material solution is supplied to the raw material solution inlet 8, and is contacted with the solid particles fed from the solid particle inlet 6 while flowing down the inside of the multi-axis rotating blade tower 1, and is mixed therewith. The A component adheres to the solid particles by being squeezed, and the solid particles to which the A component adheres rise in the multi-spindle rotor tower 1 and are taken out from the attached solid particle outlet 7 to be separated and collected. In device 13 A is separated by suitable means. The regenerated solid particles are recycled to the multi-spindle rotor tower 1.

As a means for separating A, for example, selective elution can be performed using an eluent.

The type and mechanism of operation of the separation / recovery device 13 described above are specifically determined by the type of solid particles and the component to be separated, but are generally worn. It can be separated by a solution called the eluent of the eye component.

Next, the separated liquid from which at least one or more of the eye-dropping components has been removed flows down the multi-spindle impeller 1, and is supplied to a separated liquid extraction chamber provided below the solid-liquid separation plate 5. Are taken out.

After the solid particles from which the sedimentary components have been removed by the above-mentioned separation and recovery device 13, the solid particles are subjected to other treatments as necessary, and then again subjected to the multi-axis rotation by the transfer process 14. It can be sent to the wing tower 1 for recirculation and use. On the other hand, the separated liquid from which at least one or more notable components have been removed from the raw material solution gradually flows down the multi-axis rotary blade tower 1, passes through the solid-liquid separator 5, and is collected in the separated liquid chamber 9. And pipe 1

0, discharged by pump 11.

If necessary, this separated liquid is sent to another similar device and subjected to a separation treatment to further remove the remaining other eye-contacting components as described above. I can do it.

These are described when the eye component is present in the solution, but when the eye component is present in the solid particles, the eye component is added to the solution by the solid particles and the feed solution. A similar distribution as described above occurs between and and it is possible to separate the components of interest as well.

(Example)

<Example 1> Separation of fructose from an aqueous fructose solution.

Using a small laboratory two-axis rotary wing tower (tower diameter 5 cm, tower height 160 cm) as shown in Fig. 3, rotating the double screws in opposite directions I used it.

The solid particles supplied to the bottom were raised from the bottom toward the top by the action of a screw. On the other hand, the raw material solution is supplied to the top of the column, and while flowing down the column, the rotation of the double squirrel allows uniform and effective countercurrent to the planar particles rising in the column. After contacting at, it is discharged from the bottom of the tower.

Strongly acidic ion-exchange resin (sulfuric acid type, with a degree of cross-linking of 10 and an average particle size of 6) treated with a 0.1 mol aqueous solution of calcium chloride beforehand Fructose recovery It was used as functional solid particles. The operation was carried out at 20 ° C under atmospheric pressure. Immediately, the canopy-form strongly acidic ion exchange resin was used as the particle phase, and the superficial velocity of the particle phase was reduced to 3 ° C. ^{. 0 m 3 u / 'm} "9 forced in continuous 1¾ to column bottom or et at hr, whereas the concentration 5 5 results aqueous saccharide solution to column imperative et superficial velocity of ^{^{g 1 5 m J / m 2}} hr And the particles were ascending uniformly in the column and in contact with the countercurrent.

After the condition in the tower became steady, the concentration of fructose in the aqueous fructose solution discharged from the bottom of the tower was measured using a refractometer, and the average concentration was 2.8 g κ1. there were. Now, the fructose recovery rate by particles is determined by the concentration of the stock solution 1 and the concentration of the effluent 1

Recovery rate = X 100%

If defined as the stock solution concentration gZ1, the average fructose recovery rate is 95%.

However, the superficial velocity is assumed to mean that the interior of the tower is completely empty, and that particles or liquids have flowed through the empty tower, respectively, with each of them being filled with a full volume. The flow velocity at the time of flight is also called the apparent flow velocity.

It becomes.

<Example 2> Separation of glucose and fructose.

Small laboratory two-axis rotor shown in Figs. 1 and 2 Using a tower (effective height: 160 cm, diameter: 5.0 cm (circular diameter that is cocoon-shaped and constitutes a circular shape)), the double screws 4, 4 'are connected to each other. Then, it was rotated in the opposite direction, and a strongly acidic cationic resin with an average diameter of 60, which was functional solid particles, was supplied from the solid particle supply port 6 at the bottom of the twin-screw rotor blade.

The operation was performed at room temperature under atmospheric pressure.

From the aqueous sucrose solution obtained by dissolving glucose and fructose, the same strongly acidic ion-exchanged resin as the calcium type used in Example 1 was used as the functional solid particles. To separate glucose and fructose.

Immediate Chi, Yi on-exchange resin particles were added continuously fed with 2 bottom or al superficial velocity third axis rotary wing ^{^{tower. O m 3 Z m 2 hr}} .

Also, the superficial velocity 1 of water column top or colleagues as the eluent. 0 m ³ / m continuously flow down at ² hr, blanking de as a separation target raw material solution for the tower central section at the same time An aqueous solution of sugar and fructose

It was continuously supplied at a superficial velocity of 0.50 m ³ / m ² hr. <11

It contains 50 g of pudose sugar and fructose. When the aqueous solution enters the column, it is mixed with the aqueous phase flowing down from the top of the column by the action of the rotating screw. In addition, the particles are uniformly contacted with the particles rising in the column, flow countercurrently to the particles, flow down in the column, and are discharged from the bottom of the column.

By this operation, fructose is selectively distributed to the functional solid particles, discharged together with the resin particles from the top of the column, and glucose is removed. The first is to selectively distribute water flowing down, regenerate the sugar contained in the particles discharged from the bottom of the column to form an aqueous solution, and together with the aqueous solution discharged from the bottom of the column. The results of the analysis of the sugar concentration using a refractometer are as follows: 7 <-o

Immediately from the top of the column, 77% by weight of fructose (the rest is pudose), and from the bottom, 77% by weight of the fructose (the rest is fructose). I got it.

Example 3> Separation of a mixture of phenol and toluene.

As the solid particles regenerated by using the apparatus shown in FIG. 1, FIG. 2 and Example 2, styrene-based porous synthetic resin sphere particles are used as the solid particle supply port at the bottom of the tower. The height of the tower was raised at a superficial velocity of 3.0 m ³ / m ² hr. Also, the tower imperative et supplies METHANOL solution at a superficial velocity ^{^{2 5 m J / m 2 h}} r:. A ^ is Ru resin particles Ru is continuously countercurrent contact. All operations were performed at room temperature.

The raw material liquid to be separated is a methanol solution containing 0.1 mol / mol of phenol and 0.1 mol of toluene, respectively. Then, the raw material solution is continuously supplied from the inlet 8 of the raw material at the center of the tower at a superficial velocity of 0.5 πι 3 ^ύ / πι 2 ^{ώ 1} ΐ, and flows down the tower. And the mixture was mixed uniformly.

By performing the above operations, the phenol is distributed in a large amount to the liquid, discharged together with the liquid from the separated liquid taking-out chamber 9, and is analyzed by an ultraviolet spectrophotometer (250 nm). As measured, its purity is 80% (mosoole% of phenol in phenol and phenol). Was

Toluene was distributed and attached to the solid particles in a large amount, and was discharged together with the particles from the outlet 7 for the solid particles at the top of the tower.

The adhered particles were regenerated by a regenerator 13 and the purity of truene obtained in this way was 72%.

Example 4> Separation of proteins by fine hydroxyapatite particles.

Using a device similar to that used in FIG. 1, FIG. 2 and Example 2, as the functional solid particles, regenerated fine hydroxya having an average particle size of 35 nm was used. The particles of the pattern crystal are introduced from the solid particle supply port 6 at the bottom of the tower, and are raised in the tower at an empty tower speed of 1.0 m3 mhr. The operation was performed at room temperature at the inlet of the separated solution 15 near the top of the column. The phosphate concentration was adjusted to 170 mM calcium phosphate buffer.

(Κ ₂ Η Ρ 0 ^ and Κ 。. An aqueous solution in which ₄ 04 is dissolved in equimolar is called potassium phosphate buffer. Also, 水溶液 Ο 4 contained in this buffer the concentration is defined as-phosphate concentration, the concentration of the buffer was Table Wa.) superficial velocity 1. 5 m ^d arsenide de passed down that rises in mhr b key sheet § Pas data Say it

B said the particles were in continuous countercurrent contact.

The raw material feed solution to be separated by contact with the hydroxyapatite crystal particles is a phosphoric acid having a phosphoric acid concentration of 1.0 millimol. A mixture of diluted lysozyme and cytochrome C dissolved in a buffer solution. It is an aqueous solution that has been dissolved to a total concentration of 0.1 millimoles Z1.

This feed liquid is continuously supplied at a superficial velocity of 0.1 lm ³ / m ² hr from the raw material solution inlet 8 located at the approximate center of the tower, and the rotating liquid is fed. It flows down in the tower by the mixing action of the clean wings. After it is uniformly mixed with 170 milliliters of potassium phosphate buffer, it flows down in the tower.

By performing the above operations, lysozyme was obtained from the bottom of the column with the buffer solution, and its purity was 85 mol%. In addition, from the top of the tower, cytochrome C selectively adsorbed to the hydroxyapatite crystal particles was obtained. The purity of cytochrome C in the eluate obtained by the elution was 82 mol%.

(Industrial applicability)

The present invention relates to the separation of at least one or more of the ingredients contained in the solution or the solid particles, which contain at least one or more of the ingredients as raw materials. By using the method and the device of the present invention, it is possible to perform continuous and extremely efficient separation as compared with the conventional method. It can be effectively used for separation of biochemical substances from an aqueous solution containing various biochemical substances such as acids, enzymes, and proteins.

Claims

The scope of the claims

1. The screw wings attached to the outer peripheral surface of at least two parallel rotating shafts are opposite in direction to each other, and a part of them is overlapped. As the rotating shafts rotate in opposite directions, the solid particles continuously supplied to the bottom of the column are continuously pumped upward. The solid particles are continuously pumped from the bottom of the multi-axis rotating blade tower toward the tower top, and simultaneously with the solid particles. By continuously flowing the solution in the countercurrent in the counter-current, the rotation of the screw blades enables uniform and effective communication between the discharged solid particles and the flowing solution. The countercurrent contact allows the components of the mixture contained in the solution to be distributed to the solid particles and separated from the solution, or vice versa. Countercurrent separation process of the mixture characterized and paying attention this component you separation or solid particles found by distributed solution side in components are Ru contained in the solid particles child.

2. When the solution contains at least one or more eye-catching components, use solid particles that have a separation function for these eye-catching components, and the solution is placed at the top of the tower. The countercurrent separation method according to claim 1, wherein the component is supplied and brought into contact with the solid particles rising upward from the bottom of the tower and in a countercurrent to distribute and separate the target component from the solution into the particles. .

3-Solid particles contain at least one or more notable components When this is done, a solution that has a separation function for this component is used, and the solution is supplied to the top of the column, and the solid particles that rise from the bottom of the column and the countercurrent flow The method according to claim 1, wherein the contact component is separated from the solid particles into the solution by contacting the solid particles with the solution.

4. When the solution contains two species of the eye component, a combination of solid particles and an eluent that gives different resolutions to the two eye components. By using the combination, the solid particles are fed from the bottom of the column, the eluent is supplied to the top of the column, and the solution containing the component to be separated is supplied to the middle of the column. Thus, one of the two components is separated into solid particles, and the other is separated into a solution and removed from the top and bottom of the column and separated. The countercurrent separation method according to claim 1

5. The screw wings attached to the outer peripheral surface of at least two parallel rotating shafts are opposite to each other, and some of them overlap. The solid particles supplied continuously to the bottom of the tower are continuously pumped upward by rotating the rotating shafts in opposite directions to each other. A multi-axial rotary tower having a function of supplying a solution containing at least one or more components of interest in any part of the multi-axial rotary tower. A supply port for solid particles is provided near the lower part of the wing tower, and a discharge port for solid particles having at least one or more of the joint components is provided near the upper part of the multi-axis rotary wing tower. A multi-rotor tower with a plurality of small holes or mesh plates near the lower end A plurality of small holes or mesh plates are provided at the portion where the screw blades approach each other in the separated liquid discharge chamber following the liquid separation plate and, if necessary, on the side wall of the multi-axis rotary blade tower. A liquid-removal chamber and / or a chamber for separating the separated liquid that follows the solid-liquid separation plate that is provided with Or a means for enabling forced separation of the separated liquid by a pump.

6. At least the screw wings attached to the outer peripheral surface of the two parallel rotating shafts are oriented so that their directions are opposite to each other and some of them overlap each other. A multi-axis rotary blade having an operation of continuously pumping solid particles continuously supplied to the lower part of the tower upward by rotating the rotary shafts in directions opposite to each other. A supply port for a solution containing at least one or more components of interest in any part of the multi-spindle tower, and a supply port for solid particles near the lower part of the multi-spindle tower A supply port for solid particles near the lower part of the multi-shaft impeller, a supply port for eluent and / or washing liquid near the top of the multi-shaft impeller, and a small amount near the upper part of the multi-shaft impeller. In particular, an outlet for solid particles to which one or more components of interest are attached is provided, and a plurality of small holes and holes are provided near the lower end of the multi-axis rotating blade tower. Or, a separated liquid discharge chamber following a solid-liquid separation plate provided with a mesh plate, and, if necessary, a portion of the side wall of the multi-axis rotary blade tower on which the screw blades approach each other. Solid-liquid separation plate with multiple small holes or mesh plate And / or one or more chambers for the separated liquid removal chambers, and either or at normal or reduced pressure in these chambers or pumps A countercurrent separation device characterized in that it has means for forcibly assembling the separated liquid by the method described above.