WO2009036617A1

WO2009036617A1 - A solid catalyst reactive arrangement and its running method

Info

Publication number: WO2009036617A1
Application number: PCT/CN2007/003293
Authority: WO
Inventors: Caike Jin; Jun Wang
Original assignee: Bioright Worldwide Company Limited
Priority date: 2007-09-21
Filing date: 2007-11-21
Publication date: 2009-03-26
Also published as: CN101392244A; CN101392244B; HK1130832A1

Abstract

A solid catalyst reactive arrangement comprises a reactive vessel and a solid catalyst within the vessel, wherein the solid catalyst has a first end-face, a second end-face and a periphery extending between the two end-faces and being enwrapped with a waterproofing membrane. A running method of the arrangement comprises injecting reactive fluids into the reactive vessel, wherein the fluids enter into the solid catalyst via its first end-face, are confined by the waterproofing membrane and flow toward the second end-face of the catalyst while reacting with the catalyst, then the resulting solution effuses from the second end-face of the catalyst. The arrangement and the running method enable to assemble and disassemble the solid catalyst easily, avoid the short circuit due to the effusion of reactive fluids from the periphery and the deformation/shrinkage of the catalyst during running, then improve reactive efficiency and running efficiency.

Description

Solid phase catalyst reaction device and operation method thereof

The present invention relates to the field of biocatalyst technology, and in particular to a solid phase catalyst reaction device and a method for operating the same. Background technique

With the development of biotechnology, enzymes have become widely used as biocatalysts in industrial and other fields. In the above applications, the enzyme or the enzyme-containing cells are usually present in an immobilized form. This is because immobilized enzymes or immobilized cells tend to be more stable than free enzymes, and are easily separated from the product, which is easy to recycle and reuse, and is easy to store and transport.

Usually, the immobilized enzyme or the immobilized cells are used in a granular form for suspension reaction or filled in a container of a reaction device to constitute a stationary phase, and react with a substrate solution flowing between the particles. However, in the above case, the substrate solution is generally difficult to enter the inside of the particles, so that the enzyme molecules embedded in the deep layers of the particles are difficult to participate in the catalytic reaction, resulting in inefficiency.

In order to overcome the above disadvantages of the granular immobilized enzyme or the immobilized cell, the present inventors have proposed a novel structure of immobilized enzyme or immobilized cell, as disclosed in the publication No. "CN1982445", and the name of the invention is "preparation for preparation". Chinese patent application file for "enzyme or immobilized cell carrier and immobilization method using the carrier". The novel immobilized enzyme or immobilized cells have an open-cell three-dimensional lattice structure, which increases the chance of contact between the enzyme molecule and the substrate solution, increases the contact area, and improves the reaction efficiency.

One of the application methods of the immobilized product (immobilized enzyme or immobilized cell) of the novel lattice structure is to wind the strip-shaped immobilized product into a cylindrical reel structure, and the cylindrical structure of the reel structure The immobilized product directly constitutes a reaction column, or a plurality of cylindrical fixed products of such a reel structure are stacked up and down to form a reaction column as a whole, and then The reaction column is placed in a reaction vessel. For example, the Chinese Patent Application Publication No. "CN1982445", the disclosure of which is incorporated herein by reference to the entire entire entire entire entire entire entire entire entire entire entire contents The cylindrical solid phase enzyme (i.e., the immobilized product) can be used as a module to stack a plurality of such modules up and down to form a reaction column, and then the reaction column is loaded into the reaction vessel. The gap between the reaction column and the vessel wall (hereinafter referred to as the column wall gap) is naturally blocked by the solid phase enzyme block itself or the wrapping material on the surface thereof, or is filled with granular immobilized enzyme or immobilized cells. In fact. Thus, the solid phase enzyme in the container as a whole constitutes a reaction column.

However, in practical applications, the solid phase catalyst reaction apparatus provided by the above prior art inevitably has the following drawbacks:

First, since there is no gap between the solid phase enzyme block constituting the reaction column and the container wall of the reaction device, in addition to the need to overcome the weight of the enzyme block itself, it is necessary to overcome the enzyme block and the container when the solid phase enzyme block is taken out. The large frictional resistance between the walls makes it difficult to remove the solid phase enzyme block.

Second, under some industrial conditions, such as high temperature and long-term operation, the solid phase enzyme block constituting the reaction column will gradually deform/contract during operation, causing a gap between the enzyme block and the container wall to cause a short circuit. This allows a portion of the substrate solution to flow away without reacting with the solid phase enzyme, resulting in inefficient reaction and also lowering the operating efficiency of the reaction apparatus. The term "short circuit" as used in this application means that the substrate solution does not react directly with the solid phase enzyme and flows away directly from the column wall gap. Summary of the invention

In order to solve the above technical problems, the present invention provides a solid phase catalyst reaction device and a method for operating the same, which can facilitate a reaction column containing a solid phase catalyst such as an immobilized enzyme to be easily charged and taken out, and can be prevented from entering the reaction column. The liquid flows directly from the cylinder and the solid phase catalyst undergoes deformation/contraction during operation to cause a short circuit, thereby improving the reaction efficiency and operating efficiency.

To this end, the present invention provides a solid phase catalyst reaction apparatus comprising a reaction vessel and a solid phase catalyst disposed in the reaction vessel, the solid phase catalyst having a first end surface into which the reaction liquid can flow, and a product solution after the reaction a second end surface that flows out and a circumferential surface that extends between the first end surface and the second end surface. Wherein, a waterproof film is wrapped on the circumferential surface of the solid phase catalyst.

The solid phase catalyst reaction apparatus provided by the present invention further comprises an interface disk which is in close contact with the second end surface of the solid phase catalyst. The interface disk has a cavity structure and has the following parts: a third end surface having a liquid inlet groove and a second end surface of the solid phase catalyst for supporting the solid phase catalyst and Collecting a liquid from the solid phase catalyst; a fourth end surface on which a water outlet is provided for discharging the liquid in the interface disk outward; and a sealing extending between the third end surface and the fourth end surface The circumferential surface, together with the fourth end surface, constitutes a chamber for containing the liquid.

Wherein, the water outlet is an outlet pipe. Preferably, a wall of the outlet pipe section located in the inner cavity of the interface disk is provided with a hole through which liquid in the interface disk can flow into the outlet pipe.

Wherein the waterproof film extends to the interface disk, and the peripheral surface of the solid phase catalyst and the peripheral surface of the interface disk are wrapped together.

Wherein the waterproof film wraps the circumferential surface by means of an adhesive. The adhesive may include hot melt adhesive, adhesive plaster, carpet adhesive.

Preferably, the outer surface of the waterproof membrane is wound with a fastening tape for fastening the waterproof membrane so that the waterproof membrane is more firmly wrapped on the circumferential surface.

Wherein, the waterproof film is a plastic film.

Wherein, the solid phase catalyst has a columnar shape. The columnar solid phase catalyst may be wound from a sheet; it may also be made of a particulate solid phase catalyst.

Preferably, the solid phase catalyst has a central axis. Thus, the solid phase catalyst can It is wound from a sheet around the central axis. Moreover, the central shaft may be fixed to a central portion of the interface disk.

Wherein, the reaction device adopts a cis-mounting manner, that is, the solid phase catalyst is on the interface tray, and the reaction liquid enters the solid phase catalyst from the first end surface of the solid phase catalyst located above, and The top-down infiltrated flow reacts with the solid phase catalyst, and the reacted product solution is collected and discharged by the interface tray located below. Alternatively, the reaction device is in a reverse mounting manner, that is, the solid phase catalyst is under, the interface plate is on, and the reaction liquid enters the solid phase catalyst from the first end surface of the solid phase catalyst located below, and The bottom-up is infiltrated and reacted with the solid phase catalyst, and the reacted product solution is collected and discharged from the interface tray located above.

Wherein, the reaction vessel is a column tank. Preferably, the column can includes a can lid, and the can lid and/or the bottom of the can is provided with a liquid inlet through which the reaction liquid enters into the column can. More preferably, the can lid and/or the bottom of the can is provided with a central opening for the central axis of the solid phase catalyst and/or the outlet tube of the interface disk to extend.

Preferably, the tank wall of the column tank is an interlayer, and the outer wall of the interlayer is provided with a constant temperature water inlet and outlet for introducing constant temperature water into the interlayer for heat preservation. Alternatively, the can wall of the column can is a single layer, and the outer wall is covered with a heat insulating cotton and/or polyurethane foam material.

The present invention also provides a method for operating a solid phase catalyst reaction device, specifically: injecting a reaction liquid into a reaction vessel, allowing the reaction liquid to enter through the first end surface of the solid phase catalyst, and Under the constraint of the waterproof membrane, the second end surface of the solid phase catalyst flows while reacting with the solid phase catalyst, and the product solution after the reaction flows out from the second end surface of the solid phase catalyst. a gap between the inner wall of the reaction vessel and the waterproof membrane rises to the top of the solid phase catalyst, enters the solid phase catalyst from a first end surface located at the top, and is in the solid phase under the constraint of the waterproof membrane The catalyst is infiltrated downward in the flow while simultaneously reacting with the solid phase catalyst The reaction is carried out, and the product solution after the reaction flows out from the second end face at the bottom of the solid phase catalyst. Alternatively, the reaction liquid enters the reaction vessel from the top of the reaction vessel, flows down the gap between the inner wall of the reaction vessel and the waterproof membrane to the bottom of the solid phase catalyst, and is formed by the first end surface at the bottom. Entering the solid phase catalyst and infiltrating upward in the solid phase catalyst under the constraint of the waterproof membrane while reacting with the solid phase catalyst, the product solution after the reaction is from the top of the solid phase catalyst The second end faces out.

Preferably, the reaction device further comprises an interface plate which is in close contact with the second end surface of the solid phase catalyst, and the interface plate has a cavity structure and has the following parts: that is, a liquid inlet groove is provided thereon And a third end surface which is in close contact with the second end surface of the solid phase catalyst, and a fourth end surface of the water outlet and a closed circumferential surface extending between the third end surface and the fourth end surface are disposed thereon. Wherein the reaction liquid entering the solid phase catalyst reacts with the solid phase catalyst, and the product solution flows out from the second end surface of the solid phase catalyst, and is collected through the third end surface of the interface plate. The interface disk is then discharged through the water outlet of the interface disk.

Preferably, the container wall of the reaction vessel is an interlayer, and the operation method further comprises the step of introducing constant temperature water into the interlayer for heat preservation.

Compared with the prior art, the solid phase catalyst reaction apparatus and the operation method thereof provided by the present invention have the following beneficial effects:

In the solid phase catalyst reaction device provided by the present invention, the peripheral surface of the solid phase catalyst is coated with a water repellent film, and the water repellent film can make the reaction liquid in the reaction device only from the first end surface of the solid phase catalyst (ie, The open end face enters into the interior of the solid phase catalyst, and the reaction liquid entering the solid phase catalyst does not flow out through the peripheral surface, but must flow inside the solid phase catalyst, thereby increasing the contact of the reaction liquid with the solid phase catalyst. The probability, in turn, increases the reaction efficiency of the solid phase catalyst and the operating efficiency of the reaction apparatus.

Second, the solid phase catalyst reaction device provided by the invention is encapsulated during operation. The pressure at each point in the gap between the water-repellent membrane of the phase catalyst and the vessel wall is always slightly greater than the pressure at the same height point in the solid phase catalyst, and this pressure difference forces the water-repellent membrane to always adhere to the peripheral surface of the solid phase catalyst. Even if the solid phase catalyst is deformed/contracted during operation, the waterproof membrane will adhere to the peripheral surface of the phase catalyst under the pressure difference described above.

The solid phase catalyst in the reaction apparatus can sufficiently react with the reaction liquid, thereby improving the reaction efficiency of the solid phase catalyst and the operating efficiency of the reaction apparatus.

Thirdly, in the operation of the solid phase catalyst reaction device provided by the present invention, the gap between the waterproof membrane enclosing the solid phase catalyst and the vessel wall is always filled with the reaction liquid, so that the waterproof membrane is simultaneously received from the inner side of the soft wall layer (ie, The pressure generated by the liquid from the solid phase catalyst, and the pressure generated by the liquid from the outside of the soft wall layer (ie, from within the gap), thus preventing the soft wall layer from bearing only one direction The pressure is expanded and ruptured, so that the reaction liquid in the solid phase catalyst flows out through the ruptured soft wall layer. Therefore, the solid phase catalyst reaction apparatus and the operation method thereof provided by the present invention can avoid short circuit.

Fourth, the solid phase catalyst reaction device provided by the present invention comprises a reaction vessel and a solid phase catalyst. The vessel wall of the reaction vessel is called a hard wall layer of the reaction device, and a waterproof membrane is wrapped on the circumferential surface of the solid phase catalyst. The membrane constitutes the soft wall layer of the reaction device. During the operation of the reaction apparatus, a gap is always maintained between the soft wall layer and the hard wall layer, that is, the waterproof membrane enclosing the solid phase catalyst is not in contact with the container wall. Thus, when the solid phase catalyst coated with the waterproof membrane is loaded and unloaded, the solid phase catalyst and the waterproof membrane wrapped around the peripheral surface thereof are not in contact with the container wall, so that there is no frictional force with the container wall, thus, handling and unloading It is only necessary to overcome the gravity of the solid phase catalyst and the waterproof membrane itself. Therefore, the solid phase catalyst reaction apparatus provided by the present invention is easy to handle.

DRAWINGS

The present invention will be described in detail below with reference to the accompanying drawings, specific embodiments, and application examples. Bright.

1 is a schematic structural view of an interface disk used in the present invention;

2 is a schematic structural view of a column can used in the present invention;

3 is a schematic view showing the structure of a solid phase catalyst reaction device using a cis-mounting method provided by the present invention;

Figure 4 is a schematic view showing the structure of a solid phase catalyst reaction device using a reverse mounting method provided by the present invention;

Fig. 5 is a schematic view showing the structure of a conventional reaction apparatus in the prior art. detailed description , . The present invention provides a detailed description of the solid phase catalyst reaction apparatus provided by the present invention.

The solid phase catalyst reaction apparatus provided by the present invention comprises a reaction vessel and a solid phase catalyst placed in the vessel. Among them, the solid phase catalyst may be columnar, but is not limited thereto. For convenience of explanation, the columnar solid phase catalyst is exemplified below, and the solid phase catalyst is referred to as a solid phase catalyst reaction column or a reaction column together with a waterproof membrane coated on the circumferential surface thereof (column), and The columnar solid phase catalyst not coated with the waterproof membrane is called a solid phase catalyst reaction column column or a reaction column column. As for the waterproof film, it may be a soft film having a waterproof function such as a plastic film.

The reaction vessel may be a column tank, but is not limited thereto. The upper end of the column can be provided with a can lid that can be fully opened to facilitate loading and unloading of the reaction column. Both the bottom of the tank and the lid of the tank may be provided with inlet ports. Preferably, the inlet ports themselves are inlet pipes or are provided with inlet pipes.

Next, how to prepare the solid phase catalyst reaction column and the reaction apparatus used in the present invention will be explained.

First, a solid phase catalyst for producing a columnar scroll structure, that is, a solid phase catalyst reaction Column column. For example, a cylindrical reel structure can be manufactured according to the method described in the aforementioned Chinese Patent Application Laid-Open No. CN 1982 445, entitled "Essence for the Preparation of Immobilized Enzyme or Immobilized Cells and Immobilization Method Using the Carrier" Solid phase catalyst. The column has a first end surface into which the reaction liquid can flow (that is, an open end surface of the column), a second end surface through which the product solution after the reaction can flow out, and an extension between the first end surface and the second end surface The circumference of the surface.

Then, the cylinder of the column of the solid phase catalyst reaction column is sealed with a water-repellent membrane to obtain a solid phase catalyst reaction column.

Finally, the obtained solid phase catalyst reaction column is installed in a reaction vessel such as a column tank to obtain a solid phase catalyst reaction apparatus.

Preferably, the solid phase catalyst reaction column further comprises an interface disk stacked on the column of the solid phase catalyst reaction column. The so-called interface disk refers to a cylindrical or disk-shaped cavity container for collecting and containing liquid from the column of the reaction column. The inflow face of the interface disk (ie, the end face that is in contact with the column of the reaction column and from which the liquid from the column of the reaction column flows into the interface plate, also referred to as the third end face) has a mesh or has a mutual communication a ring groove structure, the liquid from the column of the reaction column flows into the interface plate by means of the mesh or the multi-ring groove structure; the outflow surface of the interface plate (ie, away from the column of the reaction column and the liquid in the interface plate is discharged therefrom) The end face, also referred to as the fourth end face, may be provided with a water outlet through which liquid in the interface disk is discharged. The interface plate has a cylindrical surface that is sealed to contain liquid. More preferably, the shape and size of the inflow face of the interface disk matches the shape and size of the second end face of the column of the reaction column.

The reaction column with the interface plate can be installed into the reaction vessel in two ways: cis (ie, the interface plate is below, the solid phase catalyst is on) and the trans (ie, the interface plate is on, the solid phase catalyst is under ). When the cis-mounting method is adopted, the reaction liquid enters the reaction column from the first end surface located at the top of the reaction column, and is immersed downward to react with the solid phase catalyst, and the product solution is merged into the interface plate at the lower part of the reaction column, and is passed through the interface plate. The outlet of the water flows out. Adopt In the reverse installation mode, the reaction liquid enters the reaction column from the first end surface located at the bottom of the reaction column, and is infiltrated upward to react with the solid phase catalyst, and the product solution is recirculated into the interface plate at the upper portion of the reaction column, and is discharged through the interface plate. The nozzle is flowing out.

In addition, a central axis can also be fixed on the interface plate. The center axis is a pillar of the solid phase catalyst reaction column, which may be located at the center of the reaction column, for example, it may serve as a winding center of the strip-shaped solid phase catalyst. The central axis can extend through both ends of the reaction column.

The interface disk used in the present invention will be further described below with reference to the accompanying drawings.

Referring to Figure 1, the interface disk used in the present invention includes a center shaft 1, an interface plate 2, and a water outlet pipe 4. Wherein, the interface plate 2 is a disc-shaped cavity structure, and the inflow surface thereof is a bonding surface with a solid phase catalyst, and the bonding surface is made of a mesh plate with a mesh, so it is called a mesh surface 3; An outlet pipe 4 is provided on the surface. The center shaft 1 is fixed to the center of the mesh surface 3 of the interface plate 2 for winding a strip-shaped solid phase catalyst, for example, a solid phase enzyme. The outlet pipe 4 is inserted into the inner cavity of the interface plate 2 and fixed to the center of both sides of the interface plate 2, that is, the center of the inner cavity. A part of the outlet pipe 4 located in the interface plate 2 has four through-holes 5 therethrough. In practical applications, the product solution after the reaction solution of the substrate solution and the solid phase enzyme can enter the inner cavity of the interface plate 2 through the mesh of the mesh surface 3, and then collects into the outlet pipe 4 through the horizontal hole 5, and flows out therefrom. .

In the present embodiment, all the components of the interface disk 2 are made of stainless steel. The center shaft 1 and the outlet pipe 4 have the same outer diameter, both of which are 20 mm; the interface plate 2 has a diameter of 145 mm. Of course, the size can be expanded or reduced as needed.

It should be noted that the number of the horizontal holes 5 in the water outlet pipe 4 is not limited to four as described in the embodiment, and may be more or four. As for the installation position of the water outlet pipe 4, it is not necessarily limited to the center disposed on both sides of the interface plate 2 as described in the embodiment, as long as the outlet pipe 4 can be received from the inner cavity of the interface disk 2, any such The location of the setting.

The reaction vessel used in the present invention will be described in detail below with reference to the accompanying drawings and taking a column can. Referring to Figure 2, the column canister used in the present invention includes a can body 6 and a can lid 7. The bottom of the tank cover 7 and the bottom surface of the tank body 6 (the bottom of the tank) have a water outlet pipe 4 for the solid phase catalyst reaction column or a hole 8 or a hole 9 extending out of the tank. The hole 8 or the hole 9 is provided with and A locking sealing screw that cooperates with the water pipe 4 or the center shaft 1 for locking the water outlet pipe 4 or the center shaft 1 and sealing the hole 8 or the hole 9. Both the can lid 7 and the bottom of the can have a liquid inlet 10 or 11 that communicates with the can cavity. The can lid 7 is also provided with a viewing hole 12 and a thermometer socket for inserting the thermometer 13. In this embodiment, the tank wall adopts a sandwich structure, and the interlayer can be filled with constant temperature circulating water for heat preservation. The inlet and outlet port 14 of the constant temperature circulating water is disposed on the tank wall. However, in practical applications, the method of tank insulation can also be carried out in such a manner that the insulation material such as insulation cotton or polyurethane foam is covered outside the tank wall.

In this embodiment, all the components of the column can are made of stainless steel, and the main dimensions are as follows: The inner height of the column can is 300 mm, and the inner diameter is 170 mm. Of course, the size can be expanded or reduced as needed.

The preparation of the solid phase catalyst reaction column and its column will be described below by way of specific examples.

First, the preparation of the column of the solid phase catalyst reaction column will be described. It can be understood that when the solid phase catalyst reaction column comprises an interface plate, the so-called column refers to a column formed by the columnar solid phase catalyst and the interface disk as a whole without a waterproof membrane; when the solid phase catalyst reaction column does not contain In the case of the interface disk, the so-called column is as described above, and is a column formed of a columnar solid phase catalyst not coated with a water repellent film.

Example 1. Preparation of immobilized glucose isomerase column

First, according to the method described in the above-mentioned publication No. CN1982445, entitled "Carbs for Preparation of Immobilized Enzymes or Immobilized Cells and Immobilization Methods Using the Carriers", a thickness of 5 mm is prepared. a strip-shaped immobilized glucose isomerase having a width of 50 mm; then, the above-mentioned strip-shaped immobilized glucose isomerase was wound into a thickness of 50 mm and a diameter of 150 mm with the center axis 1 shown in Fig. 1 as an axis. Disc-shaped immobilized glucose isomerase block; repeated winding operation to make four disc-shaped immobilized glucose After constructing the enzyme block; then, the four enzyme blocks are pressed against each other, stacked into a 200 mm high enzyme block cylinder, and attached to the mesh surface 3 of the interface plate 2 shown in Fig. 1 to be fixed. Glucose isomerase column.

Next, the preparation of a solid phase catalyst reaction column will be explained.

Example 2. Preparation method of immobilized glucose isomerase reaction column 1

First, a column of immobilized glucose isomerase is prepared according to the method described above (ie, a column of a solid phase catalyst reaction column); then, a hot melt pressure sensitive adhesive having a melting point of 90 ° C is sprayed on the cylinder surface of the column; The column is wrapped with a waterproof film such as a plastic film, and the plastic film wrapped on the interface plate 2 is fastened with a silicone tape.

Example 3. Preparation method of immobilized glucose isomerase reaction column 2

First, a column of immobilized glucose isomerase is prepared according to the method described above; then, the column of the column is wound and covered with a strip of carpet rubber (this is a gauze substrate double-sided tape); A waterproof film such as a plastic film is pasted and wrapped, and the plastic film wrapped around the cylindrical surface of the column is fixed by a silicone tape.

Example 4. Preparation method of immobilized glucose isomerase reaction column 3

First, the column of the immobilized glucose isomerase is prepared according to the method described above; then, the cylinder of the column is pasted with a plastic film coated with a hot melt pressure sensitive adhesive, and wrapped in the column of the column with a silica gel tape The plastic film on the interface plate 2 is fastened.

Example 5. Preparation method of immobilized glucose isomerase reaction column 4

First, a column of immobilized glucose isomerase is prepared according to the method described above; then, two layers are coated on the cylinder surface of the column with a plastic film, and the end of the surface plastic film is sealed with a hot melt pressure sensitive adhesive, and the silicone tape is used. The plastic film wrapped on the column surface of the column plate 2 is fastened and fixed.

Example 6. Preparation method of immobilized glucose isomerase reaction column 5

First, a column of immobilized glucose isomerase is prepared according to the method described above; then, a plastic film sleeve having a slightly larger diameter is sleeved on the column, and both ends of the plastic film sleeve are separated by a silica gel strip. Do not fix it on the interface plate 2 and the middle shaft 1 exposed on the open end face of the column, and then gently rotate the silicone belt on the middle shaft 1 and drive the end of the plastic film sleeve to twist direction, so that the plastic film sleeve is tightened plastic. The membrane and the cylinder of the column.

Example 7. Preparation method of immobilized glucose isomerase reaction column 6

First, according to the method disclosed in Chinese Patent Application Laid-Open No. "CN1982445", entitled "Essence for Preparation of Immobilized Enzyme or Immobilized Cell and Immobilization Method Using the Carrier", a thickness of 5 mm and a width are prepared. a 50 mm strip-shaped immobilized glucose isomerase; then, it was wound into a disk shape having a thickness of 50 mm and a diameter of 150 mm (ie, without a central axis and without leaving a void in the center); , a total of four disc-shaped immobilized glucose isomerase blocks of the same size were formed; after that, the four enzyme blocks were stacked close to each other to form a 200 mm high enzyme block cylinder and interface with no central axis. The inflow surface of the disc is pressed tightly to obtain an immobilized glucose isomerase reaction column; then, the column of the column is pasted and coated with a plastic film coated with a hot melt pressure sensitive adhesive, and The silicone tape is fastened to the plastic film wrapped on the interface plate of the column.

It is to be noted that the methods for preparing the solid phase catalyst reaction column described in the foregoing Embodiments 2 to 7 are to first prepare a column of the reaction column, and then wrap the column with a waterproof membrane to obtain a desired reaction column. However, in practical applications, it is also possible to preliminarily form a sleeve with a waterproof membrane, and then load a granular and/or block-shaped and/or strip-shaped solid phase catalyst or the like into the sleeve to obtain a desired reaction column. . This is because the waterproof film sleeve is soft and deformable and can be attached to the peripheral surface of the solid phase catalyst throughout the operation of the reaction apparatus, which can also avoid the defects in the prior art and achieve the object of the present invention.

It should be further noted that, in the foregoing embodiment, when preparing the reaction column with the interface plate, the solid phase catalyst and the interface plate are wrapped together with a waterproof membrane, and the silicone column is wrapped around the cylindrical column. The waterproof membrane on the interface plate is fastened. However, in practical applications, the solid phase catalyst and the interface plate may be separately wrapped with a waterproof membrane, or only the solid phase catalyst may be wrapped, and then the silica gel ribbon may be wound accordingly. Of course, in this way Preferably, the interface disk has such a structure that its third end face is recessed with respect to the circumferential surface thereof toward the interface disk cavity, and has good permeability to the reaction liquid. The area of the recessed portion may be the entire end surface, or may be between the area of the second end surface of the solid phase catalyst to which it is attached and the area of the entire end surface. Moreover, the shape of the recessed portion is preferably adapted to the shape of the second end face of the solid phase catalyst.

Next, the structure of the solid phase catalyst reaction apparatus and its operation will be described by way of specific examples.

Example 8 Preparation and Operation of Immobilized Glucose Isomerase Double Wall Reaction Device 1 Referring to Fig. 3, the structure of the column can used in this embodiment is the same as that shown in Fig. 2, and will not be described again. The preparation and operation of the solid phase catalyst reaction apparatus of this embodiment will be described in detail below with reference to Fig. 3.

First, an immobilized glucose isomerase reaction column was prepared in accordance with the method described in the above Examples 2-6.

Then, open the can lid 7 of the column can, loosen the can lid 7 and the central locking screws 15 and 16 at the bottom of the can, and install the reaction column in the column can in a cis mode so that the outlet pipe 4 of the reaction column is from the bottom of the can The central hole 9 is extended and the central locking screw 16 of the bottom of the can is locked to close the liquid inlet 10 of the bottom of the can.

Next, the substrate solution (50% (w/v) glucose, 1 mM magnesium sulphate, 0.04% sodium sulfite, pH 7.8) was poured into the tank and filled. Thereafter, the substrate solution is continuously replenished to maintain the full tank state, allowing the substrate solution to permeate into the reaction column and flow downward.

Then, when the outlet pipe 4 of the reaction column has liquid and no bubbles flow out, the water pipe 4 is closed; the can lid 7 is covered, and the central shaft 1 of the reaction column is extended from the central hole 8 of the can lid 7; the thermometer 13 is inserted The thermometer socket is locked and locked, and the tank cover 7 and the observation port 12 on the tank cover 7 and the central locking screw 15 are tightly sealed; the liquid inlet 11 on the tank cover 7 is closed, and the constant temperature cycle of opening at 75 ° C is opened. Water inlet and outlet interface 14. Open the water outlet 4 and the liquid inlet 10 of the bottom of the tank, and pump the substrate solution heated to 75 °C from the liquid inlet 10 of the tank bottom to the tank at a rate of 200 ml/min. Inside, keep running.

EXAMPLE 9 Preparation and Operation of Immobilized Glucose Isomerase Double Wall Reaction Apparatus 2 Referring to Figure 4, the structure of the column can used in this embodiment is the same as that shown in Figure 2, and will not be described again. The preparation and operation of the solid phase catalyst reaction apparatus in this embodiment will be described in detail below with reference to FIG.

Then, open the can lid 7 of the column can, loosen the can lid 7 and the central locking screws 15 and 16 at the bottom of the can, and install the reaction column in the column can in a reverse manner, so that the central axis 1 of the reaction column is from the bottom of the can The central hole 9 is extended, and the central locking screw 16 of the bottom of the can is locked; the can lid 7 is covered, and the outlet pipe 4 of the reaction column is extended from the central hole 8 of the can lid 7; the thermometer 13 is inserted into the thermometer socket And locking, the can lid 7 and the observation port 12 on the can lid 7 are tightly sealed; the liquid inlet 10 of the bottom of the can is closed, and the circulating water of 75 ° C is connected.

Next, a substrate solution of 75 ° C (the composition of which is the same as in Example 8) was pumped from the fixed inlet port 11 into the tank at a rate of 200 ml/min, and the outlet pipe 4 of the reaction column was discharged from the liquid. At this time, the observation port 12 is released. When the liquid in the observation port 12 flows out, the observation port 12 is locked. Continue to run in the above state.

Example 10, Preparation and Operation of Immobilized Glucose Isomerase Double Wall Reaction Apparatus 3 The structure of the column tank used in this embodiment is the same as that shown in Fig. 2, and the operation process is similar to that of the foregoing embodiment 9, No longer.

This embodiment has the following differences from the embodiment 9: First, the immobilized glucose isomerase reaction column used in the present embodiment is prepared according to the method described in the foregoing embodiment 7, in other words, the embodiment The immobilized glucose isomerase reaction column used in the column does not have a central axis; secondly, since the reaction column in this embodiment does not have a central axis, it is necessary to seal the central hole 9 of the bottom of the column can, for example, Solid short shaft sealing can be used.

Example 11, Preparation and operation of a conventional reaction device for immobilized glucose isomerase. The preparation and operation of the prior art device will be described by taking the conventional reaction device for immobilizing glucose isomerase as an example in conjunction with FIG. 5 to further illustrate the beneficial effects of the solid phase catalyst reaction device provided by the present invention.

The preparation process and structure of the solid phase catalyst reaction column used in the prior device are as follows:

First, a sheet having a thickness of 5 mm and a width of 50 Å is prepared in accordance with the Chinese Patent Application Laid-Open No. "CN1982445", entitled "A Carrier for Preparing Immobilized Enzyme or Immobilized Cells, and an Immobilization Method Using the Carrier". Band-shaped immobilized glucose isomerase.

Then, the strip-shaped immobilized glucose isomerase was wound into a disc having a thickness of 50 mm and a diameter of 170 mm, with a solid stainless steel shaft having a diameter of 20 awake as an axis. It is adhered and fixed with a small amount of hot melt adhesive at the winding end.

Thereafter, the winding operation was repeated to prepare four disc-shaped immobilized glucose isomerase blocks of the same size. The four enzyme blocks are stacked one upon another into a 200 mm high enzyme block cylinder 18, i.e., a solid phase catalyst reaction column 18.

The structure of the column can used in this embodiment is the same as that shown in FIG. 2, and details are not described herein again. Only the operation of the conventional reaction apparatus will be described below.

First, the prepared enzyme block cylinder 18 is inserted into the column canister so that it is located at the center of the can, and the central axis 17 of the enzyme block cylinder 18 is passed through the can lid 7 and the central holes 8 and 9 of the can bottom. , Lock the can lid 7 and the locking screws 15 and 16 of the central holes 8 and 9.

Then, the inlet and outlet port 14 of 75 ° C constant temperature circulating water is connected; and the substrate solution of 75 ° C is pumped from the liquid inlet 10 of the tank bottom into the tank at a rate of 200 ml/min until the tank lid 7 is filled. Port 11 flows out of the liquid. Continue to run in the above state.

Next, the test results of the respective examples described above were compared.

The test was carried out in accordance with the methods described in the above Examples 8 to 11, and the effluent of the reaction column was collected periodically every day. According to the publication No. "CN1982445", the name of the invention is "a carrier for preparing an immobilized enzyme or an immobilized cell, and an immobilization method using the same". The fructose conversion rate of the substrate solution was determined, and the half-life of the solid phase enzyme in each example was calculated from the degree of attenuation of the conversion rate with time. The results are as follows:

As can be seen from the above table, the half-life of the solid phase enzyme in the solid phase catalyst reaction apparatus provided by the present invention is 16 to 19 days; the half-life of the solid phase enzyme in the reaction apparatus is 4 days.

It should be noted that the shape of the solid phase catalyst reaction column used in the present invention may not be limited to the cylindrical shape described in the foregoing embodiment, and may be a column of other shapes such as a prism, or may be a non-column. Other shapes. Similarly, the central axis of the reaction column may also be a column of other shapes such as a prism. Further, the shape of the interface disk is not limited to the shape of the disk described in the foregoing embodiment, but a column having a polygonal end face or the like may be employed. Preferably, the shape and size of the end face of the interface plate match the end face of the columnar solid phase catalyst to which it is attached. As for the number of the reaction column outlet pipes used in the present invention, it may not be limited to one as described in the foregoing embodiment, or may be plural, so that the can lid of the column can or the water outlet provided on the bottom of the can is required. The quantity cannot be less than the number of outlet pipes

It is further noted that the reaction vessel used in the present invention may not be limited to the column can described in the foregoing embodiment, and may be any suitable container. Further, in the present invention The manner in which the column cans are placed may not be limited to the upright type described in the foregoing embodiments, but may take any form capable of achieving the object of the present invention.

It is to be understood that the above embodiments are merely exemplary embodiments for illustrating the principles of the invention, but the invention is not limited thereto. Various modifications and improvements can be made by those skilled in the art without departing from the spirit and scope of the invention. These modifications and improvements are also considered to be within the scope of the invention.

Claims

Claim

A solid phase catalyst reaction apparatus comprising a reaction vessel and a solid phase catalyst disposed in the reaction vessel, the solid phase catalyst having a first end surface into which the reaction liquid can flow, and a second end surface through which the product solution after the reaction can flow out And a circumferential surface extending between the first end surface and the second end surface, characterized in that a waterproof film is wrapped on a circumferential surface of the solid phase catalyst.

2. The solid phase catalyst reaction apparatus according to claim 1, further comprising an interface disk that is in close contact with the second end surface of the solid phase catalyst, the interface disk being a cavity structure having the following section:

a third end surface having a liquid inlet groove and a second end surface of the solid phase catalyst for supporting the solid phase catalyst and collecting liquid from the solid phase catalyst; a fourth end surface thereof a water outlet is arranged on the outlet for discharging the liquid in the interface plate outward;

A hermetic peripheral surface extending between the third end surface and the fourth end surface, together with the fourth end surface, constitutes a chamber for containing a liquid.

The solid phase catalyst reaction apparatus according to claim 2, wherein the water outlet is an outlet pipe.

The solid phase catalyst reaction device according to claim 3, wherein a wall of the outlet pipe section located in the inner cavity of the interface plate is provided with a hole through which liquid in the interface disk can flow The outlet pipe.

The solid phase catalyst reaction apparatus according to claim 2, wherein the water repellent film extends to the interface disk, and the solid phase catalyst peripheral surface and the interface disk circumferential surface are wrapped together.

The solid phase catalyst reaction apparatus according to claim 1 or 5, wherein the waterproof film encloses the circumferential surface by means of an adhesive.

The solid phase catalyst reaction apparatus according to claim 6, wherein the binder comprises a hot melt adhesive, an adhesive plaster, and a carpet rubber.

The solid phase catalyst reaction device according to claim 6, wherein the outer surface of the waterproof film is wound with a fastening tape for fastening the waterproof film, so that the waterproof film is more firmly Wrapped on the circumference.

The solid phase catalyst reaction apparatus according to claim 1, wherein the water repellent film is a plastic film.

The solid phase catalyst reaction apparatus according to claim 1, wherein the solid phase catalyst has a columnar shape.

The solid phase catalyst reaction apparatus according to claim 10, wherein the columnar solid phase catalyst is wound from a sheet.

The solid phase catalyst reaction apparatus according to claim 10, wherein the columnar solid phase catalyst is made of a particulate solid phase catalyst.

The solid phase catalyst reaction apparatus according to claim 1 or 2, wherein the solid phase catalyst has a central axis.

The solid phase catalyst reaction apparatus according to claim 13, wherein the solid phase catalyst is wound from a sheet around the central axis.

The solid phase catalyst reaction apparatus according to claim 13, wherein the center shaft is fixed to a central portion of the interface disk.

The solid phase catalyst reaction device according to claim 2, wherein the reaction device is in a cis-mounting manner, that is, the solid phase catalyst is on, the interface plate is under, and the reaction liquid is located above. The first end surface of the solid phase catalyst enters the solid phase catalyst, and is infiltrated from top to bottom to react with the solid phase catalyst, and the reacted product solution is collected and discharged by the interface tray located below.

.

The solid phase catalyst reaction device according to claim 2, wherein the reaction device is in a reverse mounting manner, that is, the solid phase catalyst is on the bottom, the interface plate is on, and the reaction liquid is located below. The first end surface of the solid phase catalyst enters the solid phase catalyst, and flows from the bottom to the top to react with the solid phase catalyst, and the reacted product solution is collected and discharged by the interface plate located above.

The solid phase catalyst reaction apparatus according to claim 1, wherein the reaction vessel is a column tank.

The solid phase catalyst reaction device according to claim 18, wherein the column can includes a can lid, and the can lid and/or the bottom of the can is provided with a liquid inlet, and the reaction solution is passed through The inlet port enters the column tank.

20. The solid phase catalyst reaction apparatus according to claim 19, wherein the can lid and/or the bottom of the can is provided with a central hole for the center axis of the solid phase catalyst and/or the interface plate The water pipe extends.

The solid phase catalyst reaction apparatus according to any one of claims 18 to 20, wherein the tank wall of the column tank is an interlayer, and the outer wall of the interlayer is provided with a constant temperature water inlet and outlet for introducing into the interlayer. Constant temperature water for heat preservation.

The solid phase catalyst reaction apparatus according to any one of claims 18 to 20, wherein the can wall of the column can is a single layer, and the outer wall is covered with a heat insulating cotton and/or polyurethane foam.

The method of operating a solid phase catalyst reaction apparatus according to claim 1, wherein a reaction liquid is injected into the reaction vessel, and the reaction liquid is introduced into the reaction vessel through the first end surface of the solid phase catalyst, and Flowing toward the second end surface of the solid phase catalyst under the restriction of the waterproof membrane, and simultaneously reacting with the solid phase catalyst, the product solution after the reaction flows out from the second end surface of the solid phase catalyst.

24. The method of operating a solid phase catalyst reaction apparatus according to claim 23, wherein a gap between an inner wall of the reaction vessel and the waterproof membrane rises to a top of the solid phase catalyst, and is accessed by a first end surface located at the top a solid phase catalyst, and a downward wetting flow in the solid phase catalyst under the constraint of the waterproof membrane, while reacting with the solid phase catalyst, the product solution after the reaction is from the bottom of the solid phase catalyst Two-face flow

25. The method of operating a solid phase catalyst reaction apparatus according to claim 23, wherein a gap between the inner wall of the reaction vessel and the waterproof membrane flows downward to the bottom of the solid phase catalyst, and enters from the first end surface at the bottom The solid phase catalyst, and infiltrating upward in the solid phase catalyst under the constraint of the waterproof membrane, while reacting with the solid phase catalyst, the product solution after the reaction is from the top of the solid phase catalyst The second end faces out.

The operating method of a solid phase catalyst reaction apparatus according to any one of claims 23 to 25, wherein the reaction apparatus further comprises an interface disk that is in close contact with the second end surface of the solid phase catalyst, The interface disk is a cavity structure having the following parts: that is, a third end surface having a liquid inlet groove and a second end surface of the solid phase catalyst, and a water outlet is disposed thereon a fourth end surface, a closed circumferential surface extending between the third end surface and the fourth end surface, wherein

The reaction solution entering the solid phase catalyst reacts with the solid phase catalyst, and the product solution flows out from the second end surface of the solid phase catalyst, and is collected to the interface via the third end surface of the interface disk. The disk is then discharged through the water outlet of the interface disk.

The operation method of the solid phase catalyst reaction device according to claim 23, wherein the container wall of the reaction container is an interlayer, and the operation method further comprises introducing constant temperature water into the interlayer for heat preservation. A step of.