WO2015027554A1 - Industrial dissolution apparatus for pure chitosan spinning solution - Google Patents

Abstract

An industrial dissolution apparatus for a pure chitosan spinning solution comprises a dissolution vessel (1) and a stirring apparatus. A feed inlet (5), a solvent inlet (6), a vacuum suction port (7) and a water inlet (9) are arranged on an upper head (3) of the dissolution vessel (1). A liquid outlet (11) is arranged on a lower head (4). The stirring apparatus comprises a stirring shaft and a stirring power apparatus. An upper stirring shaft (2) and a lower stirring shaft (21) with stirring paddles are fixedly connected to form the stirring shaft. The lower stirring shaft (21) with stirring paddles is fixedly provided with a first stirring paddle (23) and second stirring paddles (24). The first stirring paddle (23) is arranged on a lower part of the lower stirring shaft (21). The second stirring paddles (24) comprise at least two groups that are above the first stirring paddle (23) and arranged on the lower stirring shaft (21) upward in sequence. Blades (29) of a group of the second stirring paddles in a top layer are provided with vertical striker plates (30). Blades (28) of the first stirring paddle and the blades (29) of the second stirring paddles have an inclination angle α against an axis of the stirring shaft respectively. A range of the α is 30°-60°. Inclination directions of the inclination angles are opposite.

Description

 Industrialized dissolution device for pure chitosan spinning solution Technical field

The present invention relates to a dissolution device for a fiber raw material, and more particularly to an industrial dissolution device for a pure chitosan spinning solution.

Background technique

Pure chitosan fiber is a fiber made from the extract of shrimp and crab shell. It is extracted from discarded shrimp and crab shells and is not a petroleum resource. It is a green product. Pure chitosan fiber has broad-spectrum antibacterial activity, anti-fungal property, excellent biocompatibility and non-immunogenicity, and also has the functions of adsorption chelation, hemostasis, and scar reduction. The textiles made therefrom have Very good health care function. Based on these special properties, pure chitosan fiber can be widely used in aerospace, medical and health, military civil textiles, filtration protection and other fields, and has a huge market prospect.

An important industrial link in the preparation of pure chitosan fibers is the dissolution of pure chitosan raw materials. To achieve rapid preparation of large-volume pure chitosan spinning solution, it is necessary to adjust the contact area and dissolution temperature of pure chitosan raw material and solvent during the dissolution process. However, too high a dissolution temperature will degrade the pure chitosan molecular chain and affect the fiber quality. Therefore, it is necessary to increase the contact area between pure chitosan and solution. The larger the contact area, the more the amount of dissolution per unit time. . The conventional method of increasing the contact area between pure chitosan and solution is to dissolve the pure chitosan raw material, but the pure chitosan microstructure is affected by the strong shearing action during the grinding process and the local temperature is too high. Destruction, molecular chain breakage, affecting the mechanical properties of the final fiber. A new method is to directly dissolve the flake-form pure chitosan raw material, and the obtained chitosan solution has a complete microstructure and can exhibit excellent performance in the subsequent spinning process. However, after decalcification and deproteinization, the pure chitosan raw material will produce a large number of gaps in the structure. The filling gas in these gaps will prevent the effective contact between the pure chitosan raw material and the solvent; in addition, the chitosan filled with gas The material floats on the solvent surface and also reduces the contact of the pure chitosan material with the solvent. Therefore, how to rapidly dissolve the flaky chitosan raw materials in industrial production to prepare high-quality pure chitosan spinning solution is a huge problem.

technical problem

The invention aims at the above-mentioned difficulties existing in the prior art, and provides an industrialized dissolution device for a pure chitosan spinning solution, which can quickly and efficiently dissolve the flake-form pure chitosan raw material and realize large-scale industrial production.

Technical solution

The technical solution adopted by the invention is:

An industrialized dissolution device for a pure chitosan spinning solution, comprising a dissolution kettle and a stirring device; the upper head of the dissolution kettle is provided with a feed port, a solvent inlet, a vacuum suction port, a water inlet, and a lower seal head a stirring port is provided; the stirring device comprises a stirring shaft and a stirring power device; the stirring shaft is composed of an upper agitating shaft and a lower agitating shaft with a stirring slurry; the upper end of the upper agitating shaft and the stirring power device The output shaft of the reducer is fixedly connected, passes through the mechanical sealing device and extends into the dissolving kettle, and the lower end of the lower agitating shaft is mounted on the bottom bracket, and the bottom bracket is fixedly installed at the bottom center position of the dissolving kettle; The lower agitating shaft is fixedly provided with a first agitating paddle and a second agitating paddle; the first agitating paddle is disposed at a lower portion of the lower agitating shaft; the second agitating paddle is composed of at least two groups, located above the first agitating paddle, Provided on the lower agitating shaft in turn, the uppermost set of the second agitating paddles is further provided with a vertical baffle plate; the blades of the first agitating paddle and the blades of the second agitating paddle are respectively agitated Axis of the shaft has an inclination angle α, [alpha] range is 30 ° -60 °, a direction opposite to the inclination of the inclination angle.

Preferably, an annular solvent spray pipe is disposed in an upper portion of the kettle body of the dissolution vessel, and the annular solvent spray pipe is in communication with the solvent inlet, and is evenly distributed on the pipe wall in a 90° sector below the horizontal center plane. Filled with small holes. The annular solvent spray pipe can evenly spray the injected solvent on the pure chitosan raw material, which is beneficial to the uniform mixing contact between the pure chitosan raw material and the solvent.

Preferably, the mounting angles of the first agitating paddle and the second agitating paddle on a horizontal plane are evenly distributed. Agitating paddles evenly distributed along the circumference allows the device to have good dynamic balance performance during operation.

Preferably, the second agitating paddles are three groups.

Preferably, the blades of the first agitating paddle and the second agitating paddle are provided with a reinforcing plate having a triangular cross section. Due to the high viscosity of the pure chitosan spinning solution, the blade will bear a large resistance during the working process, and it is easy to bend and deform. This preferred embodiment adds a reinforcing plate, a reinforcing plate and a blade circumference to the stirring blade. a triangular cross section, which on the one hand increases the strength of the stirring paddle, on the other hand, the triangular cross section does not form a concave angle on the stirring paddle, thereby avoiding the accumulation of the sheet-like pure chitosan raw material at the angle of the stirring process. It affects its dissolution.

Preferably, the shaft center line of the output shaft of the reducer, the axis line of the stirring shaft, the center line of the mechanical seal device, and the center line of the bottom bracket are in a straight line.

Preferably, the upper head of the dissolving kettle is provided with a vacuum inlet, a compressed air inlet, a vacuum gauge, an electric contact pressure gauge, a compressed air venting port and a safety valve, a viewing port and a sight glass lamp.

Preferably, the bottom of the dissolving kettle is provided with a sampling port, the liquid outlet is arranged at the bottom of the dissolving kettle, the liquid outlet is connected with the spinning liquid outlet and the waste water outlet through a tee, and the spinning liquid outlet is connected to the tee At the horizontal end, the waste water outlet is connected at the vertical downward end of the tee.

Preferably, the dissolution vessel is composed of an upper head, a cylinder and a lower head, and the upper head and the lower head are all elliptical heads.

Beneficial effect

The invention has the following beneficial effects:

1. The vacuum suction port is arranged on the upper head of the dissolution kettle of the invention, and a mechanical sealing device is also provided, so that the predetermined degree of vacuum can be continuously maintained in the dissolution tank. Under these conditions, the residual gas in the flake-form pure chitosan is continuously removed, and the solvent rapidly penetrates into the gap of the gas to escape, and fully contacts the inside of the sheet-like chitosan, thereby accelerating the dissolution of the flake-form pure chitosan. Speed, improve the preparation efficiency of pure chitosan spinning solution.

2. The uppermost second agitating paddle of the device of the invention is provided with a vertical baffle plate, the upper edge of which is higher than the liquid surface, and can agitate and disperse the flake-shaped pure chitosan floating on the liquid surface, which is beneficial to The flake-form pure chitosan is stirred into the liquid surface; at the same time, the flake-form pure chitosan of the spray solvent is stirred into the solution, so that the solvent is fully diffused in the solution, so that the concentration of the solution is uniform, and the flake-form pure chitosan is avoided. The dissolution rate is not uniform, thereby shortening the dissolution time of the flake-form pure chitosan, and preparing a high-quality pure chitosan spinning solution.

3. The invention provides a first agitating paddle and a second agitating paddle, wherein the blade of the first agitating paddle and the blade of the second agitating paddle respectively have an inclination angle α with respect to the axis of the agitating shaft, and the range of α is 30°-60 °, the tilt direction remains the opposite. The design of the inclined angle increases the shearing area of the stirring paddle during operation and the solution, and accelerates the dissolution of the flake-form pure chitosan. In addition, due to the special structure of the blade of the first agitating paddle on the lower agitating shaft and the blade of the second agitating paddle opposite to the axis of the shaft, the solution in the dissolving kettle is turned up and down to promote mutual diffusion and accelerate the pure shell of the sheet. The dissolution of the glycan.

Therefore, under the combined action of the stirring device and the vacuuming of the present invention, the flake-form pure chitosan can be quickly and efficiently dissolved to prepare a high-quality pure chitosan spinning solution.

From the actual effect of dissolution, the viscosity after decontamination is 1500mpa · s A pure chitosan spinning solution prepared by dissolving 93% of 500Kg of flake-form pure chitosan as an example, using existing dissolution technology, it takes 48-60 hours to complete, and using the dissolution apparatus of the present invention for 10-12 hours It can be done. It can be seen that the invention greatly improves the dissolution efficiency of the flaky chitosan and can be applied to large-scale industrial production.

DRAWINGS

Figure 1 is a schematic view showing the structure of a dissolution apparatus of the present invention;

Figure 2 is a schematic plan view of the dissolution vessel;

Figure 3 is a plan view of the plane of the stirring paddle of the dissolving device;

Figure 4 is a schematic view showing the inclination angle of the blade on the stirring paddle;

Figure 5 is a cross-sectional view of the reinforcing plate on the first stirring paddle;

Figure 6 is a cross-sectional view of the reinforcing plate on the second stirring paddle;

The markings in the figure indicate: 1---dissolving kettle, 2---upper shaft, 3---upper head, 4---lower head, 5--feeding port, 6 --- Solvent inlet, 7 --- vacuum pumping port, 8 --- breaking vacuum air inlet, 9 --- water inlet, 10 --- compressed air inlet, 11 --- liquid outlet, 12 --- Annular solvent spray pipe, 13 --- discharge orifice, 14 --- sampling port, 15 --- waste water outlet, 16 --- vacuum gauge, 17 --- electric contact pressure gauge, 18 - --Safety valve, 19 --- Observing port, 20 --- mirror light, 21 --- lower mixing shaft, 22 --- compressed air venting port, 23 --- first mixing paddle, 24 --- second mixing paddle, 25 ---Power bearing, 26---mechanical seal, 27 --- bottom bracket, 28 --- blade of the first paddle, 29 --- blade of the second paddle, 30 --- baffle plate, 31 --- Strengthening plate, 32---spinning liquid outlet, 33--- bracket.

Embodiments of the invention

The invention will be described in detail below with reference to the accompanying drawings and embodiments.

As shown in Figure 1, the dissolution device of the pure chitosan spinning solution provided by the present invention comprises a dissolving kettle 1, a stirring device, and the dissolving kettle 1 is composed of an upper head 3, a cylinder and a lower head 4 welded. The upper head 3 and the lower head 4 are oval heads.

As shown in FIG. 1 and FIG. 2, the upper head 3 of the dissolution vessel 1 is provided with a feed port 5 for discharging pure chitosan raw materials and personnel entering the dissolution tank 1 for maintenance work, and the feed port 5 Correspondingly, a closure is provided, and the dissolution vessel 1 is sealed during operation to seal.

As shown in FIG. 1, the upper head 3 of the dissolution tank 1 is provided with a solvent inlet 6 for inputting a solvent, and an automatic valve and a flow meter are disposed at the solvent inlet 6; as shown in FIG. 3 and FIG. The upper part of the kettle 1 is provided with an annular solvent spray pipe 12, which communicates with the solvent inlet 6, and uniformly distributes the liquid outlet hole 13 in the pipe wall in the 90° fan-shaped surface below the horizontal center surface; the annular solvent spray pipe 12 The mounting position is fixed on the baffle plate 30 on the vane 29 of the second agitating paddle by welding to the bracket 33 on the inner wall of the dissolving tank 1.

As shown in FIG. 1 and FIG. 2, the upper header 3 of the dissolution vessel 1 is provided with a vacuum suction port 7 and a vacuum evacuation port 8; the vacuum suction port 7 and the destruction vacuum inlet port 8 may be independently provided ports. However, it can also be placed on one port by the control of the tee and the valve. The vacuum suction port 7 is for evacuating the dissolution tank 1, and the vacuum inlet port 8 is broken for releasing air into the dissolution tank 1.

The upper head 3 of the dissolution tank 1 is provided with a water inlet 9 for injecting water into the dissolution tank 1, and an automatic valve and a flow meter are disposed at the water inlet 9.

The upper head 3 of the dissolution tank 1 is also provided with a compressed air inlet port 10. After the dissolution is completed, the compressed air is filled into the dissolution vessel 1 to effect the extrusion of the high-viscosity chitosan spinning solution from the liquid outlet 11, and input it to a subsequent process apparatus.

The liquid outlet 11 is disposed at a central position of the lower header 4 of the dissolution vessel 1, and is connected with a tee. In one embodiment, the other two interfaces of the tee are respectively connected to the spinning solution outlet 32 and the waste water outlet 15, the spinning solution. The outlet 32 is connected to the horizontal end of the tee, and the waste water outlet 15 is connected to the vertically downward end of the tee.

The dissolution kettle 1 is further provided with a sampling port 14, a vacuum gauge 16, an electric contact pressure gauge 17, a safety valve 18, a viewing port 19, a mirror lamp 20, and a compressed air venting port 22, wherein the compressed air venting port 22 can be separately set A port can also be placed in one port by a tee and a safety valve 18.

As shown in Fig. 1, the agitating shaft of the present invention is composed of an upper agitating shaft 2 and a lower agitating shaft 21 with agitating slurry, and the lower end of the upper agitating shaft 2 and the upper end of the lower agitating shaft 21 with agitating slurry. The flange with the ribs is welded, and the two are fixedly connected by bolts. This is not only the need to assemble the dissolving kettle, but also the need to repair the device; the bottom bracket 27 is fixed with a wear-resistant bushing of Teflon material. The lower end of the lower agitating shaft 21 is directly fit in the sleeve of the bottom bracket 27, and the bottom bracket 27 functions to support the fixed agitating shaft; the agitating power device includes a power bearing 25, a motor table, a motor and a matching reducer The lower end of the power bearing 25 is fixedly installed at the center of the outer wall of the upper head of the dissolution tank 1, and the seat bearing is fixedly mounted therein, and the function is to stabilize the stirring shaft; the motor table is fixedly mounted on the power branch by bolts. The upper end of the seat 25 functions as a platform for fixing the motor and the associated reducer; the output shaft of the reducer and the upper end of the upper agitator shaft 2 are fixedly connected by a coupling.

The axis line of the output shaft of the reducer, the axis line of the stirring shaft, the center line of the mechanical seal 26, and the center line of the bottom bracket 27 are in a straight line.

The mechanical seal device 26 is fixedly mounted at the center of the upper head of the dissolution vessel 1 for sealing the gap between the dissolution tank 1 and the upper agitator shaft 2.

As shown in FIG. 1, the first agitating paddle 23 is attached to the bottom of the agitating shaft, and the second agitating paddle 24 is attached above the first agitating paddle 23. The stirring paddle is composed of a blade and a sleeve. The blade is fixed on the sleeve, and the sleeve is mounted on the stirring shaft. When the stirring shaft rotates, the sleeve and the blade are rotated to realize the stirring and shearing of the pure chitosan spinning solution. The second agitating paddles 24 have at least two groups, wherein the upper edge position of the blades 29 of the uppermost second agitating paddle is flush with the liquid level of the effective volume line of the dissolution vessel 1.

As shown in FIG. 3, the mounting angles of the first agitating paddle 23 and the second agitating paddle 24 on the horizontal plane are evenly distributed. Agitating paddles evenly distributed along the circumference allows the device of the present invention to have good dynamic balance properties during operation.

As shown in Fig. 4, the blades 28 of the first agitating paddle and the blades 29 of the second agitating paddle respectively have an inclination angle α with respect to the axis of the agitating shaft, and α ranges from 30° to 60°, and the inclination direction remains opposite. When the agitating shaft rotates clockwise or counterclockwise, the blades 28 of the first agitating paddle exert an upward or downward force on the spinning solution, and the blades 29 of the second agitating paddle exert a downward or upward force on the spinning solution. . That is, by adjusting the direction of rotation of the agitating shaft, it is possible to achieve the effect of the blade of the first agitating paddle and the blade of the second agitating paddle exerting an upward or downward force on the spinning solution.

As shown in FIG. 1, a plurality of vertical baffle plates 30 are welded to the blades 29 of the uppermost second agitating paddles, and the welding method is such that the baffle plates 30 are substantially in the vertical direction during operation, and the baffle plates 30 are provided. The height is between 250mm and 350mm. Of course, it is also possible to fix the baffle 30 by means other than welding.

As shown in FIGS. 5 and 6, the reinforcing blade 31 is welded to the blade 28 of the first agitating paddle and the blade 29 of the second agitating paddle, and the reinforcing plate 31 and the blade are formed in a triangular cross section.

The above-described embodiments and the accompanying drawings are intended to be illustrative of the principles of the invention, and are intended to be It is intended to be included within the scope of the appended claims.

Claims (1)

An industrial dissolution apparatus for a pure chitosan spinning solution, comprising a dissolution vessel (1) and a stirring device; a feed port (5) is provided on an upper head (3) of the dissolution kettle (1), a solvent inlet (6), a vacuum suction port (7), a water inlet (9), and a lower outlet head (4) having a liquid outlet (11); the stirring device includes a stirring shaft and a stirring power device; the stirring The shaft is composed of an upper agitating shaft (2) and a lower agitating shaft (21) with agitating slurry; the upper end of the upper agitating shaft (2) is fixedly connected with the output shaft of the agitating power unit through the mechanical seal The device (26) extends into the dissolution kettle (1), and the lower end of the lower agitating shaft (21) is mounted on the bottom bracket (27), and the bottom bracket (27) is fixedly installed at the bottom center position of the dissolution kettle (1); The lower agitating shaft (21) with a stirring slurry is fixedly provided with a first stirring paddle (23) and a second agitating paddle (24); the first agitating paddle (23) is disposed at a lower portion of the lower agitating shaft (21); the second agitating paddle (24) is composed of at least two groups, located at the first agitating Above the paddle (23), arranged upwardly on the lower agitating shaft (21), the uppermost set of second agitating paddle blades (29) is further provided with a vertical baffle plate (30); the first agitating The blades (28) of the paddle and the blades (29) of the second agitating paddle respectively have an inclination angle α with respect to the axis of the agitating shaft, and α ranges from 30° to 60°, and the inclination angles of the inclination angles are opposite. 2. The industrialized dissolving device for a pure chitosan spinning solution according to claim 1, characterized in that the upper part of the autoclave of the dissolving kettle (1) is provided with an annular solvent spraying pipe (12), and the annular solvent spraying The shower pipe (12) is in communication with the solvent inlet (6), and a plurality of liquid outlet holes (13) are arranged in the lower portion of the annular solvent spray pipe (12). 3. The industrialized dissolution apparatus for a pure chitosan spinning solution according to claim 2, characterized in that the first agitating paddle (23) and the second agitating paddle (24) are evenly distributed at a horizontal plane circumference. 4. An industrial dissolution apparatus for a pure chitosan spinning solution according to claim 1 or 2 or 3, wherein the first agitating paddle (23) and the second agitating paddle (24) are provided on the blade A stiffener (31) with a triangular cross section. 5. The industrialized dissolving device for a pure chitosan spinning solution according to claim 4, characterized in that: the shaft center line of the output shaft of the reducer, the shaft center line of the stirring shaft, and the mechanical sealing device (26) The center line and the center line of the bottom bracket (27) are in a straight line. The industrialized dissolving device for a pure chitosan spinning solution according to claim 4, characterized in that the upper head (3) of the dissolving kettle (1) is provided with a broken vacuum inlet ( 8), compressed air inlet (10), vacuum gauge (16), electrical contact pressure gauge (17), compressed air vent (22) and safety valve (18), observation port (19) and mirror light ( 20). 7. The industrialized dissolution apparatus for a pure chitosan spinning solution according to claim 5, characterized in that the lower head (4) of the dissolution kettle (1) is provided with a sampling port (14), The liquid outlet (11) is disposed at the bottom of the dissolution vessel (1), and the liquid outlet (11) is connected to the spinning solution outlet (32) and the waste water outlet (15) through a tee, and the spinning solution outlet (32) is connected At the horizontal end of the tee, the waste water outlet (15) is connected to the vertically downward end of the tee. 8. The industrialized dissolution apparatus for a pure chitosan spinning solution according to claim 6, characterized in that the dissolution vessel (1) is composed of an upper head (3), a cylinder body and a lower head (4) The welding composition, the upper head (3) and the lower head (4) are all elliptical heads.

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