CN114775069B - Spinning solution defoaming method for industrially producing pure chitosan fibers - Google Patents
Spinning solution defoaming method for industrially producing pure chitosan fibers Download PDFInfo
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- CN114775069B CN114775069B CN202210462468.7A CN202210462468A CN114775069B CN 114775069 B CN114775069 B CN 114775069B CN 202210462468 A CN202210462468 A CN 202210462468A CN 114775069 B CN114775069 B CN 114775069B
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- 238000009987 spinning Methods 0.000 title claims abstract description 118
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000835 fiber Substances 0.000 title claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 230000008859 change Effects 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims description 12
- 230000007480 spreading Effects 0.000 claims description 10
- 238000003892 spreading Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 230000007246 mechanism Effects 0.000 claims description 7
- 230000003068 static effect Effects 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 5
- 241000276425 Xiphophorus maculatus Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 208000032544 Cicatrix Diseases 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000003544 deproteinization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 230000005847 immunogenicity Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- 230000037387 scars Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention relates to a spinning solution defoaming method for industrially producing pure chitosan fibers, which comprises the following steps: step one, sealing the reaction kettle and vacuumizing; step two, a feed inlet of the reaction kettle is opened, spinning solution flows into an annular feed pipe through the feed inlet, and then falls to an umbrella-shaped guide plate at the upper layer through a liquid outlet of the annular feed pipe; step three, the first defoamed spinning solution flows onto an upper umbrella-shaped guide plate to automatically flow and spread a film to form a liquid film; fourthly, the second defoamed spinning solution flows onto an umbrella-shaped deflector at the lower layer to automatically flow and spread the film to form a liquid film; fifthly, flowing the defoamed spinning solution into the bottom of the reaction kettle for the third time, wherein a defoamed device of the reaction kettle moves along with the change of the liquid level of the spinning solution, and the defoamed device rotates; and step six, standing the spinning solution in a reaction kettle. By adopting the scheme, the original state structure of the molecular chain of the chitosan is ensured, and the spinning solution bubbles can be rapidly and uniformly removed in unit time, so that the method is suitable for industrial continuous production.
Description
Technical Field
The invention relates to the technical field of chitosan fiber preparation, in particular to a spinning solution defoaming method for industrially producing pure chitosan fibers.
Background
Chitosan fibers refer to fibers made from extracts from shrimp and crab shells, which have a number of particular advantages over traditional land natural fibers and synthetic fibers. Firstly, the method does not depend on petroleum and contend with grains for land, and opens up a third raw material source of chemical fibers; and secondly, the waste is utilized, and the sustainable development trend of green and environmental protection is met. Furthermore, the pure chitosan fiber has broad-spectrum antibacterial property, mildew resistance, excellent biocompatibility and no immunogenicity, and also has the effects of adsorbing chelation, stopping bleeding, promoting healing and reducing scars. Based on the function, the fiber composite material can be widely applied to the fields of aerospace, medical treatment and health, military and civil textiles, filtration protection and the like, has huge market potential, and plays a positive role in promoting the health of human beings.
The degree of deacetylation and viscosity are two important quality indicators of chitosan. It is known that the larger the molecular weight of chitosan, the larger the viscosity, and the relationship between the viscosity and the molecular weight shows that, namely: [ eta ] = K M alpha, (eta: viscosity, mpa.s, K: constant, M: relative molecular mass, alpha: a value related to molecular weight) thus, the higher the viscosity of the pure chitosan spinning solution, the higher the molecular weight, the higher the dry breaking strength of the spun pure chitosan fiber, and the higher the breaking elongation, and the better the spinnability. Therefore, only the high-viscosity chitosan solution meets the spinning requirement of the high-performance chitosan fiber.
One key link in the preparation of chitosan fibers is to dissolve chitosan raw materials, wherein the chitosan raw materials are generally platy chitosan, and the platy chitosan can generate a large amount of gaps in tissues after decalcification and deproteinization, and the gaps are filled with air; in addition, the flaky chitosan raw material is formed by superposing 2 or more sheets, and a large amount of gas is also stored in gaps among the flaky chitosan raw material, and the gas is adhered in the chitosan solution in the chitosan dissolving process and cannot escape; meanwhile, a large amount of bubbles can be generated in the processes of stirring, dissolving, filtering and conveying the chitosan solution.
In wet spinning, the chitosan solution must be sprayed from a spinneret plate into a coagulation bath without bubbles, and if the chitosan solution is sprayed from the spinneret plate into the coagulation bath with bubbles, the bubbles escape to cause yarn breakage, so that a defoaming treatment must be performed before spinning.
Disclosure of Invention
The invention overcomes the defects of the prior art, and provides a spinning solution defoaming method for industrially producing pure chitosan fibers, which ensures the original state structure of molecular chains of chitosan, and can rapidly and uniformly remove spinning solution bubbles in unit time so as to meet the requirements of industrial continuous production.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a spinning solution defoaming method for industrially producing pure chitosan fibers comprises the following steps:
step one, sealing the reaction kettle, and vacuumizing, wherein the vacuum degree is-75 to-85 kPa, the constant temperature in the reaction kettle is kept at 25-30 ℃, and the pressure in the reaction kettle is less than or equal to 5000pa;
step two, a feed inlet of the reaction kettle is opened, spinning solution flows into an annular feed pipe through the feed inlet, then falls to an umbrella-shaped guide plate at the upper layer through a liquid outlet hole of the annular feed pipe, extrusion shearing operation is carried out on the spinning solution through the liquid outlet hole, and bubbles larger than the diameter of the liquid outlet hole are removed to form spinning solution for primary defoaming;
thirdly, automatically flowing the first defoamed spinning solution onto an upper umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the upper umbrella-shaped guide plate is 1.8-2.4t/h, the thickness of the liquid film is 6-20mm, and the second defoamed spinning solution is formed by removing bubbles in the process of spreading the film;
fourthly, automatically flowing the spinning solution subjected to the second deaeration onto the lower umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the lower umbrella-shaped guide plate is 1.8-2.4t/h, the thickness of the liquid film is 5-18mm, and removing bubbles in the process of spreading the film to form a spinning solution subjected to the third deaeration;
fifthly, the defoamed spinning solution flows into the bottom of the reaction kettle for the third time, the defoamed device of the reaction kettle moves along with the change of the liquid level of the spinning solution, the defoamed device rotates at the rotation speed of 26-60 revolutions per minute, and the defoamed device cuts off bubbles on the liquid level of the spinning solution, so that the dynamic rotation defoamed operation of the spinning solution is realized;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and performing tertiary circulation to realize static defoaming operation of the spinning solution.
By adopting the scheme, the high-viscosity chitosan spinning solution with pressure enters the annular feeding pipe through the feeding port, and is extruded out of the liquid outlet hole, and the bubbles with the diameter larger than that of the liquid outlet hole can be removed completely due to the small diameter of the liquid outlet hole and the pressure in the tank body smaller than 5000pa; when the spinning solution flows onto the upper umbrella-shaped guide plate, a liquid film is formed due to the action of gravity and the inclination angle of the guide plate, the defoaming area is increased, and under the condition that the pressure in the tank body is less than 5000pa, partial bubbles are freely separated by controlling the flow speed and the thickness of the spinning solution, and the defoaming rate can reach 20-30% after passing through the upper umbrella-shaped guide plate; when the spinning solution flows onto the lower umbrella-shaped guide plate, a liquid film is formed due to the action of gravity and the inclination angle of the guide plate, the defoaming area is increased, and under the condition that the pressure in the tank body is less than 5000pa, partial bubbles are freely separated by controlling the flow speed and the thickness of the spinning solution, and the defoaming rate can reach 30-40% after passing through the lower umbrella-shaped guide plate; the number of umbrella-shaped guide plates can be increased, the number of defoaming times can be increased, the lower umbrella-shaped guide plates can guide the shell spinning solution to the bottom of the tank body, the defoaming device can adjust the position up and down along with the liquid level of the spinning solution, and can cut off bubbles on the liquid level of the spinning solution in a rotating mode, so that dynamic rotating defoaming operation of the spinning solution is realized, the defoaming rate can reach 30-50%, when the spinning solution stands still in the reaction kettle, the bubbles in the spinning solution are released, the air is exhausted and pumped out once every two hours, three times of circulation are generally carried out, the defoaming rate can reach 10-20%, and the static defoaming of the spinning solution is matched with the dynamic defoaming device, so that the defect that the spinning solution at the bottom of the tank body is difficult to defoam can be solved, the molecular chain original state structure of chitosan can be ensured, and the bubbles of the spinning solution can be quickly and uniformly released in unit time, so that the method is suitable for industrial continuous production.
The invention is further provided with the following steps: the liquid outlet hole is a round hole with the diameter smaller than 3 mm.
By adopting the scheme, bubbles with diameters larger than 3mm can be completely removed.
The invention is further provided with the following steps: the length of the upper umbrella-shaped guide plate is 680-720 mm, and the inclination angle is 12-25 degrees.
By adopting the scheme, the design is reasonable, and the requirements of the flow speed and the thickness of the spinning solution are met.
The invention is further provided with the following steps: the length of the umbrella-shaped deflector at the lower layer is 980-1000mm, and the inclination angle is 12-25 degrees.
By adopting the scheme, the design is reasonable, and the requirements of the flow speed and the thickness of the spinning solution are met.
The invention is further provided with the following steps: the reaction kettle comprises a tank body and a defoaming device, wherein a feed inlet is formed in the upper portion of the tank body, a discharge outlet is formed in the bottom of the tank body, an annular feed pipe is arranged in the tank body and communicated with the feed inlet, an upper umbrella-shaped guide plate and a lower umbrella-shaped guide plate are sequentially arranged below the annular feed pipe, the upper umbrella-shaped guide plate and the lower umbrella-shaped guide plate are respectively arranged in a downward inclined mode, the annular feed pipe is provided with a plurality of liquid outlet holes at positions corresponding to the upper umbrella-shaped guide plate, the defoaming device comprises a rotary table and a cutter, the rotary table is arranged along the central axis of the tank body, the rotary table rotates around the central axis of the rotary table and moves up and down along the central axis of the rotary table, the cutter is provided with a plurality of driving mechanisms which are arranged on the rotary table at intervals, and the tank body is provided with a driving mechanism which drives the rotary table to rotate and drives the rotary table to move up and down.
Through adopting above-mentioned scheme, actuating mechanism not only can drive carousel and sword and reciprocate, can also drive carousel and sword and rotate, simple structure, reasonable in design.
The invention is further provided with the following steps: the outer edge of the lower umbrella-shaped guide plate extends to the side wall of the tank body, and the spinning solution is guided to the side wall of the tank body.
Through adopting above-mentioned scheme, the spinning solution flows into the bottom of jar body through the lateral wall of jar body, when flowing along the lateral wall of jar body, can form the solution film, also can increase the deaeration area, and the bubble of being convenient for deviate from, simple structure, reasonable in design.
The invention is further provided with the following steps: the upper umbrella-shaped guide plate is connected with the upper side wall of the tank body through a first connecting plate, the upper umbrella-shaped guide plate and the lower umbrella-shaped guide plate are connected with each other through a second connecting plate, and a baffle is arranged at the inner edge of the lower umbrella-shaped guide plate.
Through adopting above-mentioned scheme, the connected mode of guide plate is simple, and the baffle plays the backstop effect, avoids the spinning solution that leaves from upper umbrella-shaped guide plate to flow from the inner edge of lower floor umbrella-shaped guide plate.
The invention is further provided with the following steps: the tank body is also provided with a hole, a thermometer port, a vacuum port, a pressure gauge port, an air inlet, an acetic acid solution inlet, a safety valve port, a sampling port, a water inlet and a sight glass port.
Through adopting above-mentioned scheme, simple structure, reasonable in design.
The invention is further described below with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a reaction kettle;
FIG. 2 is a schematic top view of the reactor;
FIG. 3 is an enlarged schematic view of portion A of FIG. 1;
fig. 4 is a schematic view of the structure of the turntable and the knife.
Description of the embodiments
In the description of the present invention, it should be understood that the terms "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate description of the present invention and simplify the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Example 1, a spinning solution deaeration method for industrially producing pure chitosan fibers, comprising the following steps:
step one, sealing the reaction kettle, and vacuumizing to the vacuum degree of-75 kPa, wherein the constant temperature in the reaction kettle is kept to be 25 ℃, and the pressure in the reaction kettle is less than or equal to 5000Pa;
step two, a feed inlet of the reaction kettle is opened, spinning solution flows into an annular feed pipe through the feed inlet, then falls to an umbrella-shaped guide plate at the upper layer through a liquid outlet hole of the annular feed pipe, the liquid outlet hole is a round hole with the diameter smaller than 3mm, extrusion shearing operation is carried out on the spinning solution through the liquid outlet hole, and bubbles with the diameter larger than the liquid outlet hole are removed, so that the spinning solution subjected to primary defoaming is formed;
thirdly, automatically flowing the first defoamed spinning solution onto an upper umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the upper umbrella-shaped guide plate is 1.8t/h, the thickness of the liquid film is 6mm, the length of the upper umbrella-shaped guide plate is 680mm, the inclination angle is 12 degrees, and the second defoamed spinning solution is formed by removing bubbles in the film spreading process;
fourthly, automatically flowing the defoamed spinning solution onto the lower umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the lower umbrella-shaped guide plate is 1.8t/h, the thickness of the liquid film is 5mm, the length of the lower umbrella-shaped guide plate is 980mm, the inclination angle is 12 degrees, and the defoamed spinning solution is formed by removing bubbles in the film spreading process;
fifthly, the defoamed spinning solution flows into the bottom of the reaction kettle for the third time, the defoamed device of the reaction kettle moves along with the change of the liquid level of the spinning solution, the defoamed device can rotate at the rotation speed of 26 revolutions per minute, and the defoamed device cuts off bubbles on the liquid level of the spinning solution, so that the dynamic rotation defoamed operation of the spinning solution is realized;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and performing tertiary circulation to realize static defoaming operation of the spinning solution.
Example 2, a method for defoaming spinning solution for industrially producing pure chitosan fibers, comprises the following steps:
step one, sealing the reaction kettle, and vacuumizing, wherein the vacuum degree is-80 kPa, the constant temperature in the reaction kettle is kept at 27 ℃, and the pressure in the reaction kettle is less than or equal to 5000Pa;
step two, a feed inlet of the reaction kettle is opened, spinning solution flows into an annular feed pipe through the feed inlet, then falls to an umbrella-shaped guide plate at the upper layer through a liquid outlet hole of the annular feed pipe, the liquid outlet hole is a round hole with the diameter smaller than 3mm, extrusion shearing operation can be carried out on the spinning solution through the liquid outlet hole, and bubbles larger than the diameter of the liquid outlet hole are removed to form spinning solution subjected to primary defoaming;
thirdly, automatically flowing the first defoamed spinning solution onto an upper umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the upper umbrella-shaped guide plate is 2.1t/h, the thickness of the liquid film is 13mm, the length of the upper umbrella-shaped guide plate is 700mm, the inclination angle is 18 degrees, and the second defoamed spinning solution is formed by removing bubbles in the film spreading process;
fourthly, automatically flowing the defoamed spinning solution onto the lower umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the lower umbrella-shaped guide plate is 2.1t/h, the thickness of the liquid film is 11mm, the length of the lower umbrella-shaped guide plate is 990mm, the inclination angle is 18 degrees, and the defoamed spinning solution is formed by removing bubbles in the film spreading process;
fifthly, the defoamed spinning solution flows into the bottom of the reaction kettle for the third time, the defoamed device of the reaction kettle moves along with the change of the liquid level of the spinning solution, the defoamed device rotates at the rotation speed of 43 revolutions per minute, and the defoamed device cuts off bubbles on the liquid level of the spinning solution, so that the dynamic rotation defoamed operation of the spinning solution is realized;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and performing tertiary circulation to realize static defoaming operation of the spinning solution.
Example 3, a spinning solution deaeration method for industrially producing pure chitosan fibers, comprises the following steps:
step one, sealing the reaction kettle, and vacuumizing to the vacuum degree of-85 kPa, wherein the constant temperature in the reaction kettle is kept to be 30 ℃, and the pressure in the reaction kettle is less than or equal to 5000Pa;
step two, a feed inlet of the reaction kettle is opened, spinning solution flows into an annular feed pipe through the feed inlet, then falls to an umbrella-shaped guide plate at the upper layer through a liquid outlet hole of the annular feed pipe, the liquid outlet hole is a round hole with the diameter smaller than 3mm, extrusion shearing operation is carried out on the spinning solution through the liquid outlet hole, and bubbles with the diameter larger than the liquid outlet hole are removed, so that the spinning solution subjected to primary defoaming is formed;
thirdly, automatically flowing the first defoamed spinning solution onto an upper umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the upper umbrella-shaped guide plate is 2.4t/h, the thickness of the liquid film is 20mm, the length of the upper umbrella-shaped guide plate is 720mm, the inclination angle is 25 degrees, and the second defoamed spinning solution is formed by removing bubbles in the film spreading process;
fourthly, automatically flowing the defoamed spinning solution onto the lower umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the lower umbrella-shaped guide plate is 2.4t/h, the thickness of the liquid film is 18mm, the length of the lower umbrella-shaped guide plate is 990mm, the inclination angle is 25 degrees, and the defoamed spinning solution is formed by removing bubbles in the film spreading process;
fifthly, the defoamed spinning solution flows into the bottom of the reaction kettle for the third time, the defoamed device of the reaction kettle moves along with the change of the liquid level of the spinning solution, the defoamed device rotates at the rotation speed of 60 revolutions per minute, and the defoamed device cuts off bubbles on the liquid level of the spinning solution, so that the dynamic rotation defoamed operation of the spinning solution is realized;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and performing tertiary circulation to realize static defoaming operation of the spinning solution.
Comparative example 1 dynamic rotation defoaming was performed without using a defoaming device, and the other steps were the same as in example 2.
The number of bubbles in the dope was measured sequentially for example 1, example 2, example 3 and comparative example 1, as shown in table 1.
List one
In order to realize the method for defoaming the spinning solution, a reaction kettle is adopted for defoaming treatment, as shown in fig. 1-4: the reaction kettle comprises a tank body 1 and a defoaming device, wherein a feed inlet 11 is formed in the upper portion of the tank body 1, a discharge outlet 12 is formed in the bottom of the tank body 1, an annular feed pipe 2 is arranged in the tank body 1, the annular feed pipe 2 is communicated with the feed inlet 12, an upper umbrella-shaped guide plate 3 and a lower umbrella-shaped guide plate 4 are sequentially arranged below the annular feed pipe 2 in the tank body 1, the upper umbrella-shaped guide plate 3 and the lower umbrella-shaped guide plate 4 are respectively arranged in a downward inclined mode, a plurality of liquid outlet holes 21 are formed in the annular feed pipe 2 at positions corresponding to the upper umbrella-shaped guide plate 3, the defoaming device comprises a rotary disc 5 and a cutter 6, the rotary disc 5 is arranged along the central axis of the tank body 1, the rotary disc 5 rotates around the central axis of the rotary disc 5 and moves up and down along the central axis of the rotary disc 5, the cutter 6 is arranged on the rotary disc 5 at intervals, and a driving mechanism for driving the rotary disc 5 to rotate and drive the rotary disc 5 to move up and down is arranged on the tank body 1. The driving mechanism may be a structure of a motor and a transmission shaft, so long as the turntable can rotate or move, so that the driving mechanism is a conventional technology and is not specifically described herein.
Wherein the outer edge of the lower umbrella-shaped guide plate 4 extends to the side wall of the tank body 1, so that the spinning solution can be guided to the side wall of the tank body.
Wherein the upper umbrella-shaped guide plate 3 is connected with the upper side wall of the tank body 1 through a first connecting plate 71, the upper umbrella-shaped guide plate 3 and the lower umbrella-shaped guide plate 4 are connected with each other through a second connecting plate 72, and a baffle 41 is arranged at the inner edge of the lower umbrella-shaped guide plate 4.
The tank body 1 is also provided with an inlet hole 13, a thermometer port 14, a vacuum port 15, a pressure gauge port 16, an air inlet 17, an acetic acid solution inlet 18, a safety valve port 19, a sampling port 101, a water inlet 102 and a sight glass port 103.
The above embodiments are only preferred embodiments of the present invention, and common variations and substitutions by those skilled in the art within the scope of the technical solution of the present invention are included in the scope of the present invention.
Claims (1)
1. A spinning solution defoaming method for industrially producing pure chitosan fibers is characterized by comprising the following steps: the method comprises the following steps:
step one, sealing the reaction kettle, and vacuumizing, wherein the vacuum degree is-75 to-85 kPa, the constant temperature in the reaction kettle is kept at 25-30 ℃, and the pressure in the reaction kettle is less than or equal to 5000pa;
step two, a feed inlet of the reaction kettle is opened, spinning solution flows into an annular feed pipe through the feed inlet, then falls to an umbrella-shaped guide plate at the upper layer through a liquid outlet hole of the annular feed pipe, extrusion shearing operation is carried out on the spinning solution through the liquid outlet hole, and bubbles larger than the diameter of the liquid outlet hole are removed to form spinning solution for primary defoaming;
thirdly, automatically flowing the first defoamed spinning solution onto an upper umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the upper umbrella-shaped guide plate is 1.8-2.4t/h, the thickness of the liquid film is 6-20mm, and the second defoamed spinning solution is formed by removing bubbles in the process of spreading the film;
fourthly, automatically flowing the spinning solution subjected to the second deaeration onto the lower umbrella-shaped guide plate to form a liquid film, wherein the flow speed of the spinning solution on the lower umbrella-shaped guide plate is 1.8-2.4t/h, the thickness of the liquid film is 5-18mm, and removing bubbles in the process of spreading the film to form a spinning solution subjected to the third deaeration;
fifthly, the defoamed spinning solution flows into the bottom of the reaction kettle for the third time, the defoamed device of the reaction kettle moves along with the change of the liquid level of the spinning solution, the defoamed device rotates at the rotation speed of 26-60 revolutions per minute, and the defoamed device cuts off bubbles on the liquid level of the spinning solution, so that the dynamic rotation defoamed operation of the spinning solution is realized;
step six, standing the spinning solution in a reaction kettle, and deflating and evacuating the reaction kettle once every two hours to perform tertiary circulation so as to realize static defoaming operation of the spinning solution;
the liquid outlet hole is a round hole with the diameter smaller than 3mm, the length of the upper umbrella-shaped guide plate is 680-720 mm, the inclination angle is 12-25 degrees, the length of the lower umbrella-shaped guide plate is 980-1000mm, and the inclination angle is 12-25 degrees;
the reaction kettle comprises a tank body and a defoaming device, wherein a feed inlet is formed in the upper portion of the tank body, a discharge outlet is formed in the bottom of the tank body, an annular feed pipe is arranged in the tank body and communicated with the feed inlet, an upper umbrella-shaped guide plate and a lower umbrella-shaped guide plate are sequentially arranged below the annular feed pipe, the upper umbrella-shaped guide plate and the lower umbrella-shaped guide plate are respectively arranged in a downward inclined mode, the annular feed pipe is provided with a plurality of liquid outlet holes at positions corresponding to the upper umbrella-shaped guide plate, the defoaming device comprises a rotary table and a cutter, the rotary table is arranged along the central axis of the tank body, the rotary table rotates around the central axis of the rotary table and moves up and down along the central axis of the rotary table, the cutter is provided with a plurality of driving mechanisms which are arranged on the rotary table at intervals and drive the rotary table to rotate and drive the rotary table to move up and down;
the outer edge of the lower umbrella-shaped guide plate extends to the side wall of the tank body, the spinning solution is guided to the side wall of the tank body, the upper umbrella-shaped guide plate is connected with the upper side wall of the tank body through a first connecting plate, the upper umbrella-shaped guide plate and the lower umbrella-shaped guide plate are connected with each other through a second connecting plate, a baffle is arranged at the inner edge of the lower umbrella-shaped guide plate, and the tank body is further provided with a hole, a thermometer port, a vacuum port, a pressure gauge port, an air inlet, an acetic acid solution inlet, a safety valve port, a sampling port, a water inlet and a sight glass port.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210462468.7A CN114775069B (en) | 2022-04-28 | 2022-04-28 | Spinning solution defoaming method for industrially producing pure chitosan fibers |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210462468.7A CN114775069B (en) | 2022-04-28 | 2022-04-28 | Spinning solution defoaming method for industrially producing pure chitosan fibers |
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| CN113617064A (en) * | 2020-05-09 | 2021-11-09 | 中国石油化工股份有限公司 | Continuous defoaming device for high-viscosity fluid, application of continuous defoaming device and defoaming method for polyamide acid spinning solution |
| CN215781698U (en) * | 2021-09-27 | 2022-02-11 | 上海禧合应用材料有限公司 | Vacuum defoaming device |
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