CN114775069A - Spinning solution defoaming method for industrially producing pure chitosan fiber - Google Patents
Spinning solution defoaming method for industrially producing pure chitosan fiber Download PDFInfo
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- CN114775069A CN114775069A CN202210462468.7A CN202210462468A CN114775069A CN 114775069 A CN114775069 A CN 114775069A CN 202210462468 A CN202210462468 A CN 202210462468A CN 114775069 A CN114775069 A CN 114775069A
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- 238000009987 spinning Methods 0.000 title claims abstract description 126
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000835 fiber Substances 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 65
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 230000007480 spreading Effects 0.000 claims abstract description 16
- 238000003892 spreading Methods 0.000 claims abstract description 16
- 230000008859 change Effects 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 230000008569 process Effects 0.000 claims description 12
- 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 6
- 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
- 238000009776 industrial production Methods 0.000 claims 1
- 230000005484 gravity Effects 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000036541 health Effects 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
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000003544 deproteinization Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric 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
- 238000002360 preparation method Methods 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
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- 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)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a defoaming method of spinning solution for industrially producing pure chitosan fiber, which comprises the following steps: step one, sealing a reaction kettle and then vacuumizing; opening a feed inlet of the reaction kettle, allowing the spinning solution to flow into the annular feed pipe through the feed inlet, and allowing the spinning solution to fall to an upper umbrella-shaped guide plate through a liquid outlet hole of the annular feed pipe; thirdly, enabling the spinning solution subjected to primary defoaming to flow onto an umbrella-shaped guide plate on the upper layer to form a liquid film by gravity flow spreading; step four, flowing the spinning solution subjected to secondary defoaming onto a lower umbrella-shaped guide plate to automatically flow and form a liquid film; step five, the spinning solution defoamed for the third time flows into the bottom of the reaction kettle, a defoaming device of the reaction kettle can move along with the change of the liquid level of the spinning solution, and the defoaming device can rotate; 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 bubbles of the spinning solution can be quickly and uniformly removed in unit time, so that the requirement of industrial continuous production is met.
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 fiber.
Background
The chitosan fiber is prepared from the extract of shrimp and crab shells, and has a plurality of special advantages compared with the traditional terrestrial natural fiber and synthetic fiber. Firstly, the method does not depend on petroleum and compete for land with grains, and a third raw material source of chemical fibers is developed; and secondly, the waste is utilized, so that the method accords with the sustainable development trend of green and environmental protection. Furthermore, the pure chitosan fiber has broad-spectrum antibacterial activity, mildew resistance, excellent biocompatibility and no immunogenicity, and also has the effects of adsorbing and chelating, stopping bleeding, promoting healing and reducing scars. Based on the functional effects, the fabric can be widely applied to the fields of aerospace, medical treatment and health, military and civil textiles, filtration and protection and the like, has huge market potential, and plays a positive role in promoting the health career of human beings.
The degree of deacetylation and viscosity are two important quality indicators for chitosan. As is well known, the higher the molecular weight of chitosan, the higher the viscosity of the chitosan, and the relation between the viscosity and the molecular weight is shown by Mark-Houwink, namely: [ eta ] = K M alpha, (eta: viscosity, mpa · s, K: constant, M: relative molecular mass, alpha: a value related to molecular weight) it can be seen that the higher the viscosity of the pure chitosan dope, the larger the molecular weight, the higher the dry breaking strength of the spun pure chitosan fiber, the larger 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 better.
A key link for preparing chitosan fiber is to dissolve chitosan raw material, the chitosan raw material is generally flaky chitosan, a large amount of gaps can be generated in tissues of the flaky chitosan after decalcification and deproteinization, and the gaps can be filled with air; in addition, the flaky chitosan raw material is formed by overlapping 2 or more pieces, a large amount of gas also exists in gaps, and the gas is bonded in the chitosan solution in the chitosan dissolving process and cannot escape; meanwhile, a large amount of bubbles are generated in the processes of stirring, dissolving, filtering and conveying of the chitosan solution.
In wet spinning, the chitosan solution must have no bubbles to be sprayed out from a spinneret plate into a coagulating bath, if the chitosan solution carries bubbles to be sprayed into the coagulating bath, the bubbles escape to cause yarn breakage, and therefore defoaming treatment must be carried out 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 molecular chain original state structure of chitosan, can quickly and uniformly remove the bubbles of the spinning solution in unit time, and is suitable for the requirement of industrial continuous production.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for defoaming spinning solution for industrially producing pure chitosan fiber comprises the following steps:
step one, vacuumizing a sealed reaction kettle, wherein the vacuum degree is-75 to-85 kPa, keeping the constant temperature in the reaction kettle at 25 to 30 ℃, and the pressure in the reaction kettle is less than or equal to 5000 pa;
step two, opening a feed inlet of the reaction kettle, enabling the spinning solution to flow into an annular feed pipe through the feed inlet, and then enabling the spinning solution to fall to an upper umbrella-shaped guide plate through a liquid outlet hole of the annular feed pipe, wherein the liquid outlet hole can perform extrusion shearing operation on the spinning solution, and can remove bubbles with diameters larger than the diameter of the liquid outlet hole to form the first-time defoamed spinning solution;
step three, enabling the spinning solution subjected to primary defoaming to flow onto an upper umbrella-shaped guide plate to automatically form a liquid film by spreading, enabling the flow velocity of the spinning solution on the upper umbrella-shaped guide plate to be 1.8-2.4t/h, enabling the thickness of the liquid film to be 6-20mm, and removing bubbles in the film spreading process to form the spinning solution subjected to secondary defoaming;
step four, the spinning solution subjected to secondary defoaming flows onto a lower umbrella-shaped guide plate to automatically flow and form a liquid film, the flow rate of the spinning solution on the upper umbrella-shaped guide plate is 1.8-2.4t/h, the thickness of the liquid film is 5-18mm, and bubbles are removed in the film spreading process to form the spinning solution subjected to tertiary defoaming;
step five, enabling the spinning solution defoamed for the third time to flow into the bottom of the reaction kettle, enabling a defoaming device of the reaction kettle to move along with the change of the liquid level of the spinning solution, enabling the defoaming device to rotate at a rotating speed of 26-60 rpm, and enabling the defoaming device to cut bubbles on the liquid level of the spinning solution to achieve dynamic rotating defoaming operation of the spinning solution;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and generally performing three cycles 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 hole and is extruded out of the liquid outlet hole, and all bubbles with the diameter larger than that of the liquid outlet hole can be removed due to the small diameter of the liquid outlet hole and the pressure in the tank body smaller than 5000 pa; 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, under the condition that the pressure in the tank body is less than 5000pa, partial bubbles are freely removed by controlling the flow rate 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, partial bubbles freely escape by controlling the flow rate and the thickness of the spinning solution under the condition that the pressure in the tank body is less than 5000pa, and the defoaming rate can reach 30-40% after passing through the lower umbrella-shaped guide plate; certainly, the number of the umbrella-shaped guide plates can be increased to increase the times of deaeration, the lower umbrella-shaped guide plate 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, the bubbles on the liquid surface of the spinning solution can be cut through in a rotating mode, the dynamic rotating defoaming operation of the spinning solution is realized, the defoaming rate can reach 30-50%, when the spinning solution is kept stand in a reaction kettle, the bubbles in the spinning solution are removed, the air is discharged and evacuated once every two hours, three times of circulation is generally carried out, the defoaming rate can reach 10-20%, the static defoaming of the spinning solution is matched with the dynamic defoaming of a defoaming device, the defect that the spinning solution at the bottom of a tank body is difficult to defoam can be solved, the method ensures the molecular chain original state structure of the chitosan, and can quickly and uniformly remove the bubbles of the spinning solution in unit time, thereby being suitable for the requirement of industrial continuous production.
The invention further provides that: the liquid outlet hole is a round hole with the diameter smaller than 3 mm.
By adopting the scheme, the bubbles with the diameter of more than 3mm can be completely removed.
The invention further provides that: 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 further comprises the following steps: the length of the lower umbrella-shaped guide plate 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 further provides that: reation kettle is including jar body and fire fighting equipment, the upper portion of the jar body is provided with the feed inlet, and the bottom of the jar body is provided with the discharge gate, the internal annular inlet pipe that is provided with of jar, annular inlet pipe and feed inlet intercommunication, the jar body has set gradually upper umbrella-type guide plate and lower floor umbrella-type guide plate in the below of annular inlet pipe, and upper umbrella-type guide plate and lower floor umbrella-type guide plate downward sloping setting respectively, and annular inlet pipe is provided with a plurality of in the department that corresponds upper umbrella-type guide plate and goes out the liquid hole, fire fighting equipment includes carousel and sword, and the carousel sets up along the center pin of the jar body, and the carousel can rotate around its center pin and along the setting that its center pin reciprocated internal at the jar, and the sword is provided with a plurality of and the interval sets up on the carousel, sets up the actuating mechanism that drives the carousel rotation and drive the carousel and reciprocate on the jar body.
Through adopting above-mentioned scheme, actuating mechanism can not only drive carousel and sword and reciprocate, can also drive carousel and sword and rotate, simple structure, reasonable in design.
The invention further provides that: the outer edge of the lower umbrella-shaped guide plate extends to the side wall of the tank body, and the spinning solution can be guided to the side wall of the tank body.
By adopting the above scheme, the spinning solution flows into the bottom of the tank body through the side wall of the tank body, and when flowing along the side wall of the tank body, a solution film can be formed, the defoaming area can be increased, bubbles can be conveniently removed, the structure is simple, and the design is reasonable.
The invention further comprises 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 backstop effect, avoids flowing from the inner fringe department of lower floor umbrella-type guide plate from the spinning liquid that upper umbrella-type guide plate left.
The invention further provides the following steps: the tank body is also provided with an inlet 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.
By adopting the scheme, the structure is simple, and the design is reasonable.
The invention is further described below with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic view of the overall structure of a reaction vessel;
FIG. 2 is a schematic top view of a reaction vessel;
FIG. 3 is an enlarged view of the portion A of FIG. 1;
fig. 4 is a schematic view of the structure of the turntable and the knife.
Detailed Description
In the description of the present invention, it is to 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 orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention.
Embodiment 1, a method for defoaming spinning solution for industrially producing pure chitosan fiber, comprising the following steps:
step one, vacuumizing a sealed reaction kettle with the vacuum degree of-75 kPa, keeping the constant temperature in the reaction kettle at 25 ℃ and the pressure in the reaction kettle at or below 5000 pa;
step two, opening a feed inlet of the reaction kettle, enabling the spinning solution to flow into an annular feed pipe through the feed inlet, and then enabling the spinning solution to fall to an upper umbrella-shaped guide plate through a liquid outlet hole of the annular feed pipe, wherein the liquid outlet hole is a round hole with the diameter smaller than 3mm, the liquid outlet hole can perform extrusion shearing operation on the spinning solution, and bubbles larger than the diameter of the liquid outlet hole can be removed to form the spinning solution subjected to primary deaeration;
step three, enabling the spinning solution subjected to primary defoaming to flow onto an upper umbrella-shaped guide plate to automatically form a liquid film by spreading the spinning solution, wherein the flow velocity 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 removing bubbles in the film spreading process to form the spinning solution subjected to secondary defoaming;
step four, the spinning solution subjected to secondary defoaming flows onto an umbrella-shaped guide plate at the lower layer to automatically flow and form a liquid film, the flow velocity of the spinning solution on the umbrella-shaped guide plate at the upper layer is 1.8t/h, the thickness of the liquid film is 5mm, the length of the umbrella-shaped guide plate at the lower layer is 980mm, the inclination angle is 12 degrees, and bubbles are removed in the film spreading process to form the spinning solution subjected to tertiary defoaming;
step five, enabling the spinning solution subjected to third defoaming to flow into the bottom of the reaction kettle, enabling a defoaming device of the reaction kettle to move along with the change of the liquid level of the spinning solution, enabling the defoaming device to rotate at a rotation speed of 26 revolutions per minute, and enabling the defoaming device to cut bubbles on the liquid level of the spinning solution, so as to achieve dynamic rotation defoaming operation of the spinning solution;
and step six, standing the spinning solution in a reaction kettle, discharging gas and evacuating once every two hours, and generally performing three times of circulation to realize static defoaming operation of the spinning solution.
step one, sealing a reaction kettle, vacuumizing to a vacuum degree of-80 kPa, keeping the constant temperature in the reaction kettle at 27 ℃, and keeping the pressure in the reaction kettle at less than or equal to 5000 pa;
step two, opening a feed inlet of the reaction kettle, enabling the spinning solution to flow into an annular feed pipe through the feed inlet, and then enabling the spinning solution to fall to an umbrella-shaped guide plate on the upper layer through a liquid outlet hole of the annular feed pipe, wherein the liquid outlet hole is a round hole with the diameter smaller than 3mm, the liquid outlet hole can be used for carrying out extrusion shearing operation on the spinning solution, and bubbles larger than the diameter of the liquid outlet hole can be removed to form the first-time defoamed spinning solution;
step three, enabling the spinning solution subjected to primary defoaming to flow onto an upper umbrella-shaped guide plate to automatically form a liquid film by spreading the spinning solution, wherein the flow velocity 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 removing bubbles in the film spreading process to form the spinning solution subjected to secondary defoaming;
step four, the spinning solution subjected to secondary defoaming flows onto a lower umbrella-shaped guide plate to automatically flow and form a liquid film, the flow velocity of the spinning solution on the upper 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 bubbles are removed in the film spreading process to form the spinning solution subjected to tertiary defoaming;
step five, enabling the spinning solution defoamed for the third time to flow into the bottom of the reaction kettle, enabling a defoaming device of the reaction kettle to move along with the change of the liquid level of the spinning solution, enabling the defoaming device to rotate at a rotating speed of 43 revolutions per minute, and enabling the defoaming device to cut bubbles on the liquid level of the spinning solution to achieve dynamic rotating defoaming operation of the spinning solution;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and generally performing three cycles to realize static defoaming operation of the spinning solution.
Embodiment 3, a method for defoaming spinning solution for industrially producing pure chitosan fiber, comprising the following steps:
step one, vacuumizing a sealed reaction kettle with the vacuum degree of-85 kPa, keeping the constant temperature in the reaction kettle at 30 ℃ and the pressure in the reaction kettle less than or equal to 5000 pa;
step two, opening a feed inlet of the reaction kettle, enabling the spinning solution to flow into an annular feed pipe through the feed inlet, and then enabling the spinning solution to fall to an umbrella-shaped guide plate on the upper layer through a liquid outlet hole of the annular feed pipe, wherein the liquid outlet hole is a round hole with the diameter smaller than 3mm, the liquid outlet hole can be used for carrying out extrusion shearing operation on the spinning solution, and bubbles larger than the diameter of the liquid outlet hole can be removed to form the first-time defoamed spinning solution;
thirdly, enabling the spinning solution subjected to the first defoaming to flow onto an upper umbrella-shaped guide plate to automatically form a liquid film through spreading, enabling the flow speed of the spinning solution on the upper umbrella-shaped guide plate to be 2.4t/h, enabling the thickness of the liquid film to be 20mm, enabling the length of the upper umbrella-shaped guide plate to be 720mm, enabling the angle of inclination to be 25 degrees, and removing bubbles in the film spreading process to form the spinning solution subjected to the second defoaming;
step four, flowing the spinning solution subjected to secondary defoaming onto a lower-layer umbrella-shaped guide plate to form a liquid film by gravity flow spreading, wherein the flow velocity of the spinning solution on the upper-layer umbrella-shaped guide plate is 2.4t/h, the thickness of the liquid film is 18mm, the length of the lower-layer umbrella-shaped guide plate is 990mm, the inclination angle is 25 degrees, and removing bubbles in the film spreading process to form the spinning solution subjected to tertiary defoaming;
step five, enabling the spinning solution defoamed for the third time to flow into the bottom of the reaction kettle, enabling a defoaming device of the reaction kettle to move along with the change of the liquid level of the spinning solution, enabling the defoaming device to rotate at a rotation speed of 60 revolutions per minute, and enabling the defoaming device to cut bubbles on the liquid level of the spinning solution to achieve dynamic rotating defoaming operation of the spinning solution;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and generally performing three cycles to realize static defoaming operation of the spinning solution.
Comparative example 1, dynamic spin defoaming without defoaming device, and the other steps were the same as in example 2.
The number of bubbles in the spinning dope was measured for example 1, example 2, example 3 and comparative example 1 in order as shown in table 1:
watch 1
In order to realize the above-mentioned deaeration method for the spinning solution, deaeration treatment is performed using a reaction vessel, as shown in fig. 1 to 4: the reation kettle includes jar body 1 and fire fighting equipment, the upper portion of jar body 1 is provided with feed inlet 11, the bottom of jar body 1 is provided with discharge gate 12, be provided with annular inlet pipe 2 in the jar body 1, annular inlet pipe 2 and feed inlet 12 intercommunication, jar body 1 has set gradually upper umbrella-type guide plate 3 and lower floor umbrella-type guide plate 4 in the below of annular inlet pipe 2, upper umbrella-type guide plate 3 and lower floor umbrella-type guide plate 4 downward sloping setting respectively, annular inlet pipe 2 is provided with a plurality of play liquid hole 21 in corresponding upper umbrella-type guide plate 3 department, fire fighting equipment includes carousel 5 and sword 6, carousel 5 sets up along the center pin of jar body 1, setting that carousel 5 can rotate around its center pin and reciprocate along its center pin is in jar body 1, sword 6 is provided with a plurality of and the interval sets up on carousel 5, set up the drive mechanism that drives carousel 5 and rotate and drive carousel 5 and reciprocate on jar body 1. The driving mechanism can be a structure of a motor and a transmission shaft as long as the turntable can rotate or move, so that the driving mechanism is a conventional technology and is not specifically described in the text.
Wherein the outer edge of the lower umbrella-shaped guide plate 4 extends to the side wall of the tank body 1, and 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 the inner edge of the lower umbrella-shaped guide plate 4 is provided with a baffle 41.
Wherein, 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 general changes and substitutions by those skilled in the art within the technical scope of the present invention are included in the protection scope of the present invention.
Claims (8)
1. A spinning solution defoaming method for industrially producing pure chitosan fiber is characterized in that: the method comprises the following steps:
step one, sealing a reaction kettle, and vacuumizing to ensure that the vacuum degree is-75 to-85 kPa, keeping the constant temperature in the reaction kettle at 25 to 30 ℃, and the pressure in the reaction kettle is less than or equal to 5000 pa;
step two, opening a feed inlet of the reaction kettle, enabling the spinning solution to flow into an annular feed pipe through the feed inlet, and then enabling the spinning solution to fall to an upper umbrella-shaped guide plate through a liquid outlet hole of the annular feed pipe, wherein the liquid outlet hole can perform extrusion shearing operation on the spinning solution, and can remove bubbles with diameters larger than the diameter of the liquid outlet hole to form the first-time defoamed spinning solution;
thirdly, the spinning solution subjected to the first defoaming flows onto an upper umbrella-shaped guide plate to automatically flow and form a liquid film, the flow velocity 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 bubbles are removed in the film spreading process to form the spinning solution subjected to the second defoaming;
step four, the spinning solution subjected to secondary defoaming flows onto a lower umbrella-shaped guide plate to automatically flow and form a liquid film, the flow rate of the spinning solution on the upper umbrella-shaped guide plate is 1.8-2.4t/h, the thickness of the liquid film is 5-18mm, and bubbles are removed in the film spreading process to form the spinning solution subjected to tertiary defoaming;
step five, enabling the spinning solution subjected to third defoaming to flow into the bottom of the reaction kettle, enabling a defoaming device of the reaction kettle to move along with the change of the liquid level of the spinning solution, enabling the defoaming device to rotate at a rotation speed of 26-60 revolutions per minute, and enabling the defoaming device to cut bubbles on the liquid level of the spinning solution to achieve dynamic rotation defoaming operation of the spinning solution;
and step six, standing the spinning solution in a reaction kettle, deflating and evacuating the reaction kettle once every two hours, and generally performing three cycles to realize static defoaming operation of the spinning solution.
2. The method for industrially producing pure chitosan fiber dope defoaming as claimed in claim 1, wherein: the liquid outlet hole is a round hole with the diameter smaller than 3 mm.
3. The dope defoaming method for industrially producing pure chitosan fiber according to claim 1 or 2, wherein: the length of the upper umbrella-shaped guide plate is 680-720 mm, and the inclination angle is 12-25 degrees.
4. The dope defoaming method for industrially producing pure chitosan fiber according to claim 1 or 2, wherein: the length of the lower umbrella-shaped guide plate is 980-1000mm, and the inclination angle is 12-25 degrees.
5. The method for industrially producing pure chitosan fiber dope defoaming as claimed in claim 1, wherein: the reation kettle includes a jar body and fire fighting equipment, the upper portion of the jar body is provided with the feed inlet, and the bottom of the jar body is provided with the discharge gate, the internal annular inlet pipe that is provided with of jar, annular inlet pipe and feed inlet intercommunication, the jar body has set gradually upper umbrella-type guide plate and lower floor umbrella-type guide plate in the below of annular inlet pipe, and upper umbrella-type guide plate and lower floor umbrella-type guide plate downward sloping setting respectively, and annular inlet pipe is provided with a plurality of liquid hole in corresponding upper umbrella-type guide plate department, fire fighting equipment includes carousel and sword, and the carousel sets up along the center pin of the jar body, and the carousel can rotate around its center pin and along the setting that its center pin reciprocated internal at the jar, and the sword is provided with a plurality of and the interval sets up on the carousel, sets up the actuating mechanism that drives the carousel and rotate and drive the carousel and reciprocate on the jar body.
6. The dope defoaming method for the industrial production of pure chitosan fiber according to claim 5, characterized in that: the outer edge of the lower umbrella-shaped guide plate extends to the side wall of the tank body, and the spinning solution can be guided to the side wall of the tank body.
7. The dope defoaming method for industrially producing pure chitosan fiber according to claim 5 or 6, wherein: 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.
8. The dope defoaming method for industrially producing pure chitosan fiber according to claim 5 or 6, wherein: the tank body is also provided with an inlet 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.
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