WO2015027957A1 - 一种高黏度纯壳聚糖纺丝液的复合式脱泡方法 - Google Patents

一种高黏度纯壳聚糖纺丝液的复合式脱泡方法 Download PDF

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Publication number
WO2015027957A1
WO2015027957A1 PCT/CN2014/085696 CN2014085696W WO2015027957A1 WO 2015027957 A1 WO2015027957 A1 WO 2015027957A1 CN 2014085696 W CN2014085696 W CN 2014085696W WO 2015027957 A1 WO2015027957 A1 WO 2015027957A1
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Prior art keywords
kettle
degassing
umbrella
defoaming
spinning solution
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PCT/CN2014/085696
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English (en)
French (fr)
Inventor
周家村
胡广敏
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海斯摩尔生物科技有限公司
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Application filed by 海斯摩尔生物科技有限公司 filed Critical 海斯摩尔生物科技有限公司
Priority to US14/916,024 priority Critical patent/US10040003B2/en
Priority to JP2016539407A priority patent/JP6152479B2/ja
Priority to KR1020167008786A priority patent/KR101770659B1/ko
Priority to EP14841045.9A priority patent/EP3042706B1/en
Priority to CA2926041A priority patent/CA2926041C/en
Publication of WO2015027957A1 publication Critical patent/WO2015027957A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/02—Foam dispersion or prevention
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/91—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with propellers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
    • B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
    • B29B7/12—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with single shaft
    • B29B7/14—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with single shaft with screw or helix
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/84—Venting or degassing ; Removing liquids, e.g. by evaporating components
    • B29B7/845—Venting, degassing or removing evaporated components in devices with rotary stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/86—Component parts, details or accessories; Auxiliary operations for working at sub- or superatmospheric pressure
    • 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
    • D01D1/06—Feeding liquid to the spinning head
    • D01D1/065—Addition and mixing of substances to the spinning solution or to the melt; Homogenising
    • 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
    • D01D1/103—De-aerating
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • 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

Definitions

  • the present invention relates to a method for defoaming ultra-high viscosity spinning solution, and more particularly to a method for defoaming ultra-high viscosity pure chitosan spinning solution.
  • Pure chitosan fibers refer to fibers made from extracts from shrimp and crab shells, which have many special advantages over conventional terrestrial natural fibers and synthetic fibers. The first is that it does not rely on oil, nor does it compete with food for land, and opens up a third source of chemical fiber. Second, waste utilization is in line with the sustainable development trend of green and environmental protection. Further, the pure chitosan fiber has broad-spectrum bacteriostasis, mildew resistance, excellent biocompatibility and non-immunogenicity, and also has the functions of adsorption chelation, hemostasis, and scar reduction. Based on its function, it can be widely used in aerospace, medical and health, military civil textiles, filtration protection and other fields. It has great market potential and plays a positive role in promoting human health.
  • the flaky chitosan itself has a large amount of gaps in the tissue after decalcification and deproteinization, and these gaps have air filling; in addition, the flaky chitosan raw material is a stack of 2 or more sheets. It also has a large amount of gas between the gaps. These gases are bound to the inside of the chitosan solution during the dissolution of chitosan, and cannot escape; at the same time, the chitosan spinning solution is dissolved, filtered, and transported. Part of the bubbles are also generated during the process, and these bubbles are transported to the defoaming kettle along with the spinning solution.
  • the spinning solution In wet spinning, the spinning solution must be ejected from the spinneret into the coagulation bath without bubbles. If the spinning solution has a bubble jet to the coagulation bath, the bubbles will escape and the filament will be broken.
  • the viscosity of the spinning solution of sugar fiber is greater than 4 50000mpa ⁇ s, the viscosity of the spinning solution is nearly ten times that of the usual viscose spinning solution. It is defoamed by a conventional process and has extremely low production efficiency, making it difficult to achieve industrial production.
  • the technical problem to be solved by the present invention is to overcome the deficiencies of the prior art, and provide a defoaming method with high defoaming efficiency, good defoaming effect, and wide application of a wide range of viscosity of the spinning solution.
  • a composite defoaming method for a high-viscosity pure chitosan spinning solution comprising the following steps: [0009] Step 1, the spinning solution is fully dissolved through a dissolution vessel, and the viscosity thereof is reached.
  • Step two the spinning solution in the first step, from the dissolution tank powered by compressed air, through a filter, and sent to the feed port of the defoaming kettle;
  • Step 3 in the defoaming kettle, under the condition of vacuuming and maintaining the pressure in the defoaming kettle of 500pa - 3000pa, the spinning solution in the second step is integrated into the film by separation, scraping, lifting and shearing.
  • the composite defoaming method is continuously processed, and specifically includes:
  • a) high-pressure separation shear the spinning liquid that is transported by the above-mentioned compressed aerodynamics to the feed port of the defoaming kettle in the second step, is extruded through the discharge orifice filled in the bottom of the annular feed pipe ;
  • step (c) is performed cyclically;
  • Step 4 through the spinning solution of step 3, sampling at the sampling port to detect the degree of defoaming, and after passing the test, the defoaming process is completed; if not, repeat step 3 until the test is passed to complete the defoaming process.
  • the defoaming kettle comprises a defoaming kettle body (1) and a stirring device (2), and the upper part of the defoaming kettle body (1) is provided with a feeding port (3), a vacuum port (5), and destruction.
  • An inner cylinder body (9) is fixedly disposed at a position of a shaft center in the defoaming kettle body (1), and an upper end portion of the inner cylinder body (9) is filled with a diameter of 0.5 mm.
  • the circular plate of the 5mm liquid discharge orifice (11) is closed, and the lower end cylinder body opening is open;
  • the outer circumference of the upper half of the inner cylinder body (9) is fixed with an umbrella-shaped diffuser plate (10), and the inner cylinder body (9) Divided into upper and lower portions by the umbrella-shaped diffuser plate (10); a gap of 100 mm - 200 mm is formed between the outer edge of the umbrella-shaped diffuser plate (10) and the inner wall of the defoaming kettle body (1);
  • the inner cylinder body (9) is filled with a small hole (11) having a diameter of 0.5 mm to 5 mm on the upper portion of the umbrella-shaped diffuser plate (10);
  • the lower edge of the umbrella diffuser (10) is above the effective volume level of the defoaming kettle body (1), the axis of the umbrella diffuser (10) and the inner cylinder (9)
  • the angle a 65 ° ⁇ 80 °;
  • the agitation power device 13 includes a motor, a reducer, and a power bracket 25, and the power bracket 25 is installed at a center position of a top outer wall of the reaction vessel 1, and a reducer and a motor are mounted on the power bracket 25;
  • the upper end is mounted on the agitating power unit 13, specifically, the agitating shaft 12 is coupled with the output shaft of the speed reducer; the agitating shaft 12 passes downwardly from the upper end through the mounted bearing provided in the power bracket 25, and passes through the sealing reaction.
  • the mechanical seal device 16 having a gap between the kettle 1 and the agitating shaft 12 is inserted into the dissolution vessel 1, and the lower end is fixed to the bottom seat bearing 6, and the agitator shaft 12 is more stable after being fixed by the upper and lower ends.
  • the spinning solution is driven from the dissolution vessel by a compressed air of 0.8 MPa to 1.2 MPa, filtered through a two-stage filter, and sent to a feed port of the defoaming kettle.
  • the agitating shaft with the propeller is lifted to the umbrella-shaped diffuser plate at a speed of 60-90 rpm.
  • the beneficial effects of the present invention are: [0026] a, because the upper part of the kettle body is provided with an annular feed pipe, the annular feed pipe is connected with the feed port and the bottom is provided with a plurality of discharge small holes, high viscosity pure chitosan with pressure When the spinning solution enters the annular feed pipe through the feed port and is extruded from the discharge orifice, the diameter of the discharge orifice is only 0.
  • the first defoaming of the pure chitosan spinning solution evenly drip on the umbrella-shaped diffuser, due to the effect of gravity and the angle of inclination of the umbrella-shaped diffuser, the spinning solution from the umbrella
  • the inner edge of the diffuser flows toward the outer edge of the umbrella-shaped diffuser, and the formed spinning film increases the defoaming area.
  • the pressure in the defoaming kettle is less than 3000pa, some bubbles are free to escape; the spinning solution When flowing to the outer edge of the umbrella-shaped diffuser, the spinning solution is free to flow down to the bottom of the reactor under the action of gravity.
  • the outer edge of the umbrella-shaped diffuser plate shears the spinning solution, and the spinning solution interface layer A change occurs, the bubble quickly escapes, and the second defoaming process of the wiped film is completed.
  • the defoaming kettle of the present invention has an inner cylinder and a stirring shaft with a propeller, and the inner cylinder wall and the upper end sealing cover of the umbrella-shaped diffuser plate are filled with liquid
  • the special structure of the small hole, the pure chitosan spinning solution which realizes the second defoaming process is stirred by the propeller, and is lifted from the bottom of the kettle body to the upper part of the inner cylinder body.
  • the defoaming effect of the (a) process can be achieved by extrusion through the liquid outlet orifice; the defoaming effect of the process (b) is achieved during the process of spinning the droplets onto the top of the umbrella-shaped diffuser plate to the bottom of the kettle body,
  • the completion of this agitation lifting device achieves the defoaming effect of the two defoaming processes (a) and (b).
  • the disadvantage of the conventional defoaming method in which the spinning solution at the bottom of the defoaming tank is difficult to defoam is avoided.
  • the unit operates continuously for high efficiency, high quality defoaming.
  • 1 is a flow chart of the present invention
  • 2 is a schematic structural view of the present invention
  • Example 1 6 tons of ultra-high viscosity pure chitosan spinning solution with a viscosity of 500000 mpa ⁇ s fully dissolved in a dissolution kettle, powered by compressed air of 0. 8Mpa from the dissolution kettle, through two-stage filtration Filtered, sent to the feed port of the defoaming kettle, and then into the annular feed pipe in the defoaming kettle which is vacuumed and continuously maintained at a pressure of 500pa in the defoaming tank and extruded from the discharge orifice, the spinning solution Freely falling under the action of gravity to the umbrella-shaped diffuser plate, the bubbles in the spinning solution are sheared when separated from the discharge orifice, the interface layer of the spinning solution changes, the bubbles quickly escape, and the high-pressure separation shear is completed.
  • the first defoaming process 6 tons of ultra-high viscosity pure chitosan spinning solution with a viscosity of 500000 mpa ⁇ s fully dissolved in
  • the first defoaming pure chitosan spinning solution is uniformly trickled on the umbrella-shaped diffuser plate, and the spinning solution is dispersed from the umbrella shape due to the action of gravity and the inclination angle of the umbrella-shaped diffuser plate.
  • the inner edge of the flow plate flows toward the outer edge of the umbrella-shaped diffuser plate, and the spinning liquid film formed increases the defoaming area.
  • the spinning solution flows to the umbrella
  • the outer edge of the diffuser is used, the spinning solution is free to flow down to the bottom of the reactor under the action of gravity.
  • the outer edge of the umbrella-shaped diffuser plate shears the spinning solution, and the interface layer of the spinning solution changes. The bubble is quickly released, and the second defoaming process of the wiper film is completed.
  • the pure chitosan spinning solution for realizing the second defoaming process is stirred by a propeller, and is lifted from the propeller to the umbrella shape by a stirring shaft with a propeller at a constant speed of 90 rpm.
  • the defoamed spinning solution is sampled, and the sample is taken at the sampling port to detect the degree of defoaming. After passing the test, the defoaming process is completed; if it is not, the step 3 is repeated until the test is passed to complete the defoaming process. .
  • the continuous defoaming treatment is carried out by a combination of separation, scraping, lifting, and shearing, and the high-viscosity pure chitosan spinning of 6 tons of viscosity which is fully dissolved in the dissolution vessel is 500000 mpa ⁇ s. Liquid 6 - 8 hours to remove the bubbles.
  • Example 2 Repeat the steps of the first embodiment, the dissolution of the fully dissolved 6 tons of ultra-high viscosity pure chitosan spinning solution with a viscosity of 450,000 mpa ⁇ s, with 1.2 Mpa compressed air as the power; In the case of vacuum and continuous maintenance of the defoaming kettle at a pressure of 3000 Pa in the defoaming kettle; the stirring shaft was rotated at a constant speed of 60 rpm; the high efficiency and high quality defoaming of the present invention was achieved.
  • Example 3 Repeat the steps of the first embodiment, the 6 ton of ultra-high viscosity pure chitosan spinning solution with a viscosity of 480,000 mpa ⁇ s fully dissolved in the dissolution kettle, powered by compressed air of 1.0 MPa; In the case of a vacuum and continuously maintaining a defoaming kettle having a pressure of 2000 Pa in the defoaming kettle; the stirring shaft was rotated at a constant speed of 70 rpm; and the high efficiency and high quality defoaming of the present invention was achieved.
  • the invention not only realizes continuous industrial production but also reduces the degradation of the spinning solution viscosity by improving the efficiency of defoaming of the pure chitosan spinning solution, thereby ensuring the quality of the pure chitosan fiber.
  • the invention is also applicable to the defoaming of other high viscosity spinning solutions.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

一种高黏度纯壳聚糖纺丝液的复合式脱泡方法，包括如下步骤：一，纺丝液经过溶解釜充分溶解，其黏度达到450000mpa.s---500000mpa.s，待用；二，将步骤一中待用的纺丝液，从溶解釜以压缩空气为动力，通过过滤，输送到脱泡釜（1）的进料口（3）处；三，在脱泡釜（1）中，持续保持脱泡釜（1）内压力500pa---3000pa的条件下，通过集分离、刮膜、提升、剪切于一体的复合式脱泡方法进行连续处理；四，在取样口（18）取样进行脱泡程度的检测，经检测合格则完成脱泡过程；若不合格则重复步骤三，直至检测合格从而完成脱泡过程。

Description

说明书 发明名称： 一种高黏度纯壳聚糖纺丝液的复合式脱泡方法 技术领域
[0001] 本发明涉及一种超高黏度纺丝液的脱泡方法，尤其涉及一种超高黏度纯壳聚糖 纺丝液的脱泡方法。
背景技术
[0002] 纯壳聚糖纤维是指利用虾蟹壳中的提取物制成的纤维， 与传统的陆地天然纤维 与合成纤维相比具有许多特殊优点。 首先是既不依赖石油， 又不与粮食争夺土 地， 开辟了化学纤维的第三原料来源； 二是废物利用， 符合绿色、 环保的可持 续发展趋势。 进一步讲， 纯壳聚糖纤维具有广谱抑菌性、 防霉性、 优异的生物 相容性和无免疫原性， 还具有吸附螯合， 止血促愈、 减少疤痕的作用。 基于其 功能作用， 可广泛应用于航天、 医疗卫生、 军用民用纺织品、 过滤防护等领域 ， 市场潜力巨大， 同时对人类的健康事业的起到积极地推动作用。
[0003] 脱乙酰度和黏度是壳聚糖的两个重要质量指标。 众所周知， 壳聚糖分子量越大 ， 其黏度越大， 黏度与分子量的关系 Mark-Houwink表明， SP : [ ] = k M °，
( ： 黏度， mpa · s， K: 常数， Μ: 相对分子质量， α： 是一个与分子量有关 的数值） 由此就可以看出纯壳聚糖纺丝液的黏度越高， 其分子量越大， 所纺制 的纯壳聚糖纤维的干断裂强度越高， 断裂伸长率越大， 可纺性越好。 因此， 只 有髙黏度的纯壳聚糖纺丝液才更符合高品质纯壳聚糖纤维的纺丝要求， 现在纺 制出高品质的纯壳聚糖纤维所需的纺丝液的黏度以大于 450000mpa · s为宜。
[0004] 片状壳聚糖本身在脱钙、 脱蛋白质后， 其组织中会产生大量的间隙， 这些间隙 会有空气充盈； 另外， 片状壳聚糖原料是 2片或多片的叠合而成， 其间隙间也存 有大量气体， 这些气体在壳聚糖溶解过程中， 粘结在壳聚糖溶液内部， 无法逸 出； 同时， 壳聚糖纺丝液在搅拌溶解、 过滤、 输送的过程中也会产生部分气泡 ， 这些气泡随纺丝液被输送到脱泡釜内。
[0005] 湿法纺丝时， 纺丝液必须无气泡从喷丝板喷出进入凝固浴， 若纺丝液带有气泡 喷丝至凝固浴， 气泡逸出会导致断丝， 同时纯壳聚糖纤维的纺丝液的黏度大于 4 50000mpa · s， 该黏度的纺丝液是通常黏胶纺丝液黏度的近十倍， 采用常规工艺 脱泡， 生产效率极低， 难以实现工业化生产。
技术问题
[0006] 本发明所要解决的技术问题是克服现有技术的不足， 提供一种脱泡效率高、 脱 泡效果好， 适用纺丝液的黏度范围广的脱泡方法。
问题的解决方案
技术解决方案
[0007] 本发明所采用的技术方案是 ：
[0008] 一种高黏度纯壳聚糖纺丝液的复合式脱泡方法， 其特征在于， 包括如下步骤： [0009] 步骤一， 纺丝液经过溶解釜充分溶解， 其黏度达到
450000—— 500000mpa. s, 待用；
[0010] 步骤二， 将步骤一中的纺丝液， 从溶解釜以压缩空气为动力， 通过过滤器， 输 送至脱泡釜的进料口；
[0011] 步骤三， 脱泡釜中， 在抽真空且持续保持脱泡釜内压力 500pa -— 3000pa的条件 下， 步骤二中的纺丝液通过集分离、 刮膜、 提升、 剪切于一体的复合式脱泡方 法进行连续处理， 具体包括：
[0012] a) 高压分离剪切： 将步骤二中通过上述压缩空气动力输送到脱泡釜进料口处 的纺丝液， 通过环状进料管道底部上布满的出料小孔挤出；
[0013] b ) 刮膜剪切： 上述 （a) 步骤中挤出的纺丝液滴落在脱泡釜内的伞状散流板上
， 从伞状散流板内边缘向伞状散流板外边缘流动， 当流至伞状散流板外边缘处 时滴流至脱泡釜的底部；
[0014] c ) 提升分离剪切、 刮膜剪切： 上述 （b ) 步骤中滴流至脱泡釜的底部的纺丝液 经带有螺旋浆的搅拌轴提升至位于伞状散流板上方的内筒体内， 再经出液小孔 分离滴流到伞状散流板， 后沿伞状散流板滴流到脱泡釜的底部；
[0015] 上述 （c ) 步骤循环进行；
[0016] 所述步骤三的 a、 b、 c在所述脱泡釜中完成；
[0017] 步骤四， 经步骤三的纺丝液， 在取样口取样进行脱泡程度的检测， 经检测合 格则完成脱泡过程； 若不合格则重复步骤三， 直至检测合格从而完成脱泡过程 [0018] 所述脱泡釜， 包括脱泡釜体（1)、 搅拌装置 (2)， 所述脱泡釜体（1)上部设有进 料口 （3)、 真空口 （5) 、 破坏真空进气口 （15) 、 真空表 （17) ； 底部中心位 置设有出料口（4)， 底部侧面设有取样口 （18); 所述脱泡釜体（1)内上方固定设 有环状进料管道 (7)， 所述环状进料管道 (7)与进料口 （3) 连通， 所述环状进料 管道（7)水平中心面以下部分布满直径为 0.5mm-5mm出料小孔 （8) ；
[0019] 在所述脱泡釜体（1)内的轴心位置固定设置有内筒体 （9) ， 所述内筒体 （9) 的上端部筒体口用布满直径为 0.5mm-5mm出液小孔 （11) 的圆板封闭， 下端部筒 体口开放； 内筒体 （9) 上半部的外周上固定设有伞状散流板 （10) ， 内筒体 （ 9) 被伞状散流板 （10) 分成上部与下部两部分； 所述伞状散流板 （10) 的外边 缘与脱泡釜体（1)的内壁之间有 100mm-200mm的间隙； 所述内筒体 （9) 在伞状散 流板 （10) 上面部分的筒体上布满直径为 0.5mm-5mm出液小孔 （11) ；
[0020] 所述伞状散流板 （10) 下边缘在脱泡釜体（1)的有效容积液面之上， 所述伞状 散流板（10)与内筒体 （9) 的轴线夹角 a = 65° 〜80° ；
[0021] 所述搅拌动力装置 13包括电机、 减速机、 动力支架 25， 动力支架 25安装在反 应釜 1的顶部外壁中心位置上， 在动力支架 25上安装着减速机和电机； 搅拌轴 12 的上端安装在搅拌动力装置 13上， 具体是搅拌轴 12和减速机的输出轴联动； 所 述搅拌轴 12从上端向下穿过动力支架 25内设有的带座轴承， 穿过用来密封反应 釜 1与述搅拌轴 12之间装配间隙的机械密封装置 16， 进入溶解釜 1中， 下端固定 在底部带座轴承 6上 ， 通过上下两端固定后， 搅拌轴 12运行更稳定。
[0022] 所述内筒体 （9) 的内壁与螺旋浆 （14) 之间有 3mm-5mm的间隙。
[0023] 在步骤二中， 纺丝液从溶解釜以 0.8Mpa -— 1.2Mpa的压缩空气为动力， 通过两 级过滤器过滤， 输送到脱泡釜的进料口处。
[0024] 在步骤三中， 所述的带有螺旋浆的搅拌轴以 60 -90转 /分钟的转速， 将脱泡釜 底部的纺丝液提升到伞状散流板上。
发明的有益效果
有益效果
[0025] 本发明的有益效果是 ： [0026] a、 由于釜体内上方设有环状进料管道， 所述环状进料管道与进料口连通且 底部设有多个出料小孔， 带有压力的高黏度纯壳聚糖纺丝液通过进料口进入环 状进料管道再由出料小孔挤出时， 由于出料小孔直径仅有 0. 5mm-5mm， 且脱泡釜 内压力小于 3000pa， 纺丝液在重力的作用下自由下落至伞状散流板上， 纺丝液 内的气泡从出料小孔分离时受到剪切， 纺丝液界面层发生变化， 气泡快速脱出 ， 完成高压分离剪切的第一次脱泡过程。
[0027] b、 实现第一次脱泡的纯壳聚糖纺丝液均匀的滴流在伞状散流板上， 由于重力 的作用和伞状散流板的倾斜角度， 纺丝液从伞状散流板内边缘向伞状散流板外 边缘流动， 形成的纺丝液薄膜， 增大了脱泡面积， 在脱泡釜内压力小于 3000pa 条件下， 部分气泡自由逸出； 纺丝液流到伞状散流板外边缘时， 纺丝液在重力 的作用下自由下流至反应釜底部， 下流时， 伞状散流板外边缘对纺丝液产生剪 切作用， 纺丝液界面层发生变化， 气泡快速脱出， 完成刮膜剪切的第二次脱泡 过程。
[0028] c、 本发明所述的脱泡釜具有内筒体和带有螺旋浆的搅拌轴， 以及所述伞状散 流板上部的内筒体壁和上端部密封盖上布满出液小孔的特殊结构的， 实现第二 次脱泡过程的纯壳聚糖纺丝液经过螺旋浆搅拌， 从釜体底部提升至内筒体的上 部， 那么， 这些纯壳聚糖纺丝液只能通过出液小孔挤出， 实现 （a) 过程的脱泡 效果； 当纺丝液滴流到伞状散流板上面至釜体底部的过程中， 实现 （b ) 过程的 脱泡效果， 完成这一搅拌提升装置的一个流程就实现了 （a) 和 （b ) 两个脱泡 过程的脱泡效果。 特别是避免了常规脱泡法在脱泡釜底部的纺丝液难以脱泡的 弊病。 此装置连续运行， 实现高效率、 高质量脱泡。
[0029] d、 从脱泡的实际效果来看： 在同容积、 同截面积的脱泡釜内用本发明， 6吨黏 度为 500000 mpa · s的纯壳聚糖纺丝液 8小时内能完全脱泡， 用常规脱泡技术， 6 吨黏度为 500000 mpa · s的纯壳聚糖纺丝液 40—55小时能完全脱泡， 可见， 本发 明能提高脱泡效率 5-7倍。
对附图的简要说明
附图说明
[0030] 图 1为本发明的流程图； [0031] 图 2为本发明的结构示意图；
[0032] 说明书中数字说明：
[0033] 脱泡釜体 --- 1， 搅拌装置 --- 2， 进料口 -一 3， 出料口 --- 4， 真空口 --- 5， 带 座滑动轴承一-6 ， 环状进料管道一-7， 出料小孔一-8， 内筒体一-9， 伞状散流 板 --- 10， 出液小孔 --- 11， 搅拌轴 --- 12， 搅拌动力装置 --- 13， 螺旋浆 -一 14， 破坏真空进气口 -— 15， 机械密封装置 --- 16， 真空表 -一 17， 取样口 -一 18。 实施该发明的最佳实施例
本发明的最佳实施方式
[0034] 为了把本专利说明清楚， 现结合附图 1、 2, 具体说明如下。
[0035] 实施例一： 经过溶解釜充分溶解的 6吨黏度为 500000 mpa · s的超高黏度纯壳聚 糖纺丝液， 从溶解釜以 0. 8Mpa的压缩空气为动力， 通过两级过滤器过滤， 输送 到脱泡釜的进料口后， 再进入抽真空且持续保持脱泡釜内压力 500pa的脱泡釜中 的环状进料管道并由出料小孔挤出， 纺丝液在重力的作用下自由下落至伞状散 流板上， 纺丝液内的气泡从出料小孔分离时受到剪切， 纺丝液界面层发生变化 ， 气泡快速脱出， 完成高压分离剪切的第一次脱泡过程。
[0036] 实现第一次脱泡的纯壳聚糖纺丝液均匀的滴流在伞状散流板上， 由于重力的作 用和伞状散流板的倾斜角度， 纺丝液从伞状散流板内边缘向伞状散流板外边缘 流动， 形成的纺丝液薄膜， 增大了脱泡面积， 在脱泡釜内压力 500pa条件下， 部 分气泡自由逸出； 纺丝液流到伞状散流板外边缘时， 纺丝液在重力的作用下自 由下流至反应釜底部， 下流时， 伞状散流板外边缘对纺丝液产生剪切作用， 纺 丝液界面层发生变化， 气泡快速脱出， 完成刮膜剪切的第二次脱泡过程。
[0037] 实现第二次脱泡过程的纯壳聚糖纺丝液经过螺旋浆搅拌， 经带有螺旋浆的搅拌 轴， 以匀速 90转 /分钟的转速， 由螺旋浆提升至所述伞状散流板上部的内筒体内 ， 由于所述伞状散流板上部的内筒体筒壁和上部筒口上设有若干出液小孔， 这 些纺丝液通过出液小孔挤出， 实现 （a) 过程的脱泡效果； 当纺丝液滴流到伞状 散流板上面至釜体底部的过程中， 实现 （b ) 过程的脱泡效果， 完成这一搅拌提 升装置的一个流程就实现了 （a) 和 （b ) 两个脱泡过程的效果。 特别是避免了 常规脱泡法在脱泡釜底部的纺丝液难以脱泡的弊病。 此装置连续运行， 实现高 效率、 高质量脱泡。
[0038] 经搅拌提升脱泡后的纺丝液， 在取样口取样进行脱泡程度的检测， 经检测合格 则完成脱泡过程； 若不合格则重复步骤三， 直至检测合格从而完成脱泡过程。
[0039] 这样， 通过集分离、 刮膜、 提升、 剪切于一体的复合式进行连续脱泡处理， 经 过溶解釜充分溶解的 6吨黏度为 500000 mpa · s的高黏度纯壳聚糖纺丝液 6 -— 8小 时将气泡脱离干净。
发明实施例
本发明的实施方式
[0040] 实施例二： 重复实施例一的步骤， 溶解釜充分溶解的 6吨黏度为 450000 mpa · s 的超高黏度纯壳聚糖纺丝液， 以 1. 2Mpa的压缩空气为动力； 抽真空且持续保持 脱泡釜内压力 3000pa的脱泡釜的情况下； 搅拌轴以匀速 60转 /分钟的转速； 实现 本发明高效率、 高质量脱泡。
[0041] 实施例三： 重复实施例一的步骤， 溶解釜充分溶解的 6吨黏度为 480000 mpa · s 的超高黏度纯壳聚糖纺丝液， 以 l. OMpa的压缩空气为动力； 抽真空且持续保持 脱泡釜内压力 2000pa的脱泡釜的情况下； 搅拌轴以匀速 70转 /分钟的转速； 实现 本发明高效率、 高质量脱泡。
工业实用性
[0042] 众所周知， 纯壳聚糖纺丝液的黏度越高， 由其制备成的壳聚糖纤维干断裂强度 越高， 断裂伸长率越高， 可纺性越好。 在常温下， 纯壳聚糖纺丝液会随着时间 的延长发生降解， 黏度降低， 这就导致制备成的纯壳聚糖纤维质量下降。
[0043] 本发明通过提高纯壳聚糖纺丝液脱泡的效率不但实现了连续的工业化生产而且 减少了纺丝液黏度的降解， 从而保证了纯壳聚糖纤维的品质。
[0044] 该发明也适用其他高黏度纺丝液的脱泡。

Claims

权利要求书
[权利要求 1] 一种高黏度纯壳聚糖纺丝液的复合式脱泡方法， 其特征在于， 包 括如下步骤：
步骤一， 纺丝液经过溶解釜充分溶解， 其黏度达到
450000—- 500000mpa. s, 待用；
步骤二， 将步骤一中的纺丝液， 从溶解釜以压缩空气为动力， 通 过过滤器， 输送至脱泡釜的进料口；
步骤三， 脱泡釜中， 在抽真空且持续保持脱泡釜内压力 500pa -— 3 OOOpa的条件下， 步骤二中的纺丝液通过集分离、 刮膜、 提升、 剪 切于一体的复合式脱泡方法进行连续处理， 具体包括：
a) 高压分离剪切： 将步骤二中通过上述压缩空气动力输送到脱泡 釜进料口处的纺丝液， 通过环状进料管道底部上布满的出料小孔 挤出；
b ) 刮膜剪切： 上述 （a) 步骤中挤出的纺丝液滴落在脱泡釜内的 伞状散流板上， 从伞状散流板内边缘向伞状散流板外边缘流动， 当流至伞状散流板外边缘处时滴流至脱泡釜的底部；
c ) 提升分离剪切、 刮膜剪切： 上述 （b ) 步骤中滴流至脱泡釜的 底部的纺丝液经带有螺旋浆的搅拌轴提升至位于伞状散流板上方 的内筒体内， 再经出液小孔分离滴流到伞状散流板， 后沿伞状散 流板滴流到脱泡釜的底部；
上述 （c ) 步骤循环进行；
所述步骤三的 a、 b、 c在所述脱泡釜中完成； 步骤四， 经步骤三的纺丝液， 在取样口取样进行脱泡程度的检测 ， 经检测合格则完成脱泡过程； 若不合格则重复步骤三， 直至检 测合格从而完成脱泡过程。
[权利要求 2] 如权利要求 1所述一种高黏度纯壳聚糖纺丝液的复合式脱泡方法， 其特征在于， 在步骤二中， 纺丝液从溶解釜以 0. 8Mpa -— 1. 2Mpa的 压缩空气为动力， 通过两级过滤器过滤， 输送到脱泡釜的进料口 处。
[权利要求 3] 如权利要求 1或 2所述一种高黏度纯壳聚糖纺丝液的复合式脱泡方 法， 其特征在于， 在步骤三中， 所述的带有螺旋浆的搅拌轴以 60- 90转 /分钟的转速， 将脱泡釜底部的纺丝液提升到伞状散流板上
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