CN115787120A - Protein modified lyocell fiber and production method thereof - Google Patents
Protein modified lyocell fiber and production method thereof Download PDFInfo
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- CN115787120A CN115787120A CN202211164634.1A CN202211164634A CN115787120A CN 115787120 A CN115787120 A CN 115787120A CN 202211164634 A CN202211164634 A CN 202211164634A CN 115787120 A CN115787120 A CN 115787120A
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- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims abstract description 27
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- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 claims description 18
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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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Abstract
The application discloses a protein modified lyocell fiber and a production method thereof. The production method of the present application comprises the steps of: dissolving phosphorylated soybean protein powder by using 45-55% of N-methylmorpholine-N-oxide aqueous solution to obtain phosphorylated soybean protein solution; the mass ratio of the phosphorylated soybean protein powder to the N-methylmorpholine-N-oxide is 5 to 9 percent; adding the phosphorylated soybean protein solution into a lyocell fiber raw material spinning solution to obtain a spinning stock solution; and (3) sequentially carrying out spinning, washing, oiling, curling, drying and cutting on the spinning stock solution to obtain the protein modified lyocell fiber. Compared with the conventional lyocell fiber, the protein modified lyocell fiber prepared by the method has better antibacterial property and mechanical property.
Description
Technical Field
The application belongs to the technical field of preparation of lyocell fibers, and particularly relates to a protein modified lyocell fiber and a production method thereof.
Background
Lyocell is a novel man-made fiber, the main component of which is cellulose fiber; it has excellent mechanical property and has the advantages of other fibers, such as: comfort of cotton fibers, soft hand feeling of real silk, elegant luster of silk and the like; it is widely applied in the field of various textiles and belongs to high-grade textile fibers.
The natural antibacterial property, the moisture absorption and the air permeability of the natural plant fiber are incomparable with those of the artificial synthetic fiber, and the modification of the fiber by adding the natural plant fiber or the natural plant protein powder into the artificial synthetic fiber is a mainstream research direction at present. For example, CN201911272098.5 discloses a preparation method of a skin-care antibacterial cotton-flax fabric, which comprises the following steps: preparing raw materials: the antibacterial fabric is prepared from cotton-flax fibers, aloe fibers, bamboo charcoal fibers, soybean protein fibers, silver fibers, acrylic fibers and an antibacterial agent through spinning by a spinning machine to prepare lining, an interlayer and fabric, adding the antibacterial agent for reaction, cleaning with clear water, ironing, drying and sewing. This patent is through adopting natural plant fiber such as aloe fibre, bamboo charcoal fiber, soybean protein fiber, has taken natural antibacterial property and the moisture absorption of natural plant fiber, and air permeability, not only environmental protection has more guaranteed whole surface fabric's gas permeability, travelling comfort simultaneously.
If a protein-modified lyocell fiber can be prepared by adding a vegetable protein to a lyocell fiber, the comfort of wearing, skin-friendliness, antibacterial properties, and the like of the lyocell fiber can be further improved. However, due to the particularity of the lyocell fiber preparation system, at present, there is no report on the direct addition of vegetable protein powder to the lyocell fiber preparation system to prepare protein-modified lyocell fibers.
Disclosure of Invention
The application aims to overcome the defects of the prior art and provide the protein modified lyocell fiber and the production method thereof.
In order to achieve the above object, according to a first aspect of the present application, there is provided a method for producing protein-modified lyocell fiber, comprising the steps of:
dissolving phosphorylated soybean protein powder by using 45-55% of N-methylmorpholine-N-oxide aqueous solution to obtain phosphorylated soybean protein solution; the mass ratio of the phosphorylated soybean protein powder to the N-methylmorpholine-N-oxide is 5-9%;
adding the phosphorylated soybean protein solution into a lyocell fiber raw material spinning solution to obtain a spinning stock solution;
and sequentially carrying out spinning, washing, oiling, curling, drying and cutting on the spinning stock solution to obtain the protein modified lyocell fiber.
Further, the phosphorylated soybean protein powder is prepared by the following method:
adding sodium trimetaphosphate into the alkaline soy protein isolate solution, and reacting for 2-4 h at 40-50 ℃; and after the reaction is finished, adjusting the pH value of the reaction solution to be acidic to terminate the reaction, and separating and removing impurities from the product to obtain the phosphorylated soybean protein powder.
Further, the preparation of the phosphorylated soy protein solution is carried out in a swelling-dissolving apparatus comprising:
the stirring swelling tank is internally provided with a first stirring paddle; the stirring swelling tank is provided with a first heating part;
the stirring and dissolving tank is internally provided with a second stirring paddle; the stirring and dissolving tank is provided with a second heating part; the stirring dissolving tank is communicated with the stirring swelling tank through a first discharge pipeline; and
the balance storage tank is internally provided with a third stirring paddle; the balance storage tank is provided with a third heating part; the balance storage tank is communicated with the stirring and dissolving tank through a second discharge pipeline; a third discharge pipeline of the balance storage tank is communicated with the lyocell spinning solution, and a delivery pump is arranged on the third discharge pipeline;
the preparation process of the phosphorylated soybean protein solution comprises the following steps:
adding the N-methylmorpholine-N-oxide aqueous solution into the stirring swelling tank, heating to 40-50 ℃, adding the phosphorylated soybean protein powder, and stirring for swelling for 1.5-2.5 h;
transferring the swelled mixture into the stirring and dissolving tank, heating to 90-100 ℃, and stirring and dissolving for 1.5-2.5 h to obtain a uniform phosphorylated soybean protein solution;
and transferring the phosphorylated soybean protein solution into the equilibrium storage tank, keeping the temperature at 80-100 ℃, and conveying the phosphorylated soybean protein solution into the lyocell fiber raw material spinning solution through the equilibrium storage tank.
Further, the swelling-dissolving device also comprises a first circulating pipeline, one end of the first circulating pipeline is communicated with the first discharging pipeline, and the other end of the first circulating pipeline is communicated with the stirring swelling tank; and a first circulating pump is arranged on the first circulating pipeline.
Further, the swelling-dissolving device also comprises a second circulating pipeline, one end of the second circulating pipeline is communicated with the second discharging pipeline, and the other end of the second circulating pipeline is communicated with the stirring and dissolving tank; and a second circulating pump is arranged on the second circulating pipeline.
Further, the spinning solution contains wood pulp powder, 88-89% by mass of N-methylmorpholine-N-oxide aqueous solution, the phosphorylated soybean protein solution and propyl gallate.
Further, in the spinning solution, the solid content of the wood pulp powder is 8-12%, and the addition amount of the propyl gallate is 0.1-1 per mill of the mass of the wood pulp powder.
Further, the spinning process is as follows: and adding the spinning solution into a screw extruder, further dissolving at 95-110 ℃, filtering, and then feeding into a spinning system.
Further, the temperature of the water washing is 70-75 ℃, and the time is 2-3 minutes; the temperature of the oiling is 50-55 ℃, and the time is 3-5 seconds.
In a second aspect of the present application, there is provided a protein-modified lyocell fiber produced by the production method described in any one of the above.
Compared with the prior art, the method has the following technical effects:
compared with the original lyocell fiber, the phosphorylated soybean protein modified lyocell fiber has better wearing comfort, skin-friendly property, antibacterial property and the like. And through detection, the mechanical property of the phosphorylated soybean protein modified lyocell fiber is hardly influenced, the bacteriostasis rate to staphylococcus aureus reaches more than 99%, the bacteriostasis rate to escherichia coli reaches more than 90%, and the bacteriostasis rate to candida albicans reaches more than 94%.
Drawings
In order to more clearly illustrate the detailed description of the present application or the technical solutions in the prior art, the drawings needed to be used in the detailed description of the present application or the prior art description will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of a swelling-dissolving apparatus provided in an embodiment of the present application.
Wherein, in the figures, the various reference numbers:
1. stirring dissolving and swelling groove, 2, first stirring slurry, 3, first heating part, 4, stirring dissolving groove, 5, second stirring slurry, 6, second heating part, 7, first discharge pipeline, 8, balance storage tank, 9, third stirring slurry, 10, third heating part, 11, second discharge pipeline, 12, third discharge pipeline, 13, delivery pump, 14, first circulation pipeline, 15, first circulation pump, 16, second circulation pipeline, 17, second circulation pump, 18, first sewage discharge pipeline, 19, second sewage discharge pipeline, 20, third sewage discharge pipeline, 21, sampling pipeline.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of and not restrictive on the broad application.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In this application, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (one) of a, b, or c," or "at least one (one) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, and c may be single or plural, respectively.
It should be understood that, in various embodiments of the present application, the sequence numbers of the above-mentioned processes do not mean the execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weight of the related components mentioned in the description of the embodiments of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present application as long as it is scaled up or down according to the description of the embodiments of the present application. Specifically, the mass described in the specification of the embodiments of the present application may be a mass unit known in the chemical industry field such as μ g, mg, g, kg, etc.
The terms "first" and "second" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another, and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
In a first aspect, the embodiments of the present application provide a method for producing protein-modified lyocell fibers, including the following steps:
(1) Dissolving phosphorylated soybean protein powder by using 45-55% of N-methylmorpholine-N-oxide (NMMO) aqueous solution to obtain phosphorylated soybean protein solution; the mass ratio of the phosphorylated soybean protein powder to the N-methylmorpholine-N-oxide is 5 to 9 percent;
(2) Adding the phosphorylated soybean protein solution into a lyocell fiber raw material spinning solution, and carrying out reduced pressure concentration to obtain a spinning stock solution;
(3) And (3) spinning, washing, oiling, curling, drying and cutting the spinning solution in sequence to obtain the protein modified lyocell fiber.
In the step (1), the phosphorylated soybean protein powder is used for modifying the lyocell fiber, and due to the poor compatibility between the conventional soybean protein powder and a lyocell fiber raw material spinning solution, the problems that the uniform dispersion is difficult and the mutual binding force between the conventional soybean protein powder and the lyocell fiber raw material spinning solution is weak exist, so that the finally prepared protein modified lyocell fiber has poor antibacterial property, mechanical property and the like. Therefore, the phosphorylated soybean protein powder is adopted to replace the conventional soybean protein powder, and after phosphorylation treatment, the molecular structure of the soybean protein powder contains more active groups, so that the phosphorylated soybean protein powder is favorable for dissolving in N-methylmorpholine-N-oxide (NMMO) aqueous solution on one hand, and can be prepared into uniform protein solution more quickly; on the other hand, the method is favorable for generating stronger chemical bonding force between the protein modified lyocell and lyocell fiber spinning raw materials, so that the antibacterial property, the mechanical property and the like of the finally prepared protein modified lyocell fiber are improved.
In the present examples, phosphorylated soy protein powder may be prepared by the following method:
adding Sodium Trimetaphosphate (STMP) into the alkaline soy protein isolate solution, and reacting for 2-4 h at 40-50 ℃; and after the reaction is finished, adjusting the pH value of the reaction solution to be acidic to terminate the reaction, and separating and removing impurities from the product to obtain the phosphorylated soybean protein powder.
Specifically, a 4% SPI (soy protein isolate) solution was prepared, the pH was adjusted to 11.50, STMP was added in a mass ratio of STMP (sodium trimetaphosphate): SPI =100 (g: kg), and the mixture was stirred in a water bath at 45 ℃ for 3 hours. After the reaction, the pH of the protein solution was adjusted to 3.80 with 2mol/L HCl to terminate the phosphorylation reaction. Cooling to room temperature, centrifuging at 10000r/min for 5min, removing supernatant of phosphorylated protein solution, washing precipitate with water twice, adjusting pH to 7, dialyzing at 4 deg.C for 24 hr, and removing excessive STMP and its sodium salt. And freeze-drying for 24h to obtain the phosphorylated soybean protein powder.
In addition, in the embodiment of the application, the process of preparing the phosphorylated soybean protein powder into the uniform phosphorylated soybean protein solution with stable quality is also very critical, the quality stability of the phosphorylated soybean protein solution affects the quality stability of the finally prepared protein-modified lyocell fiber, and if the quality stability of the phosphorylated soybean protein solution is not ensured, the mechanical property of the finally prepared protein-modified lyocell fiber may be poor.
The swelling-dissolving process of the conventional protein powder is usually carried out in only one heating type stirring reaction kettle, and because the swelling and dissolving processes of the protein powder need to control different temperatures, the swelling and dissolving processes of the protein powder cannot be accurately controlled by adopting a mode of operating the heating stirring kettle, so that the quality of the prepared protein powder solution is unstable, and the mechanical property of the finally prepared protein modified lyocell fiber is influenced.
In order to overcome the defects of the conventional operation, the preparation of the phosphorylated soybean protein solution of the embodiment of the present application is performed in a swelling-dissolving device, the structure diagram of which is shown in fig. 1, and the swelling-dissolving device comprises a stirring-swelling tank 1, a stirring-dissolving tank 4 and a balance storage tank 8, wherein a first stirring paddle 2 is arranged in the stirring-swelling tank 1; the stirring swelling tank 1 is provided with a first heating part 3. A second stirring paddle 5 is arranged in the stirring and dissolving tank 4; the stirring and dissolving tank 4 is provided with a second heating part 6; the stirring and dissolving tank 4 is communicated with the stirring and dissolving tank 1 through a first discharge pipeline 7. A third stirring paddle 9 is arranged in the balance storage tank 8; the balance storage tank 8 is provided with a third heating component 10; the balance storage tank 8 is communicated with the stirring and dissolving tank 4 through a second discharge pipeline 11; a third discharge pipeline 12 of the balance storage tank 8 is communicated with the lyocell spinning solution, and a delivery pump 13 is arranged on the third discharge pipeline 12.
The preparation process of the phosphorylated soybean protein solution comprises the following steps:
firstly, adding 45-55 mass percent of N-methylmorpholine-N-oxide aqueous solution into a stirring swelling tank 1, heating the N-methylmorpholine-N-oxide aqueous solution to 40-50 ℃ through a first heating part 3, adding phosphorylated soybean protein powder, starting a first stirring paddle 2 for stirring, and stirring and swelling for 1.5-2.5 hours until the protein powder is in a uniform porridge shape.
And then transferring the swelled mixture into a stirring and dissolving tank 4, heating the swelled mixture to 90-100 ℃ by a second heating part 6, starting a second stirring paddle 5, and stirring and dissolving for 1.5-2.5 hours to obtain a uniform yellow phosphorylated soybean protein solution.
And finally, transferring the phosphorylated soybean protein solution into an equilibrium storage tank 8, keeping the temperature of the phosphorylated soybean protein solution at 80-100 ℃ by a third heating part 10, starting a third stirring paddle 9, and conveying the phosphorylated soybean protein solution into the lyocell fiber raw material spinning solution through the equilibrium storage tank 8.
The embodiment of this application adopts the swelling-dissolving device with the swelling of albumen powder, the dissolving process goes on respectively in stirring swelling groove 1 and 4 reactors of stirring dissolving tank, first heater block 3 and second heater block 6 through stirring swelling groove 1 and on the stirring dissolving tank 4 heat the accuse temperature respectively alone, can realize the albumen powder swelling, the accurate control of dissolving process, do benefit to the stability of quality that improves the albumen powder solution of preparing, and then can improve the mechanical properties of the modified lyocell of the albumen of final preparation.
The protein powder swelling and dissolving device provided by the embodiment of the application further comprises a first circulating pipeline 14, one end of the first circulating pipeline 14 is communicated with the first discharging pipeline 7, and the other end of the first circulating pipeline 14 is communicated with the stirring and swelling tank 1; a first circulation pump 15 is provided on the first circulation line 14. When the protein powder is subjected to swelling treatment, the first circulating pipeline 14 and the first circulating pump 15 are additionally arranged, so that the protein powder is ceaselessly swelled in the stirring swelling tank 1 through self-circulation, and the swelling process is promoted.
The protein powder swelling and dissolving device provided by the embodiment of the application further comprises a second circulating pipeline 16, one end of the second circulating pipeline 16 is communicated with the second discharging pipeline 11, and the other end of the second circulating pipeline 16 is communicated with the stirring and dissolving tank 4; a second circulation pump 17 is provided on the second circulation line 16. When carrying out dissolving treatment to albumen powder, through addding second circulation pipeline 16 and second circulating pump 17, can make albumen powder dissolve in stirring dissolving tank 4 ceaselessly through the self-loopa, promote going on of dissolving process.
In the embodiment of the present application, the first heating member 3, the second heating member 6, and the third heating member 10 are all steam coil heaters, and the purpose of heating is achieved by introducing high-temperature steam into the steam coil heaters. In one embodiment of the present application, the first stirring paddle 2, the second stirring paddle 5 and the third stirring paddle 9 are all driven by a motor.
In the embodiment of the application, the stirring swelling tank 1 is also connected with a first sewage discharge pipeline 18, and the first sewage discharge pipeline 18 can discharge the cleaning sewage in the production process.
In the embodiment of the application, a second sewage draining pipeline 19 is further connected to the stirring and dissolving tank 4, and the cleaning sewage in the production process can be discharged through the second sewage draining pipeline 19.
In the embodiment of the present application, a third sewage line 20 is further connected to the equalizing storage tank 8, and the cleaning sewage in the production process can be discharged through the third sewage line 20.
In this application embodiment, the third discharging pipeline 12 is further connected with a sampling pipeline 21, and a small amount of sampling analysis can be performed on the swollen and dissolved protein powder solution through the sampling pipeline 21, so as to determine whether the quality of the prepared protein powder solution is qualified.
In the step (2), in the present embodiment, the spinning solution contains wood pulp powder, an aqueous solution of N-methylmorpholine-N-oxide with a mass fraction of 88 to 89%, a phosphorylated soy protein solution, and propyl gallate. Furthermore, in the spinning solution, the solid content of the wood pulp powder is 8-12%, and the addition amount of the propyl gallate is 0.1-1 per mill of the mass of the wood pulp powder.
In the step (3), in the embodiment of the present application, the spinning process is as follows: adding the spinning solution into a screw extruder, further dissolving at 95-110 ℃, filtering and then entering a spinning system. Further, the temperature of washing is 70-75 ℃, and the time is 2-3 minutes; the temperature of oiling is 50-55 ℃, and the time is 3-5 seconds.
In a second aspect of the embodiments of the present application, there is provided a protein-modified lyocell fiber, which is produced by the above-described production method.
Hereinafter, a protein-modified lyocell fiber and a method for producing the same according to examples of the present application will be described with reference to specific examples.
Example 1
The embodiment 1 of the application provides a protein modified lyocell fiber and a production method thereof, and the production method comprises the following steps:
(1) Dissolving phosphorylated soybean protein powder by using a swelling-dissolving device shown in fig. 1, and dissolving phosphorylated soybean protein powder by using a 50% by mass aqueous solution of N-methylmorpholine-N-oxide (NMMO) to obtain a phosphorylated soybean protein solution; the mass ratio of the phosphorylated soybean protein powder to the N-methylmorpholine-N-oxide is 5%. Controlling the temperature in the stirring swelling tank 1 at 45 ℃, and stirring for swelling for 1.5-2.5 h until the protein powder is in a uniform porridge shape. Controlling the temperature in the stirring and dissolving tank 4 to be 95 ℃, and stirring and dissolving for 1.5-2.5 h to obtain a uniform yellow phosphorylated soybean protein solution. The temperature in the equilibrium storage tank 8 is controlled to be 80-100 ℃.
(2) Adding the phosphorylated soybean protein solution into a lyocell fiber raw material spinning solution to obtain a spinning stock solution; in the spinning solution, the solid content of the wood pulp powder is 10%, and the addition amount of the propyl gallate is 0.3 per mill of the mass of the wood pulp powder.
(3) Adding the spinning solution into a screw extruder, further dissolving at 95 ℃, filtering and then entering a spinning system. Wherein, the length of the air gap is 8cm, the spinning speed is 40m/min, the aperture of the spinneret plate is 95um, the length of the capillary tube is 500um, the sprayed silk is vertically stretched in the air and enters a coagulating bath for forming; then soaking the glass fiber cloth into hot water at the temperature of 75 ℃ for washing for 2 minutes; then, the steel sheet was immersed in an oil bath at a temperature of 55 ℃ for oiling for 3 seconds. Finally, the protein modified lyocell fiber is prepared by curling, drying and cutting.
Example 2
The embodiment 2 of the application provides a protein modified lyocell fiber and a production method thereof, and the production method comprises the following steps:
(1) Dissolving phosphorylated soybean protein powder by using a swelling-dissolving device shown in fig. 1, and dissolving phosphorylated soybean protein powder by using 45 mass percent of N-methylmorpholine-N-oxide (NMMO) aqueous solution to obtain phosphorylated soybean protein solution; the mass ratio of the phosphorylated soybean protein powder to the N-methylmorpholine-N-oxide is 8%. Controlling the temperature in the stirring swelling tank 1 at 40 ℃, and stirring for swelling for 1.5-2.5 h until the protein powder is in a uniform porridge shape. Controlling the temperature in the stirring and dissolving tank 4 to be 90 ℃, and stirring and dissolving for 1.5-2.5 h to obtain a uniform yellow phosphorylated soybean protein solution. The temperature in the equilibrium storage tank 8 is controlled to be 80-100 ℃.
(2) Adding the phosphorylated soybean protein solution into a lyocell fiber raw material spinning solution to obtain a spinning solution; in the spinning solution, the solid content of the wood pulp powder is 8%, and the addition amount of the propyl gallate is 0.6 per mill of the mass of the wood pulp powder.
(3) Adding the spinning solution into a screw extruder, further dissolving at 100 ℃, and filtering to enter a spinning system. Wherein, the length of the air gap is 8cm, the spinning speed is 40m/min, the aperture of the spinneret plate is 95um, the length of the capillary tube is 500um, the sprayed silk is vertically stretched in the air and enters a coagulating bath for forming; then soaking the glass substrate into hot water at the temperature of 75 ℃ for washing for 2 minutes; then, the steel sheet was immersed in an oil bath at a temperature of 55 ℃ for oiling for 3 seconds. And finally, curling, drying and cutting to obtain the protein modified lyocell fiber.
Example 3
The application embodiment 3 provides a protein modified lyocell fiber and a production method thereof, and the production method comprises the following steps:
(1) Dissolving phosphorylated soybean protein powder by using a swelling-dissolving device shown in fig. 1, and dissolving phosphorylated soybean protein powder by using 50 mass percent of N-methylmorpholine-N-oxide (NMMO) aqueous solution to obtain a phosphorylated soybean protein solution; the mass ratio of the phosphorylated soybean protein powder to the N-methylmorpholine-N-oxide was 9%. Controlling the temperature in the stirring swelling tank 1 at 50 ℃, and stirring for swelling for 1.5-2.5 h until the protein powder is in a uniform porridge shape. Controlling the temperature in the stirring and dissolving tank 4 to be 100 ℃, and stirring and dissolving for 1.5-2.5 h to obtain a uniform yellow phosphorylated soybean protein solution. The temperature in the equilibrium storage tank 8 is controlled to be 80-100 ℃.
(2) Adding the phosphorylated soybean protein solution into a lyocell fiber raw material spinning solution to obtain a spinning stock solution; in the spinning solution, the solid content of the wood pulp powder is 12%, and the addition amount of the propyl gallate is 0.9 per mill of the mass of the wood pulp powder.
(3) Adding the spinning solution into a screw extruder, further dissolving at 110 ℃, and filtering to enter a spinning system. Wherein the length of the air gap is 8cm, the spinning speed is 40m/min, the aperture of a spinneret plate is 95um, the length of a pore capillary is 500um, and the sprayed silk is vertically stretched in the air and enters a coagulating bath for forming; then soaking the glass substrate into hot water at the temperature of 75 ℃ for washing for 2 minutes; then, the steel sheet was immersed in an oil bath at a temperature of 55 ℃ for oiling for 3 seconds. Finally, the protein modified lyocell fiber is prepared by curling, drying and cutting.
Comparative example 1
The difference from the example 1 is that in the step (1), a conventional heating type stirring reaction kettle is adopted to carry out swelling and dissolving operation on the phosphorylated protein powder, the temperature in the reaction kettle is controlled to be 40 ℃ in the swelling stage, the temperature is increased to 90 ℃ after the stirring and swelling for 2 hours, and the stirring and dissolving are carried out for 2 hours to obtain the dissolved phosphorylated soybean protein solution. The other process operations were the same as in example 1.
Comparative example 2
It is different from example 1 in that a conventional lyocell fiber was prepared without adding a phosphorylated soy protein solution in step (2). The other process operations were the same as in example 1.
The antibacterial property and the mechanical property of the lyocell fibers prepared in the embodiments 1-3 and the comparative examples 1-2 of the application are tested, the mechanical property test method refers to GB/T-24218.3-2010, a FAVIMAT-BOBOBOT 2 full-automatic single fiber universal tester is adopted for testing, no less than 30 test samples are taken, and the test average value is taken. The test results are shown in the following table.
As seen from the above table, the protein-modified lyocell fibers prepared in the examples of the present application have slightly reduced mechanical properties, but significantly improved antibacterial properties, compared to conventional lyocell fibers. And the comparison of example 1 with comparative example 1 shows that the protein modified lyocell fiber prepared by the production method of the embodiment of the present application has better mechanical properties.
The above examples only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A production method of protein modified lyocell fiber is characterized by comprising the following steps:
dissolving phosphorylated soybean protein powder by using 45-55% of N-methylmorpholine-N-oxide aqueous solution to obtain phosphorylated soybean protein solution; the mass ratio of the phosphorylated soybean protein powder to the N-methylmorpholine-N-oxide is 5-9%;
adding the phosphorylated soybean protein solution into a lyocell fiber raw material spinning solution to obtain a spinning stock solution;
and sequentially spinning, washing, oiling, curling, drying and cutting the spinning solution to obtain the protein modified lyocell fiber.
2. The method for producing protein-modified lyocell fiber according to claim 1, wherein said phosphorylated soy protein powder is prepared by the following method:
adding sodium trimetaphosphate into the alkaline soy protein isolate solution, and reacting for 2-4 h at the temperature of 40-50 ℃; and after the reaction is finished, adjusting the pH value of the reaction solution to be acidic to terminate the reaction, and separating and removing impurities from the product to obtain the phosphorylated soybean protein powder.
3. The method of claim 1, wherein the preparation of the phosphorylated soy protein solution is performed in a swelling-dissolving apparatus comprising:
the stirring swelling tank is internally provided with a first stirring paddle; the stirring swelling tank is provided with a first heating part;
the stirring and dissolving tank is internally provided with a second stirring paddle; the stirring and dissolving tank is provided with a second heating part; the stirring and dissolving tank is communicated with the stirring and swelling tank through a first discharge pipeline; and
the balance storage tank is internally provided with a third stirring paddle; the balance storage tank is provided with a third heating part; the balance storage tank is communicated with the stirring and dissolving tank through a second discharge pipeline; a third discharge pipeline of the balance storage tank is communicated with the lyocell spinning solution, and a delivery pump is arranged on the third discharge pipeline;
the preparation process of the phosphorylated soybean protein solution comprises the following steps:
adding the N-methylmorpholine-N-oxide aqueous solution into the stirring swelling tank, heating to 40-50 ℃, adding the phosphorylated soybean protein powder, and stirring for swelling for 1.5-2.5 h;
transferring the swelled mixture into the stirring and dissolving tank, heating to 90-100 ℃, and stirring and dissolving for 1.5-2.5 h to obtain a uniform phosphorylated soybean protein solution;
and transferring the phosphorylated soybean protein solution into the equilibrium storage tank, keeping the temperature at 80-100 ℃, and conveying the phosphorylated soybean protein solution into the lyocell fiber raw material spinning solution through the equilibrium storage tank.
4. The process for producing protein-modified lyocell fiber according to claim 3, wherein said swelling-dissolving means further comprises a first circulation line, one end of said first circulation line being in communication with said first discharge line, and the other end of said first circulation line being in communication with said agitation swelling tank; and a first circulating pump is arranged on the first circulating pipeline.
5. The process for producing protein-modified lyocell fiber according to claim 3, wherein said swelling-dissolving means further comprises a second circulation line, one end of said second circulation line being in communication with said second discharge line, and the other end of said second circulation line being in communication with said agitation and dissolution tank; and a second circulating pump is arranged on the second circulating pipeline.
6. The process for producing protein-modified lyocell fiber according to any one of claims 1 to 5, wherein said spinning dope comprises wood pulp powder, an aqueous solution of N-methylmorpholine-N-oxide in an amount of 88 to 89% by mass, said phosphorylated soybean protein solution and propyl gallate.
7. The method for producing protein-modified lyocell fiber according to claim 6, wherein the solid content of the wood pulp powder in the spinning dope is 8 to 12%, and the addition amount of propyl gallate is 0.1 to 1% by mass of the wood pulp powder.
8. The method of producing protein-modified lyocell fiber according to claim 1, wherein said spinning process comprises: and adding the spinning solution into a screw extruder, further dissolving at 95-110 ℃, and filtering to enter a spinning system.
9. The method for producing protein-modified lyocell fiber according to claim 1, wherein the washing temperature is 70 to 75 ℃ and the time is 2 to 3 minutes; the temperature of the oiling is 50-55 ℃, and the time is 3-5 seconds.
10. A protein-modified lyocell fiber produced by the production method according to any one of claims 1 to 9.
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| CN116254700A (en) * | 2023-05-10 | 2023-06-13 | 潍坊维尼新材料有限公司 | Multifunctional protein modified lyocell fiber and preparation method thereof |
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