Preparation method of chemical fiber containing silk protein

Abstract

The invention discloses a preparation method of a chemical fiber containing silk protein, and relates to the technical field of fiber preparation, and the preparation method comprises the following steps: firstly, pretreating and modifying a silk protein raw material, and grinding through an ultralow-temperature sectional ball mill to obtain silk protein powder; mixing the silk protein powder with spinning lubricating oil to form a stable silk protein spinning lubricating oil mixed solution; the preparation method comprises the following steps: melting a base material, adding a fibroin spinning lubricating oil mixed solution, and granulating through an extrusion granulator to obtain a master batch containing fibroin powder; melting the base material, adding the master batch containing the silk protein powder, and then spinning to finally obtain the chemical fiber containing the silk protein, according to the preparation method of the chemical fiber containing the silk protein, the silk protein material is implanted into the fiber to ensure that the silk protein stably and lastingly exists in the fiber, so that the durability of the fabric is enhanced, the attractiveness of the fabric is improved, and the concepts of environmental protection and sustainable development are met.

Description

Technical Field

[0001] The invention relates to a fiber preparation technology, and in particular to a method for preparing chemical fiber containing silk protein. Background Art

[0002] Chemical fiber, also known as chemical fiber, is a fiber with textile properties made from natural polymer compounds or artificially synthesized polymer compounds through processes such as preparation of spinning solution, spinning and post-treatment. In the field of research and development and innovation of textile materials, silk protein, as a natural polymer material, has shown great application potential in fiber manufacturing due to its excellent biocompatibility, biodegradability and unique physiological functions. As a natural polymer material, silk protein can not only give the fiber excellent biological affinity and environmental friendliness, but also bring excellent mechanical properties and physiological regulation functions to the fiber through its unique three-dimensional structure, which makes silk protein fiber an important force in promoting the innovative development of textile materials.

[0003] However, commercially available silk protein powders usually have a large particle size, which not only limits its application in the field of fine processing, but also, in the spinning process, coarse powder particles easily clog the spinneret, resulting in an unstable spinning process and uneven product quality. In addition, although traditional grinding technology can reduce the particle size, it is often accompanied by the risk of silk protein structure destruction and reduced biological activity, which limits the application of silk protein in high-end fiber manufacturing.

[0004] Therefore, developing a new technology that can efficiently prepare nano-scale, structurally intact, and biologically active silk protein powder has become the key to improving the quality of silk protein fibers and broadening their application areas. At the same time, how to effectively and evenly introduce nano-scale silk protein powder into the spinning process to avoid clogging the spinneret and ensure smooth spinning is also a technical challenge currently faced. Summary of the invention

[0005] The object of the present invention is to provide a method for preparing chemical fiber containing silk protein to solve the above-mentioned shortcomings in the prior art.

[0006] In order to achieve the above object, the present invention provides the following technical solution: a method for preparing chemical fiber containing silk protein, comprising the following steps:

[0007] S1. First, high-quality silk protein raw materials are selected, and after pretreatment and modification, they are ground in an ultra-low temperature segmented ball mill to obtain nano-scale silk protein powder;

[0008] S2, mixing the ground nano-scale silk protein powder with spinning lubricant in a ratio of 1:1, and using high-speed shearing or ultrasonic dispersion technology to form a stable silk protein spinning lubricant mixture;

[0009] S3, melting the substrate at 150° C., then adding the silk protein spinning lubricant mixture, and granulating through an extrusion granulator to obtain a masterbatch containing silk protein powder;

[0010] S4. Under the condition of 200° C., the substrate is melted, and master batches containing silk protein powder are added to the molten substrate, and then spinning is performed through a spinning machine to finally obtain chemical fiber containing silk protein.

[0011] Furthermore, the pretreatment in S1 includes the following steps: adding a silk protein modifier to a silk protein solution, stirring evenly to allow the modifier to react completely with the silk protein, and then washing, dehydrating and drying the silk protein solution to obtain a modified silk protein raw material.

[0012] Furthermore, the grinding temperature of the ultra-low temperature segmented ball mill described in S1 is -100°C to -196°C.

[0013] Furthermore, the spinning lubricant described in S2 is at least one of silicone oil, mineral oil or vegetable oil.

[0014] Furthermore, the addition ratio of the substrate and the silk protein spinning lubricant mixture in S3 is 5:1 to 20:1.

[0015] Furthermore, the substrate in S3 and S4 is polyamide, polyethylene, polypropylene or polyethylene terephthalate.

[0016] Furthermore, the screw speed of the extrusion granulator in S3 is 30-100 rpm, and the temperature of the extrusion granulator is 140°C-160°C.

[0017] Furthermore, the spinning speed of S4 is 1000-5000 m / min, and the spinning tension is 5-30 cN.

[0018] Furthermore, the spinning in S4 also includes stretching and shaping the spun fibers to fix the shape and size of the fibers.

[0019] Furthermore, the content of silk protein in the chemical fiber containing silk protein described in S4 is 1%-30% of the total mass of the fiber.

[0020] Compared with the prior art, the method for preparing chemical fiber containing silk protein provided by the present invention ensures the stable and lasting existence of silk protein inside the fiber by implanting silk protein material into the fiber; the addition of silk protein not only improves the biocompatibility of the fabric, but also enhances the binding force between fibers through its unique molecular structure, making the fabric more wear-resistant and tear-resistant, and extending the service life of the fabric; the nourishing ingredients continuously released by silk protein help promote the regeneration and repair of skin cells, reduce signs of skin aging, such as fine lines and sagging, and keep the skin young; the silk protein fiber fabric can be intelligently adjusted according to the ambient humidity and human body temperature, absorb excess heat and quickly evaporate sweat in summer to keep cool; lock in warmth in winter, reduce heat loss, and maintain a moderate humidity balance to improve wearing comfort; the addition of silk protein can also give the fabric a more natural luster and delicate feel, making the fabric more advanced visually and more skin-friendly to the touch; and the use of chemical substances is reduced in the preparation process, which is in line with the concepts of environmental protection and sustainable development, and meets the pursuit of green products by modern consumers. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0022] Figure 1 A flow chart of the overall preparation method provided by an embodiment of the present invention. DETAILED DESCRIPTION

[0023] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

[0024] Embodiment 1:

[0025] See also Figure 1 A method for preparing a chemical fiber containing silk protein comprises the following steps:

[0026] S1. First, high-quality silk protein raw materials are selected, and after pretreatment and modification, they are ground in an ultra-low temperature segmented ball mill to obtain nano-scale silk protein powder;

[0027] First, carefully select high-quality silk protein raw materials, add silk protein modifiers to the silk protein solution, stir evenly, make the modifier and silk protein react completely, then wash, dehydrate and dry the silk protein solution to obtain modified silk protein raw materials. Through modification, some physical and chemical properties of silk protein can be significantly improved, such as wear resistance, wrinkle resistance, elasticity, etc., making the products made from it more durable and easy to care for, improving the hydrophilicity of silk protein, making it have better hygroscopicity and air permeability, and the stability of the modified silk protein under environmental factors such as light, temperature, and humidity may be enhanced, which helps to extend its service life and maintain stable performance; during the modification process of silk protein, its molecular segments will be affected by the modifier, making the originally tightly stacked molecular segments become relatively loose. This structural change enhances the mobility of the molecular segments during the grinding process, making it easier to be ground into fine particles.

[0028] Subsequently, the modified silk protein raw materials are ground using an advanced ultra-low temperature segmented ball mill. In an ultra-low temperature environment of -100°C to -196°C, the ball mill gradually refines the silk protein raw materials to the nano level through a segmented grinding process.

[0029] This step not only ensures the fineness and uniformity of the silk protein powder, but also effectively avoids the thermal denaturation that may occur during the grinding process, thereby retaining the natural biological activity of silk protein. In a low-temperature environment, the molecular chain of silk protein is easier to maintain its original orderly arrangement and conformation, thereby ensuring that the nano-scale silk protein powder obtained after grinding can retain its original biocompatibility, degradability and biological activity to the greatest extent. The interaction force between silk protein molecules is weakened, which is conducive to reducing the occurrence of agglomeration. The ultra-low temperature segmented ball mill has an ultra-high rotation speed and gravity acceleration, making the grinding process faster and more efficient. Through ball milling, the silk protein raw material can be refined into nano-scale powder to achieve uniform and consistent particle distribution. This uniformity is not only conducive to subsequent processing and application, but also can improve the stability and performance of the product. The ultra-low temperature segmented ball mill adopts a closed structure during the grinding process, which effectively avoids the contamination of external impurities and microorganisms. The low temperature environment also helps to inhibit the growth and reproduction of microorganisms, thereby ensuring the quality and safety of the product.

[0030] S2, mixing the ground nano-scale silk protein powder with spinning lubricant in a ratio of 1:1, and using high-speed shearing or ultrasonic dispersion technology to form a stable silk protein spinning lubricant mixture;

[0031] Silicone oil is used as the spinning lubricant. The ground nano-scale silk protein powder is mixed with the selected spinning lubricant. The silicone oil helps to evenly distribute the silk protein powder during the spinning process.

[0032] Silicone oil can reduce the friction coefficient between fibers, thereby reducing the adhesion and static electricity on the fiber surface, maintaining the fiber shape, and improving the fiber propulsion speed and spinning efficiency; silicone oil has excellent antistatic properties, which can reduce the static electricity accumulation of fibers during the spinning process, avoid fiber entanglement and stretching, and improve the toughness and ductility of fibers; silicone oil is not easy to evaporate and dry, and can maintain the lubrication effect for a long time, thereby extending the service life of the equipment; silicone oil can be used alone or in combination with other additives to achieve better spinning effects.

[0033] During mixing, high-speed shearing or ultrasonic dispersion technology is used to ensure that the silk protein powder and the spinning lubricant are fully mixed to form a stable silk protein spinning lubricant mixture. This step is crucial for the uniformity and performance of the fiber in the subsequent spinning process.

[0034] S3. Melt the polyamide, polyethylene, polypropylene or polyethylene terephthalate substrate at 150°C, and then add the silk protein spinning lubricant mixture, wherein the addition ratio of the polyamide, polyethylene, polypropylene or polyethylene terephthalate substrate to the silk protein spinning lubricant mixture is 5:1 to 20:1, and granulate by an extrusion granulator to obtain a polyamide, polyethylene, polypropylene or polyethylene terephthalate masterbatch containing silk protein powder; the screw speed of the extrusion granulator is 30-100 rpm, and the temperature is 140°C to 160°C;

[0035] The advantages of using polyamide, polyethylene, polypropylene or polyethylene terephthalate as a substrate are as follows:

[0036] The rebound rate of polyamide fiber is comparable to that of wool, which makes the made textiles have good elasticity and recovery. Polyamide fiber is the most wear-resistant fiber among all textile fibers, 10 times that of cotton, 20 times that of wool, and 50 times that of viscose fiber. Polyamide fiber has high strength. The breaking strength of general textile filament is 4.42-5.65cN / dtex, and the breaking strength of polyamide high-strength yarn for special purposes is even higher. Polyamide fiber has the advantages of general synthetic fibers such as corrosion resistance, insect resistance, and mildew resistance. The hygroscopicity of polyamide fiber is second only to vinylon among synthetic fibers.

[0037] Polyethylene fiber has a high thermal conductivity and can quickly dissipate heat. It is often used as a cooling material. The fabric woven with this fiber material feels silky and has a silk-like effect. The chemical bond structure of polyethylene fiber is stable and has certain hydrophobicity and antibacterial and mildew-proof functions. Mattresses and mats made of polyethylene fiber can increase the indoor air-conditioning temperature by 1 to 2°C in hot summer, saving electricity bills and reducing carbon emissions.

[0038] Polypropylene fiber has high strength and toughness, which makes the textiles made from it have good durability; polypropylene fiber has good resistance to a variety of chemicals and is suitable for a variety of industrial environments; fine-density polypropylene fiber has excellent wicking effect, and has excellent air permeability and moisture conduction properties, and can keep the skin dry and not feel stuffy when worn close to the skin; polypropylene fiber can be used to make a variety of textiles such as underwear, ski jackets, socks and children's clothing, and can also be used for decorative fabrics, felt, canvas, packaging bags, etc.

[0039] Polyethylene terephthalate is a highly crystalline polymer with excellent antibacterial, mechanical and physical properties; polyethylene terephthalate fiber has antibacterial properties and is suitable for textiles that require antibacterial functions; polyethylene terephthalate fiber has excellent mechanical properties, and the textiles made from it have good strength and wear resistance; polyethylene terephthalate fiber has stable physical properties and has good adaptability to various environmental factors; polyethylene terephthalate fiber can be used to make a variety of textiles such as silk-type fabrics, yarn-dyed fabrics, warp knitted fabrics and decorative fabrics, and can also be used in medical fields such as biomedical pads.

[0040] In summary, polyamide, polyethylene, polypropylene and polyethylene terephthalate each have unique benefits and applicable fields as spinning substrates.

[0041] At 150°C, a substrate such as polyamide, polyethylene, polypropylene or polyethylene terephthalate is melt-treated; these substrates have good physical and chemical properties and are ideal for preparing chemical fibers. After melting, a silk protein spinning lubricant mixture is added to the molten substrate at a ratio of 5:1 to 20:1. The mixture is granulated by a precision extrusion granulator at a screw speed of 30-100rpm and an extrusion temperature of 140°C-160°C to obtain polyamide, polyethylene, polypropylene or polyethylene terephthalate masterbatch containing silk protein powder. This step not only achieves the uniform distribution of silk protein powder in the substrate, but also facilitates the subsequent spinning process.

[0042] The screw speed of the extrusion granulator ensures that the polymer material and silk protein mixture can be fully mixed and evenly distributed between the screw and the barrel. A lower speed may be conducive to the mixing and dispersion process, but it may also lead to reduced production efficiency. Therefore, it is necessary to increase the speed as much as possible to improve production efficiency while ensuring the mixing quality, so the screw speed is set in the range of 30-100rpm. The temperature setting ensures that the polymer material can be completely melted and maintain good fluidity. At the same time, the thermal stability of silk protein needs to be considered to avoid denaturation or degradation of silk protein due to excessively high temperatures.

[0043] S4. Under the condition of 200°C, a polyamide, polyethylene, polypropylene or polyethylene terephthalate substrate is melted, and a masterbatch containing silk protein powder corresponding to the substrate is added to the molten substrate, and then spinning is carried out through a spinning machine. The spinning also includes necessary stretching and shaping treatments for the spun fibers to fix the shape and size of the fibers, and finally chemical fiber containing silk protein is obtained. The content of silk protein in the chemical fiber containing silk protein is 1%-30% of the total mass of the fiber; the spinning speed is 1000-5000m / min, and the spinning tension is 5-30cN.

[0044] At 200°C, the polyamide, polyethylene, polypropylene or polyethylene terephthalate substrate is melted again, and then the corresponding substrate masterbatch containing silk protein powder is added to the molten substrate. The mixture is spun by a spinning machine. During the spinning process, the spinning speed and spinning tension are strictly controlled to ensure the uniformity and stability of the fiber. The spinning speed is set to 1000-5000m / min, and the spinning tension is controlled in the range of 5-30cN. The increase in spinning speed means that more fibers can be produced per unit time, thereby significantly improving production efficiency, which is of great significance for large-scale industrial production, helping to reduce production costs and meet market demand; at an appropriate spinning speed, the fiber can be cooled and solidified more evenly, thereby forming a more compact and orderly structure, which helps to improve the mechanical properties and durability of the fiber; the increase in spinning speed helps the orientation of the fiber during the spinning process, so that the molecular chains inside the fiber are arranged more parallel, and this increase in orientation helps to enhance the tensile strength and modulus of the fiber.

[0045] Spinning tension is one of the key factors in controlling fiber morphology. By adjusting the spinning tension, the fiber diameter, cross-sectional shape and surface morphology can be precisely controlled, which helps ensure the uniformity and consistency of the fiber, thereby improving product quality. Appropriate spinning tension helps the fiber to stretch and solidify during the spinning process, making the molecular chains inside the fiber more closely arranged and producing more cross-linking points. This structural change helps to improve the tensile strength and elongation at break of the fiber; spinning tension can also reduce fiber defects during the spinning process, such as bubbles, breakage and entanglement. The presence of these defects will seriously affect the performance and service life of the fiber. By controlling the spinning tension, the incidence of these defects can be significantly reduced, thereby improving the overall quality of the fiber.

[0046] After spinning, the fiber is stretched and shaped as necessary to fix the shape and size of the fiber, while further improving the strength and stability of the fiber. This step is a key step in the preparation of chemical fiber containing silk protein powder, which ensures that the fiber has excellent physical properties and biocompatibility; after stretching and shaping, the fiber density increases, the pores become less, the diameter becomes thinner, the tensile strength increases, the elongation at break decreases, and the electrical conductivity and thermal conductivity are enhanced; at the same time, the appearance and feel of the fiber are also significantly improved, becoming more delicate, soft and smooth; in addition, stretching and shaping treatments also help reduce shrinkage and warping of the fiber, making it smoother and more beautiful.

[0047] Embodiment 2:

[0048] This embodiment provides a technical solution based on the first embodiment: the spinning lubricant oil used in S2 is replaced by a mixture of silicone oil and mineral oil instead of silicone oil.

[0049] The mixture of mineral oil and silicone oil as spinning lubricant combines the advantages of both oils and has many benefits and advantages. The following is a detailed analysis of its benefits:

[0050] Excellent lubrication performance: Both mineral oil and silicone oil have good lubrication performance. Their mixture can significantly reduce the friction coefficient between fibers, making the spinning process smoother; the mixture can keep the fiber surface smooth, reduce fiber breakage and wear, and improve spinning efficiency and product quality.

[0051] Good antistatic performance: Silicone oil has excellent antistatic properties and can effectively reduce the static electricity accumulation of fibers during the spinning process; although mineral oil has relatively weak antistatic properties, it can work synergistically with silicone oil to further enhance the overall antistatic effect.

[0052] High temperature stability: Silicone oil has good stability at high temperatures and is not easy to decompose and produce harmful gases; although the high temperature stability of mineral oil is slightly inferior to that of silicone oil, the mixture can still maintain a good lubrication effect in the high temperature spinning process.

[0053] Anti-rust and anti-wear properties: Mineral oil has good anti-rust properties and can protect metal parts in spinning equipment from corrosion; at the same time, mineral oil also has certain anti-wear properties, which can reduce friction and wear between machine parts.

[0054] Cost-effectiveness: Compared with pure silicone oil, the mixture of mineral oil and silicone oil has lower cost and is more easily accepted by spinning companies; while ensuring the lubrication effect, the mixture can reduce production costs and improve the economic benefits of the company.

[0055] Easy to use and maintain: The mixture of mineral oil and silicone oil is easy to use and can be directly sprayed or applied on the fiber surface; the mixture is easy to control the dosage during the spinning process, and is not easy to evaporate and dry, and can maintain the lubricating effect for a long time.

[0056] Embodiment three:

[0057] This embodiment provides a technical solution based on the first embodiment: the spinning lubricant oil used in S2 is replaced by a mixture of silicone oil and vegetable oil instead of silicone oil.

[0058] The mixture of vegetable oil and silicone oil as spinning lubricant combines the unique properties of the two oils and brings many benefits and advantages. The following is a detailed summary of its benefits:

[0059] Eco-friendly: Vegetable oil comes from natural plants, does not contain toxic and harmful substances, and does not pollute the environment; after mixing with silicone oil, the overall ecological and environmental protection is improved, which helps to reduce the negative impact of the spinning industry on the environment.

[0060] Renewable Resource: Vegetable oil is a renewable resource that is obtained by growing and harvesting plants. This means that using vegetable oil as part of the spinning lubricant helps reduce dependence on limited petroleum resources.

[0061] Excellent lubrication performance: Both vegetable oil and silicone oil have good lubrication performance. The mixture can significantly reduce the friction coefficient between fibers, making the spinning process smoother and improving fiber quality.

[0062] Anti-wear performance: Silicone oil itself has anti-wear properties. After mixing with vegetable oil, it can further enhance the overall anti-wear effect, reduce the wear of machine parts and extend the service life of equipment.

[0063] Temperature stability: Silicone oil has high temperature stability and can maintain good lubrication performance at high temperatures. After mixing with vegetable oil, the overall temperature stability is improved, making it suitable for high-temperature spinning processes.

[0064] Antioxidant property: Although the antioxidant property of vegetable oil is relatively poor, it can be improved by adding antioxidants and mixed with silicone oil to form a complementary effect, thereby improving the overall antioxidant performance and extending the service life of the lubricant.

[0065] Cost-effectiveness: Compared with pure silicone oil, the mixture of vegetable oil and silicone oil is cheaper, which helps to reduce the production costs of spinning companies. At the same time, since vegetable oil is a renewable resource, using a mixture also has sustainability advantages in the long run.

[0066] Easy to obtain and process: Vegetable oils are widely available, easy to obtain and process, and when mixed with silicone oil, they can form a stable and uniform lubricant mixture that is easy to store and use.

[0067] The above description is only by way of illustration of certain exemplary embodiments of the present invention. It is undoubted that those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A method for preparing chemical fiber containing silk protein, characterized in that: The steps include: S1. First, high-quality silk protein raw materials are selected, and after pretreatment and modification, they are ground in an ultra-low temperature segmented ball mill to obtain nano-scale silk protein powder; S2, mixing the ground nano-scale silk protein powder with spinning lubricant in a ratio of 1:1, and using high-speed shearing or ultrasonic dispersion technology to form a stable silk protein spinning lubricant mixture; S3, melting the substrate at 150° C., then adding the silk protein spinning lubricant mixture, and granulating through an extrusion granulator to obtain a masterbatch containing silk protein powder; S4. Under the condition of 200° C., the substrate is melted, and master batches containing silk protein powder are added to the molten substrate, and then spinning is performed through a spinning machine to finally obtain chemical fiber containing silk protein.

2. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: S1 The pretreatment comprises the following steps: adding a silk protein modifier to a silk protein solution, stirring evenly to allow the modifier to react completely with the silk protein, and then washing, dehydrating and drying the silk protein solution to obtain a modified silk protein raw material.

3. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: The grinding temperature of the ultra-low temperature segmented ball mill described in S1 is -100°C to -196°C.

4. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: S2 The spinning lubricant oil is at least one of silicone oil, mineral oil or vegetable oil.

5. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: S3 The addition ratio of the substrate and the silk protein spinning lubricant mixture is 5:1 to 20:

1.

6. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: The substrate in S3 and S4 is polyamide, polyethylene, polypropylene or polyethylene terephthalate.

7. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: S3: The screw speed of the extrusion granulator is 30-100 rpm, and the temperature of the extrusion granulator is 140°C-160°C.

8. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: The spinning speed of S4 is 1000-5000m / min, and the spinning tension is 5-30cN.

9. The method for preparing a chemical fiber containing silk protein according to claim 1, characterized in that: S4 The spinning also includes stretching and shaping the spun fibers to fix the shape and size of the fibers.

10. The method for preparing chemical fiber containing silk protein according to claim 1, characterized in that: S4 The content of silk protein in the chemical fiber containing silk protein is 1%-30% of the total mass of the fiber.

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