KR101919127B1 - Silk yarn with improved mechancial properties and its preparation method - Google Patents

Abstract

The present invention relates to a silk fleece with greatly improved strength and elongation and a method for producing the same. Particularly, the present invention can produce a silk yarn with high mechanical strength and high mechanical strength with high mechanical strength by performing a thermocompression bonding process under optimized conditions using a moistened silk yarn including sericin in a predetermined content range have.

Description

TECHNICAL FIELD [0001] The present invention relates to a silk yarn having improved mechanical properties and a method for producing the silk yarn,

More particularly, the present invention relates to a method for producing high-strength and high-strength silk yarn with improved strength and elongation by thermocompression bonding in the production of silk yarn. BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silk yarn having a greatly improved mechanical properties, will be.

Silk is a material made of fibroin and sericin. It is a natural fiber obtained from silkworm. It has excellent gloss and texture, and has been widely used as the best textile material for mankind. In addition, silk is a medical material that has been widely used as a surgical suture for a long time based on excellent biocompatibility. Silk yarn (raw silk yarn) is made by combining multiple strands of silk filaments coming from cocoon, and since the fineness of silk filaments coming out from silk cocoon is usually about 3 denier, depending on the number of strands of embedding silk filaments, (21 denier), 42 (42 denier), and so on. When the silk flesh is refined and sericin is removed, it becomes a degummed silk yarn. Silk silk is a natural fiber obtained from silkworm, and unlike synthetic fibers, it has a characteristic that it is difficult to artificially increase the mechanical properties such as strength and elongation of silk silk.

As a result, it has been almost 5,000 years since silk was used, but the mechanical strength of silk and silk is still about 4 g / d. Silk and silk are used as clothing materials and medical materials to date, but they also occur when usage is restricted due to lack of strength and elongation in applied fields. In other words, if the strength and elongation of the silk is higher than the current level, it can be used as a material for more active clothes which is more exerted more powerfully, and the portion to be careful in washing is greatly reduced. Even in the case of medical materials, if the strength and elongation of the silk used as the surgical suture are higher than the present level, they can be easily used in a variety of surgical fields and can be used in various fields in the medical field.

For this reason, many studies have been made to increase the strength and elongation of silk, but it is considered very difficult to improve the strength and elongation of silk obtained from nature by 10-20% ought. Therefore, it is very important to improve mechanical properties in order to actively use silk and silk in various applications.

The present invention provides silk fusing with improved strength and elongation by performing thermocompression bonding under optimized conditions in the state where silk fusing sericin is swollen, and a method for manufacturing the same.

According to one embodiment of the present invention, a wetted silk green silicate having a sericin content of 19% by weight or more is hot-pressed at a temperature of 120 ° C to 280 ° C in a pressure range of 10 gf / cm ² to 500 kgf / cm ² ), Comprising the steps of:

For example, the thermocompression process may be performed for 1 second to 1 hour based on a 200 ° C treatment temperature.

The wetted silk lacquer may contain 0.05 to 50 parts by weight of water based on the weight of the dried silk lacquer.

The method for producing high-strength high-purity silk silk yarn may further include the step of wet-treating the dried silk silk with water at a temperature of 20 ° C to 100 ° C and further adding a step of producing silk silk yarn from the silk filament of silkworm cocoons As shown in FIG. It may further comprise the step of producing silk yarn from silk filaments of silkworm cocoons and, at the same time, wet treatment in water at a temperature of 20 ° C to 100 ° C.

For example, the silk yarn may have a fineness of 2 denier or more.

On the other hand, according to another embodiment of the present invention, there is provided a high strength and high degree of silk life and death produced by the method as described above.

For example, the high-strength high-density silk greening is performed in a constant temperature and humidity room under standard conditions (temperature 20 ° C., relative humidity 65%) for one day or more to reach an equilibrium state, , A gauge length of 3 cm, a tensile strength of 5 g / d or more and a tensile elongation of 20% or more when measured at a tensile rate of 10 mm / s using a load cell of 3 kgf And the crystallinity index can be 50% or more. Also, the initial Young's modulus measured by the same method may be 80 g / d or more.

According to another embodiment of the present invention, there is provided an apparatus for manufacturing high-strength high-definition silk yarn by the method as described above. The apparatus for manufacturing high-strength high-purity silk yarn comprises a wetting unit for adding sericin raw silk having a sericin content of 19% by weight or more to swell sericin; And a thermocompression bonding unit for hot pressing the wetted silk web at a temperature of 120 ° C to 280 ° C in a pressure range of 10 gf / cm ² to 500 kgf / cm ² .

For example, the apparatus for producing silk lacquer may further include a collecting unit for thermally compressed silk after the thermocompression unit.

The apparatus for lashing and producing the present invention may further comprise a marine vessel for dissolving the dried silk lint prior to the wetting treatment unit or a silk filament for releasing the silk filament from the silkworm cocoon, To the silk yarn to produce a silk yarn.

The high-strength and high-grade silk yarn production apparatus comprises a crude candy which releases silk filaments in silkworm cocoon and swells sericin by applying water thereto, and a plurality of silk filaments of the silk filament twisted to give a sericin content of not less than 19% And a thermocompression bonding portion for hot pressing the wetted silk gathers at a temperature of 120 ° C to 280 ° C in a pressure range of 10 gf / cm ² to 500 kgf / cm ² can do.

For example, the apparatus for producing silk lacquer may further include a collecting unit for thermally compressed silk after the thermocompression unit.

According to the present invention, by carrying out the thermocompression bonding process under optimized conditions in a state in which sericin is swollen by using silk fusing comprising sericin in a predetermined content range, it is possible to obtain a high strength and high- Silk life and death can be effectively produced.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic diagram showing an apparatus for producing silk yarn with excellent mechanical properties against dried silk yarn according to an embodiment of the present invention.
Fig. 2 is a schematic diagram showing an apparatus for producing silk green silk in a conventional manner.
3 is a schematic diagram showing an apparatus for producing a silk mortar with excellent mechanical properties, starting from a cocoon by disposing a wet treatment unit separate from the crude sugar, according to another embodiment of the present invention.
4 is a schematic view showing an apparatus for manufacturing a silk mortar with excellent mechanical properties, starting from the cocoon cement, by carrying out a wet treatment process in a crude sugar without arranging a separate wet processing unit, according to another embodiment of the present invention Fig.
5 is a stress-strain curve comparing Example 1 with Control 1. FIG.

In the present invention, the terms first, second, etc. are used to describe various components, and the terms are used only for the purpose of distinguishing one component from another.

Moreover, the terminology used herein is for the purpose of describing exemplary embodiments only and is not intended to be limiting of the present invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, the terms "comprises," " comprising, "" comprising, "or" having ", mean that there exist features, numbers, steps, components (or components) It is to be understood that the specification does not preclude the presence or addition of one or more other features, numbers, steps, components (or components), or combinations thereof.

While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Hereinafter, a high strength and high degree of silk greening according to a preferred embodiment of the present invention, a manufacturing method thereof, and an apparatus for manufacturing the same will be described in detail. It is to be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

The present inventors have repeatedly studied a method for producing silk flesh and silk with excellent mechanical properties, and have found that silk silk containing sericin is wet-processed to swell sericin in a predetermined content range, It is possible to produce silk yarn with improved mechanical properties, thereby completing the present invention.

According to one embodiment of the present invention, there is provided a method for producing high-strength and high-strength silk yarn with excellent mechanical properties. The high-strength high-purity silk lacquer is produced by thermocompression of a wetted silk silk having a sericin content of 19% by weight or more at a temperature of 120 to 280 ° C. in a pressure range of 10 gf / cm ² to 500 kgf / cm ² hot press) step.

Particularly, the silk ginseng production method of the present invention is characterized by having excellent properties of silk germination as a material for clothes and medical materials such as high crystallinity and mechanical strength.

For example, according to the present invention, it is possible to produce silk filaments from a plurality of silk filaments in a process of wet-processing previously prepared silk silk yarn to swell sericin, hot press at a high temperature, Instead of wrapping it in a twisted state and wrapping it around a spinning wheel to complete the production of yarn and yarn, the yarn is subjected to a pre-rolling wet-process and a thermo-compression process, Can be manufactured.

In general, the process of manufacturing silk silk is described. The silk silk filaments of the silkworm silk filament are contaminated by the corrupt pupa, or the silk silk filaments are contaminated by mold To prevent contamination. After drying the dried silkworm, it is processed several times in high temperature water to swell the sericin, and the filaments are gathered from several silkworm cocoons and twisted to make one silk silk, wrapped in a spinning wheel and dried, .

In the present invention, the wetted silk lacquer which performs the thermocompression process has a content of sericin of 19 wt% or more, or 19 to 35 wt%, preferably 22 to 30 wt%, more preferably 24 to 28 wt% . When the content of the sericin is less than 19% by weight, the amount of sericin is so small that the fibroin fibers can not be sufficiently bonded, resulting in a problem that the mechanical properties of the silk thread are deteriorated. However, since silkworms producing silk yarns having a sericin content exceeding 35% by weight are rarely found, sericin may be 35% by weight or less.

In the present invention, the term "wetted silk linting" refers to silk linting in the wet state with moisture added thereto to sufficiently swell the sericin, and it is preferable that 0.05 to 50 parts by weight of moisture .

The fineness of the silk yarn can be 2 denier or more, or 2 denier to 300 denier, preferably 10 denier to 200 denier, and more preferably 20 denier to 100 denier.

In the present invention, the silk gypsum product finally produced through the above process may be post-treated to produce silk gypsum having greatly improved mechanical properties. As shown in FIG. 1, as a dried silk raw silk, conventional silk silk products are subjected to wet treatment with water at a certain range of temperature to swell sericin in silk silk. The wet treatment may be any method as long as it allows water to penetrate the silk thread, such as a method of immersing the silk thread in water or a method of spraying water to the silk thread.

The temperature of the water to be wet treated may be 20 to 100 캜, preferably 30 to 95 캜, more preferably 40 to 90 캜. When the temperature of the water to be wet treated is less than 20 캜, it takes too much time for the sericin to swell in the silage, and the cost for lowering the water temperature is further increased. When the temperature of the water subjected to wet treatment exceeds 100 캜, sericin dissolves in the silk thread and is removed from the silk thread, so that there is a problem that the mechanical properties of the final silk thread product may be lowered due to the lowering of the adhesive force between the silk filaments have.

The wetting treatment time of the silk green silk may be 10 seconds to 24 hours, preferably 30 seconds to 6 hours, and more preferably 1 minute to 1 hour. Such wetting treatment time may vary depending on the temperature of the water. That is, the higher the temperature of the water, the shorter the wetting time, and the lower the water temperature, the more the wetting time increases. On the other hand, when the wetting treatment time is less than 10 seconds, it is difficult to precisely match a too short time in mass production, which may result in a significant change in quality, which may cause difficulties in quality control. If the time for wet treatment exceeds 24 hours, there is a problem that the time required for the process is unnecessarily long and the cost of production of silkworm is increased.

For example, if the temperature of the water is in the range of 30 ° C. to 95 ° C., the immersion time may be 1 minute to 24 hours. If the temperature of the water exceeds 95 ° C., the immersion time may be applied within 30 minutes . In particular, it is preferable to reduce the immersion time as the water temperature approaches 100 DEG C, and it is preferable to apply it within about 20 minutes. If the wetting step is carried out excessively, there may occur a problem that the mechanical properties of the silk thread are deteriorated as the sericin is dissolved and removed.

The wetting treatment step is preferably carried out in the silk mortar on the basis of the weight of the dried silk mortar, that is, 0.05 to 50 parts by weight, preferably 0.1 to 20 parts by weight, more preferably 0.1 to 20 parts by weight, 0.5 to 10 parts by weight of water may be further contained. In the case where the moisture content of the silk yarn is less than 0.05 part by weight in the wet treatment process, the degree of adhesion of the silk filament fibers to each other during drying or thermocompression is low, May occur. Further, there is a limit to the repair performance that the silkworm can have, so that in the case of silk silkworms, it is practically impossible to contain more than 50 parts by weight of water. In addition, when excessive moisture is supplied, additional energy is required to remove water in the subsequent process, which may lead to a disadvantage that the cost for manufacturing silk waste is increased.

The wet-treated silk raw silk can be thermocompression-bonded to complete silk silk with excellent mechanical properties. The hot press process is carried out at a temperature of 120 to 280 DEG C, preferably 135 to < RTI ID = 0.0 > 265 캜, more preferably 150 캜 to 250 캜. In addition, the hot press process may be performed for 1 second to 1 hour, preferably 2 seconds to 30 minutes, more preferably 3 seconds to 10 minutes, . If the thermocompression process is shorter than one second, the sericin is deformed and it is difficult to serve as a binder for bonding the fibroin fibers to the surrounding area. If the thermocompression process is shorter than one second, the economic efficiency is lowered and the yellowing of the silk occurs, .

In the case of such a thermocompression, it is important to transfer heat energy to the silk thread. Therefore, as the thermal compression temperature increases, the time required for the processing (processing time) decreases. On the contrary, the processing time must be increased as the thermal compression temperature decreases. Therefore, the process temperature and the process time for the hot press process may be adjusted according to variables such as the temperature increase or the time increase. If the pressing temperature is less than 120 ° C, the sericin is deformed to make it difficult to serve as a binder for bonding the fibroin fibers to the periphery, or the treatment time must be prolonged, resulting in a reduction in economic efficiency. There is a problem that the molecular weight of the silk chains is severed by the high temperature and, consequently, the mechanical properties of the silk yarn are reduced.

The pressure applied to the green sheet in the thermocompression process should be 10 gf / cm ² to 500 kgf / cm ² , preferably 100 gf / cm ² to 100 kgf / cm ² , more preferably 1 kgf / cm 2 ² to 50 kgf / cm < ² >. If it is less than 10 gf / cm ² , there is a problem that the mechanical properties of the obtained silk thread are not improved because the pressure is insufficient and sericin can not serve as a binder for bonding the fibroin fibers. However, if the pressing range of the thermocompressor exceeds 500 kgf / cm ² , there may be a problem that the obtained silk life becomes too flat.

In addition, the method for producing high-strength high-purity silk green silk may further include the step of producing silk silk from silk filaments of silkworm cocoon. As an example, the silk yarn may be prepared from silk filaments of silkworm cocoons, and at the same time wet treatment may be carried out in water at a temperature of 20 ° C to 100 ° C.

In the present invention, the filaments are gathered from several cocoon cocoons to form one silk silk yarn, and then subjected to a wet process and a thermocompression process before winding the silk silk yarn to produce a silk silk yarn having excellent mechanical properties can do. That is, in the existing silk screening process (FIG. 2), only the direct wetting process and the thermocompression process are added, and then the silk screen silk having excellent mechanical properties is completed and wound around the collecting part (FIG. 3). In addition, as in the conventional silk screening process, the silkworm silk filament is swollen by immersing the silkworm cocoa in hot water to swell the silk filaments, and twisted silk filaments are twisted to produce silk yarn. (Wet processing section) is omitted, the wet processing process is performed in the crude bath, and only the thermocompression bonding process (thermocompression bonding section) can be added (FIG. 4). When the wet treatment process is carried out in the crude candy, the temperature and immersion time of the water in the crude candy can be applied in the same manner as described above.

Thus, in the process of producing the silk yarn from the silk filament of the silkworm cocoon and simultaneously performing the wetting treatment, the conditions of the wetting treatment process, the moisture content, the thermocompression temperature and the pressure are as described above.

The manufacturing method of the high-strength high-purity silk lacquer may further include a step that is conventionally employed in the technical field to which the present invention belongs, in addition to the above-described steps.

On the other hand, according to another embodiment of the present invention, there is provided a silk yarn produced by the above-described method. The silk thread has high mechanical properties and has excellent biocompatibility of natural silk.

First, in the present invention, the term "silk yarn" refers to a yarn which is formed by knitting a plurality of silk filaments in a silkworm cocoon and twisting the yarn, and has the same composition as the silk filaments in the silkworm cocoon . The silk filaments have a structure in which two fibroin strands are surrounded by sericin. The silk filaments are composed of 65 to 80 parts by weight of fibroin, 20 to 35 parts by weight of sericin, and other components such as wax, pigment, polysaccharide, The material is made up of 10 parts by weight or less of material. In the case of silk thread, silk filaments of the silk filament are produced using silk filaments. On the other hand, when a silk fabric is produced by using silk thread silk, the silk fabric is subjected to a refining process to remove sericin in order to improve the gloss and touch because it has poor gloss and feel. For reference, the yarn obtained by refining silk ginseng and removing sericin is called "ginseng silk".

 Since the silk silk yarn excellent in mechanical properties of the present invention can be produced by wet processing and thermocompression bonding, it has the same composition as the silk filament of the silkworm silk and the existing silk silk yarn product (silk yarn without performing the process of the present invention). That is, it is composed of 70 to 80 parts by weight of fibroin, 20 to 30 parts by weight of sericin, and 10 parts by weight or less of other substances (wax, polysaccharide, dye, etc.) per 100 parts by weight of the silk filament.

The fineness of the silk thread of the present invention has a value of 2 denier or more or 2 denier to 300 denier. Preferably from 10 denier to 200 denier, and more preferably from 20 denier to 100 denier. Since the silk thread is produced by collecting a plurality of silk filaments of silk filaments and the fineness of one silk filament is less than 2 deniers, the fineness of the silk thread silk is practically less than 2 deniers. Silicone silk is very rare when using 300 denier or more. In case of silk silk and silk of 300 denier or more, the sericin swells due to the process of ingestion and the thermocompression process, and is deformed by the heat treatment, In the case of silk lacquer over denier, it is difficult to obtain excellent mechanical properties of the present invention.

The silk thread of the present invention was stored in a constant temperature and humidity room at a temperature of 20 ° C and a relative humidity of 65% for 1 day or more to reach an equilibrium state. Then, a silk thread was prepared at a size of 10 cm, length is 3 cm, tensile strength is 5 g / d or more, or 5 g / d to 20 g / d when measured at a tensile speed of 10 mm / s using a load cell of 3 kgf, g / d, tensile elongation is 20% or more, or 20% to 40%. The silk thread mortar has an initial Young's modulus of 80 g / d or more or 80 g / d to 300 g / d, preferably 100 g / d or more, more preferably 150 g / d or more .

The crystallinity index of the silk lacquer may be 50% or more or 50% to 80%. , Preferably not less than 52%, and more preferably not less than 53%. When the crystallinity index is less than 50%, the natural silk is not highly crystalline and less than 50% unlike the regenerated silk. However, since there is a limit to the crystallinity that natural silk can have, it is practically impossible that the crystallinity index exceeds 80%.

The mechanical properties of the silk thread in the present invention are significantly higher than those of conventional silk threads because the adhesive strength of sericin is maximized by the process of the present invention. That is, the silk thread is produced by a plurality of silk filaments bonded together, and the adhesive strength of sericin plays an important role in the production of silk thread. Conventional silk flesh products are prepared by swelling sericin to bond silk filaments to each other. However, in the present invention, when sericin is swollen and heat and pressure are simultaneously applied (that is, when thermocompression is performed), the adhesive force of sericin is maximized The effect of bonding the silk filaments to each other is maximized, and the strength and elongation of the silk yarn obtained as a result is greatly increased.

In addition to the above-mentioned components, drugs, functional materials, additives, auxiliary ingredients and the like commonly known in the technical field to which the present invention belongs can be added to the silk silk in order to be suitable for specific use within the range of not compromising the excellent characteristics inherent in natural silk have.

According to another embodiment of the present invention, there is provided an apparatus which can be effectively used in the above-described process for producing high-strength and high-density silk yarn. The apparatus for producing high-strength and high-degree silk flesh and silk according to the present invention comprises a wetting unit for adding sericin silk with a sericin content of 19% by weight or more to swell sericin; And a thermocompression bonding unit for hot pressing the wetted silk web at a temperature of 120 ° C to 280 ° C in a pressure range of 10 gf / cm ² to 500 kgf / cm ² .

The high-strength high-definition silk yarn-producing apparatus may further include a collecting unit for thermally compressed silk yarn after the thermocompression unit.

In addition, it is preferable that the wet processing unit further includes a sea-marine unit for disassembling the dried silk yarn before the wet treatment unit, or a crude candy which releases the silk filament from the silkworm cocoon, and a plurality of silk filaments from the crude- And an irradiating unit for irradiating the irradiated region with the radiation.

An embodiment of the apparatus for producing silk yarn of the present invention can provide an apparatus capable of effectively performing a post-treatment process by using existing silk yarn products as shown in Fig. For example, marine vessels that untie existing silk and silk products; A wet processing section for treating the silk gypsum product from the marine section so as to contain moisture; A thermocompression bonding section for applying thermocompression to the wet processed silk flesh product; And a collecting part for winding the silk flesh product after the thermocompression treatment.

In addition, another embodiment of the apparatus for producing silk yarn of the present invention can provide an apparatus capable of effectively performing a post-treatment process by using a conventional silk screening apparatus or the like as shown in Fig. For example, crude candy which releases silk filaments from silkworm cocoon; An irradiating unit for twisting various strands of silk filaments coming from the crude bath to produce silk yarns; A wet processing unit for processing the silk raw silk so that the water is contained in the silk silk yarn after the irradiation is completed; A thermocompression bonding section for applying thermocompression to the wet processed silk flesh product; And a collecting part for winding the silk flesh product after the thermocompression treatment.

On the other hand, the apparatus for producing high-strength and high-grade silk flesh and silk yarns is characterized in that silk filaments are unwound from silkworms to swell sericin by applying water thereto and twisted to several strands of silk filaments coming from the silk filaments, or more wetting the check block for producing a silk green sand, and heat to the wetted silk green sand to thermal compression to a temperature of 120 ℃ to 280 ℃ 10 gf / cm ² to about 500 pressure range kgf / cm ² (hot press) And a pressing part.

The high-strength high-definition silk yarn-producing apparatus may further include a collecting unit for thermally compressed silk yarn after the thermocompression unit.

Another embodiment of the apparatus for producing silk flesh and silk of the present invention is characterized in that as shown in FIG. 4, a wet processing process is performed in crude candy or the like among existing silk screening apparatuses, and a post- An apparatus capable of performing effectively can be provided. For example, crude candy which releases silk filaments from silkworm cocoons and swells sericin by adding water; An irradiating unit for producing a wetted silk silk yarn having a sericin content of not less than 19% by weight by twisting several strands of the silk filaments coming from the crude bath; A thermocompression bonding portion for applying thermocompression to the wetted silk web; And a collecting part for winding the silk flesh product after the thermocompression treatment.

In the present invention, matters other than those described above can be added or subtracted as required, and therefore, the present invention is not particularly limited thereto.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the scope of the present invention is not limited to the following examples.

Control Example  One

First, a 21 denier (silicate content 26.5%) of silk raw silk as an existing product was used as a control 1.

Example  1 to 8

As shown in Fig. 1, using a device including a marine portion and a wet processing portion, a thermocompression bonding portion and a collecting portion was used, and as a dried silk silk thread (silk silk product), a silk silk thread 21 denier product (sericin content 26.5 %), Followed by wet pressing, followed by thermocompression, to produce silk green silk (hereinafter referred to as a post-treatment method).

First, the dried silk thread was loosened in a cone state at the maritime part, and then immersed so as to contain 0.7 part by weight of water based on the weight of the dried silk thread in a water tank of the wet treatment part. The temperature of the water contained in the water tank and the soaking time of the silk thread were as shown in Table 1 below and were applied at 40 to 100 ° C for 1 minute or 30 minutes. Thereafter, the wetted silk lye (the content of sericin 26.5%) was subjected to heat treatment at 150-150 ° C using a thermocompressor (HK 2008-1-5, Hankuk Industry Co., Korea) After thermocompression at 5 kgf / cm ² for 10 seconds at 250 ° C, the same procedure was repeated one more time. A polyester nonwoven fabric was added between the silk raw yarn and the thermocompressor in order to prevent the silk yarn from adhering to the thermocompressor before the thermocompression process so that the silk yarn did not directly touch the thermocompressor.

Example  9-12

As shown in Fig. 4, the wet treatment process is carried out in the crude candy without a separate wet processing section, and a device including an irradiating section, a thermocompression bonding section and a storing section is used together with the crude candy, The wet silk yarn obtained in the process was thermally compressed before being wound on a collection part such as a spinning wheel to produce silk yarn (this is referred to as a simultaneous treatment method).

First, the silk filaments were loosened from the silkworm cocoons in the crude silk bath, and then the silk silkworms were prepared by twisting several strands of the silk filaments coming out of the crude silkworms in the irradiation part. At this time, the temperature of the water in the crude sugar was 60 ° C, and the immersion time of the silk filaments was 30 minutes. At the same time, the silk raw silk finished with the wet treatment in the crude silk was measured based on the weight of the dried silk silk To 0.7 part by weight of water. Thereafter, the wetted silk lye (the content of sericin 26.5%) was subjected to heat treatment at 150-150 ° C using a thermocompressor (HK 2008-1-5, Hankuk Industry Co., Korea) After thermocompression at 5 kgf / cm ² for 10 seconds at 250 ° C, the same procedure was repeated one more time. A polyester nonwoven fabric was added between the silk raw yarn and the thermocompressor in order to prevent the silk yarn from adhering to the thermocompressor before the thermocompression process so that the silk yarn did not directly touch the thermocompressor.

Example  13

As shown in the following Table 1, silk greening was produced in the same manner as in Example 11, except that the pressure range applied during thermocompression was 0.5 kgf / cm ² .

Comparative Example  1 and 2

As shown in the following Table 1, silk mortars were produced in the same manner as in Example 2, except that the temperature range applied during thermocompression was changed to 100 ° C and 300 ° C, respectively.

Comparative Example  3 and 4

As shown in the following Table 1, silk and silk were produced in the same manner as in Example 9, except that the temperature ranges applied at the time of thermocompression were changed to 100 ° C. and 300 ° C., respectively.

Comparative Example  5

As shown in the following Table 1, silk mortality was produced in the same manner as in Example 11, except that the applied pressure range at the time of thermocompression was changed to 0.005 kgf / cm ² .

Test Example

The properties of the conventional silk fleece product of Control Example 1, the silk fleece prepared according to Examples 1 to 13 and Comparative Examples 1 to 5 were evaluated by the following methods, and the results of the measurement are shown in Table 1 below.

a) Measurement of strength and elongation of nonwoven fabric

The strength and elongation were measured using a universal material testing machine (OTT-003, Oriental TM, Korea) to investigate the mechanical properties of silk thread.

First, all the samples before measurement were stored for 1 day or longer in a constant temperature and humidity room at a temperature of 20 ° C and a relative humidity of 65% to reach an equilibrium state, and then the strength and elongation were measured under the same temperature and humidity conditions. At this time, the silk thread samples were prepared at a length of 10 cm and measured at a tensile speed of 10 mm / s using a 3 kgf load cell under a gauge length of 3 cm.

Wet process Thermocompression process Properties of silk Processing method Immersion
Temperature
(° C) Immersion
time
(minute) Pressure
pressure
(kgf / cm ² ) Pressure
Temperature
(° C) Pressure
time
(second) Seal
burglar
(g / d) Seal
Shindo
(%) Example 1 After treatment 40 30 5 200 20 6.1 25.3 Example 2 After treatment 60 30 5 200 20 6.0 25.4 Example 3 After treatment 80 30 5 200 20 6.1 25.3 Example 4 After treatment 95 30 5 200 20 6.0 25.4 Example 5 After treatment 60 30 5 150 20 5.1 21.6 Example 6 After treatment 60 30 5 180 20 5.5 23.3 Example 7 After treatment 60 30 5 250 20 5.1 20.8 Example 8 After treatment 100 One 5 200 20 6.0 25.4 Example 9 Concurrent processing - - 5 150 20 5.2 22.0 Example 10 Concurrent processing - - 5 180 20 5.6 23.7 Example 11 Concurrent processing - - 5 200 20 6.1 25.8 Example 12 Concurrent processing - - 5 250 20 5.1 21.2 Example 13 Concurrent processing 0.5 200 20 5.2 21.6 Control Example 1 - - - - - - 3.8 16.1 Comparative Example 1 After treatment 60 30 5 100 20 3.9 16.5 Comparative Example 2 After treatment 60 30 5 300 20 2.9 12.3 Comparative Example 3 Concurrent processing - - 5 100 20 3.8 16.1 Comparative Example 4 Concurrent processing - - 5 300 20 2.9 12.3 Comparative Example 5 Concurrent processing - - 0.005 200 20 3.8 16.1

In Examples 1 to 4, the tensile strength was higher than 6 g / d and the tensile elongation was higher than 25%. In the case of Example 1, the values increased by more than 50% (Fig. 5). On the other hand, the difference according to immersion temperature change was not large. In Examples 5 and 6, the tensile strength and tensile elongation were somewhat decreased as the pressing temperature was decreased to 150 ° C. and 180 ° C., but the strength and elongation were still higher than those of Control Example 1 (untreated) Showed improved results. Here, the strength and elongation at 150 ° C and 180 ° C were slightly lower than 200 ° C, because the pressing temperature was relatively low, and thus the adhesion of sericin was low, thus improving the mechanical properties of the silk thread. On the other hand, in the case of Example 7, as the pressing temperature increased to 250 ° C, the tensile strength decreased as compared with 200 ° C. As the pressing temperature began to increase, the cericin began to pyrolyze, It is considered that the improvement effect of the silk god of war was less. In addition, Example 8 also showed high tensile strength and elongation, which is thought to be the result of optimization of the pressing temperature to 200 캜.

Further, in the silk screening of Examples 9 to 13 produced by the simultaneous treatment of the wet treatment process with the crude sugar, the tensile strength and elongation were the highest when the pressing temperature was 200 ° C, It was found that the effect was similar to silk mortar produced by post - treatment method. That is, as the pressing temperature increased to 200 ° C, the tensile strength and elongation of the silk green yarn increased at the same time, but the tensile strength and elongation decreased at 200 ° C or higher. On the other hand, in the case of the embodiment the pressing pressure lowered to 0.5 kgf / cm ² in Example 13, the strength and elongation 5.2 g / d, and to somewhat lower the pressure range of the heat pressing machine by 21.6% compared to 5 kgf / cm ^2, Example 11 . However, this case also showed a much improved result in terms of strength and elongation as compared with Control Example 1.

On the other hand, in the case of Comparative Examples 1 and 3, in which the pressing temperature was 100 ° C, the tensile strength and elongation were not significantly different from those in Control Example 1 in which no treatment was applied, When the temperature is low, the adhesive strength of sericin is not so high, and the mechanical properties of silk and silk are not improved. Also in the case of Comparative Examples 2 and 4, in which the pressing temperature was 300 ° C, regardless of the treatment method, the tensile strength and the elongation were also lower than those in Control Example 1 in which no treatment was performed. , The thermal decomposition of sericin occurs severely and the strength and elongation are rather lowered. On the other hand, in the case of Comparative Example 5 in which the pressurizing pressure was lowered to 0.005 kgf / cm ² , there was no significant change in strength and elongation as compared with Control Example 1, and it is understood that a certain level of pressure is required.

Claims (17)

High-strength high signal comprising a (hot press) method comprising sericin content is 19 bond the silk green sand wetting or more% by weight at 150 ℃ to a temperature of 265 ℃ 0.5 kgf / cm ² to 100 kgf / pressure range of the cm ² Fig. Production method of silk silk.
The method according to claim 1,
Wherein the thermocompression bonding step is performed for 1 second to 1 hour based on a treatment temperature of 200 캜.
The method according to claim 1,
Wherein the wetted silk gathers include water in an amount of 0.05 to 50 parts by weight based on 100 parts by weight of dried silk gathers.
The method according to claim 1,
Further comprising the step of wet-treating the dried silk gypsum in water at a temperature of from 20 캜 to 100 캜.
The method according to claim 1,
Further comprising the step of producing silk silk yarn from silk filaments of silkworm cocoons.
The method according to claim 1,
Further comprising a step of producing silk yarn from silk filaments of silkworm cocoons and at the same time wet treatment in water at a temperature of from 20 캜 to 100 캜.
The method according to claim 1,
Wherein said silk germination is a high-strength high-grade silk germination yarn having a fineness of 2 denier or more.
7. A high strength, high strength, silk mortar prepared by the process of any one of claims 1 to 7 and having a tensile strength of at least 5.1 g / d and a tensile elongation of at least 20.8%.
9. The method of claim 8,
High-strength high-silk silk with a tensile strength of 6 g / d or more and a tensile elongation of 25% or more.
9. The method of claim 8,
High-strength high-silk silk life with a crystallinity index of 50% or more.
9. The method of claim 8,
High-strength high-purity silk mortar with initial Young's modulus of 80 g / d or more.
A wetting treatment unit for adding water to silk germination silk having a sericin content of 19% by weight or more to swell sericin; And
The wetted silk green yarn is thermocompression bonded at a temperature of 150 ° C to 265 ° C in a pressure range of 0.5 kgf / cm ² to 100 kgf / cm ²
Wherein said high-strength high-strength silk yarn is produced by a method comprising the steps of:
13. The method of claim 12,
Further comprising a collecting section for collecting the thermocompression bonded silk after the thermocompression bonding section.
13. The method of claim 12,
Further comprising a marine part for disassembling the dried silk silk before the wet treatment part.
13. The method of claim 12,
A high-strength high-purity silk yarn-fusing device further comprising a crude candy which loosens the silk filaments in the silkworm cocoon before the wet processing section, and an irradiating section for producing silk silk yarns by twisting several strands of the silk filaments coming out of the crude silk- .
Silk filaments are extracted from silkworm cocoons and swollen sericin is added by adding water.
An irradiating part for producing a wetted silk yarn having a sericin content of not less than 19% by weight by twisting several strands of the silk filaments coming from the crude bath, and
The wetted silk green yarn is thermocompression bonded at a temperature of 150 ° C to 265 ° C in a pressure range of 0.5 kgf / cm ² to 100 kgf / cm ²
Wherein said high-strength high-strength silk yarn is produced by a method comprising the steps of:
17. The method of claim 16,
Further comprising a collecting section for collecting the thermocompression bonded silk after the thermocompression bonding section.

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