CN109730497B - Expansion silk wadding quilt based on mulberry silk and preparation method thereof - Google Patents
Expansion silk wadding quilt based on mulberry silk and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an expanded silk wadding quilt based on mulberry silk and a preparation method thereof, wherein the preparation method comprises the following steps: adding the mixed solution of the turmeric extract, acetic acid and carboxymethyl cellulose into the degummed fibroin fiber solution, carrying out ultrasonic treatment, adding polyurea formaldehyde and selenocysteine hydrochloride, and carrying out ultrasonic treatment; preparing silk with holes into a silk floss sheet, and then soaking the silk floss sheet in an amino polyethylene glycol aqueous solution to obtain a treated silk floss sheet; placing the treated silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain a wet swelling silk floss sheet; dehydrating the expanded wet silk floss sheet, manually loosening and drying to obtain an expanded dry silk floss sheet of the silkworm; combining the swelling dry silk floss piece and the treated tussah silk floss piece, and sewing to obtain the swelling silk floss quilt. The porous bulked silk floss sheet with excellent wearability is successfully prepared by the method, has good antibacterial property, and has practical positive significance.
Description
Technical Field
The invention relates to a preparation method of silk floss, in particular to an expanded silk floss quilt based on mulberry silk and a preparation method thereof.
Background
Along with the improvement of living standard of people, people increasingly advocate and return to nature, the consumption of pure natural silk floss quilt is increased sharply, and the consumption market is expanded year by year. The silk wadding quilt is made of various real silks, wherein the silk wadding quilt made of the porous bulked real silk has more excellent wearing performances such as elasticity, heat retention, softness and the like compared with the common silk wadding quilt. The porous bulked real silk is silk with a porous structure in silk fibers, and the porous structure can form a plurality of micro spaces for storing air and can store a large amount of static air, so that the silk has good heat retention property, good air permeability and moisture permeability, and is widely concerned and deeply researched.
The mulberry silk is soft and is widely applied to the field of silk wadding quilts, but the mechanical property of the mulberry silk is poor, particularly after swelling, so that the prior art has almost no report about porous swelling mulberry silk.
The existing preparation method of the expanded yarn has poor effect, needs a large amount of chemical reagents and does not accord with the theme of green environmental protection. Therefore, the development of the expanded silk floss quilt and the preparation method thereof have positive practical significance.
Disclosure of Invention
The invention aims to provide an expanded silk wadding quilt based on mulberry silk and a preparation method thereof, so as to obtain the expanded silk wadding quilt with excellent performance.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the mulberry silk based expansive silk wadding quilt is characterized in that the preparation method of the mulberry silk based expansive silk wadding quilt comprises the following steps:
(1) degumming the cleaned mulberry silk at high temperature and high pressure to obtain a degummed mulberry silk cellulose fiber solution;
(2) adding a mixed solution of a turmeric extract, acetic acid and carboxymethyl cellulose into a degummed mulberry silk cellulose fiber solution, carrying out ultrasonic treatment for 2-3 hours, adding polyurea formaldehyde and selenocysteine hydrochloride, and carrying out ultrasonic treatment for 1-1.5 hours; then dehydrating and drying in the sun to obtain the processed mulberry silk;
the chemical structural formula of the selenocysteine hydrochloride is as follows:
(3) heating the processed mulberry silk at 160 ℃ for 40 seconds, and then heating at 200 ℃ for 25 seconds to obtain the mulberry silk with holes; preparing mulberry silk with holes into a mulberry silk floss sheet, and then soaking the mulberry silk floss sheet into an amino polyethylene glycol aqueous solution to obtain a treated mulberry silk floss sheet;
(4) placing the processed mulberry silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain a swelling wet mulberry silk floss sheet;
(5) dehydrating the expanded wet mulberry silk floss sheet, manually loosening the sheet, and drying the sheet to obtain an expanded dry mulberry silk floss sheet;
(6) degumming the washed tussah silk at high temperature and high pressure to obtain a degummed tussah silk fibroin fiber solution; adding trimethylsilanol into the degummed tussah silk fibroin fiber solution, carrying out ultrasonic treatment for 2-3 hours, and then dehydrating and drying in the sun to obtain the treated tussah silk; preparing the processed tussah silk into tussah silk cotton sheets;
(7) and combining and sewing the expanded dry mulberry silk cotton sheet and the tussah silk cotton sheet to obtain the expanded silk cotton quilt based on the mulberry silk.
A preparation method of an expanded silk wadding quilt based on mulberry silk comprises the following steps:
(1) degumming the cleaned mulberry silk at high temperature and high pressure to obtain a degummed mulberry silk cellulose fiber solution;
(2) adding a mixed solution of a turmeric extract, acetic acid and carboxymethyl cellulose into a degummed mulberry silk cellulose fiber solution, carrying out ultrasonic treatment for 2-3 hours, adding polyurea formaldehyde and selenocysteine hydrochloride, and carrying out ultrasonic treatment for 1-1.5 hours; then dehydrating and drying in the sun to obtain the processed mulberry silk;
the chemical structural formula of the selenocysteine hydrochloride is as follows:
(3) heating the processed mulberry silk at 160 ℃ for 40 seconds, and then heating at 200 ℃ for 25 seconds to obtain the mulberry silk with holes; preparing mulberry silk with holes into a mulberry silk floss sheet, and then soaking the mulberry silk floss sheet into an amino polyethylene glycol aqueous solution to obtain a treated mulberry silk floss sheet;
(4) placing the processed mulberry silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain a swelling wet mulberry silk floss sheet;
(5) dehydrating the expanded wet mulberry silk floss sheet, manually loosening the sheet, and drying the sheet to obtain an expanded dry mulberry silk floss sheet;
(6) degumming the washed tussah silk at high temperature and high pressure to obtain a degummed tussah silk fibroin fiber solution; adding trimethylsilanol into the degummed tussah silk fibroin fiber solution, carrying out ultrasonic treatment for 2-3 hours, and then dehydrating and drying in the sun to obtain the treated tussah silk; preparing the processed tussah silk into tussah silk cotton sheets;
(7) and combining and sewing the expanded dry mulberry silk cotton sheet and the tussah silk cotton sheet to obtain the expanded silk cotton quilt based on the mulberry silk.
In the technical scheme, in the step (1), the pressure of the high-temperature high-pressure degumming is 0.1-0.2 MPa, the temperature is 110-135 ℃, and the degumming time is 6-8 minutes; in the step (6), the pressure of the high-temperature high-pressure degumming is 0.15-0.3 MPa, the temperature is 110-135 ℃, and the degumming time is 10-20 minutes.
In the technical scheme, in the step (1), mulberry silk is used as a raw material, impurities are removed, rinsing is carried out, water is added to soak for at least 30min, the bath ratio is 10-20: 1, and then dehydration is carried out to finish cleaning; in the step (6), tussah silk is used as a raw material, impurities are removed, rinsing is carried out, water is added to soak for at least 30min, the bath ratio is 10-20: 1, and then dehydration is carried out to finish cleaning.
In the technical scheme, in the step (2), the mass ratio of the degummed mulberry silk cellulose fiber, the turmeric extract, the acetic acid, the carboxymethyl cellulose, the polyurea formaldehyde and the selenocysteine hydrochloride is 100: 5: 4: 5: 2; in the step (6), the mass ratio of the degummed tussah silk fibroin fiber to the trimethylsilanol is 100: 18.
In the technical scheme, in the step (2), the mass concentration of the degummed mulberry silk cellulose fiber solution is 55-62%; in the step (6), the mass concentration of the degummed tussah silk fibroin fiber solution is 75-78%. The reactivity of the treating agent with the silk fibroin fiber can be improved.
In the technical scheme, in the step (3), the mass ratio of the mulberry silk floss sheet to the amino polyethylene glycol is 100: 6, so that the silk floss sheet is soft and smooth and compatible, and the pores are uniform during expansion, and the pores are prevented from being diffused too fast.
In the technical scheme, in the step (4), when the puffing is carried out, the saturated steam pressure in the closed container is 0.08 Mpa; the closed container rotates at 12 r/min; when the saturated steam pressure in the closed container is increased to 0.5Mpa, the rupture disk is ruptured.
In the technical scheme, in the step (5), the drying is carried out at 185 ℃ for 25 seconds and then at 105 ℃ for 135 seconds; the holes of the silk floss sheet are expanded by higher temperature, and then the moisture is removed at low temperature, thereby not only achieving the drying effect, but also avoiding the residual of organic volatile matters, and improving the fluffiness of the silk floss quilt.
In the technical scheme, trimethylsilanol is used as a modification component to improve the surface performance of tussah silk, such as hydrophobicity; according to the invention, the treating agent is added into the silk fibroin fiber solution, so that the treatment uniformity and stability can be improved; the drying can improve the reaction uniformity of the treating agent on the surface of the mulberry silk, and the problem of uneven reaction caused by direct drying is avoided.
The invention also discloses the mulberry silk-based expanded silk wadding quilt obtained by the preparation method; the volume ratio of the expanded dry mulberry silk cotton sheet to the tussah silk cotton sheet is 100: 18, the mulberry silk can increase the gaps of the silk cotton quilt and provide good heat preservation, but the mechanical property is low, the physical effect between the tussah silk cotton sheet and the expanded dry mulberry silk cotton sheet is utilized to reinforce, the expanded dry mulberry silk cotton sheet and the tussah silk cotton sheet are combined to be stacked at intervals, and the expanded dry mulberry silk cotton sheet is preferably selected as the first layer and the last layer.
In the above, the step (2) is used for forming a coating on the surface of silk to make the silk have antibacterial property and keep warm, and is a method using natural green antibacterial agent; the carboxymethyl cellulose may improve the adhesion of turmeric extract and other compounds to the surface of the silk floss sheet. The polyurea formaldehyde can provide porous performance, a certain small hole can be formed on the surface of the silk fibroin fiber by matching with the selenocysteine hydrochloride and the treatment process in the step (3), the preparation and the mechanical property of the silk floss sheet are not influenced, and the pore-forming and the hole expanding are performed simultaneously during the expansion, so that the technical effect far superior to that brought by pure expansion is achieved. The dosage is controlled, on one hand, the influence on the fiber performance is avoided, and on the other hand, a product with excellent antibacterial property, mechanical property and porous property can be obtained.
The invention puts the silk floss piece into the rotary closed container with bursting film, then the high pressure saturated steam is let into the container, the pressure is kept for a certain time, under the action of the high temperature and high pressure saturated steam, the silk fiber of the silk floss piece is quickly converted into the swelling stage from swelling, when the sudden decompression generates the air explosion, the tussah silk floss piece is instantly reduced from the high pressure to the normal pressure state, the accumulated energy of the silk fiber is suddenly released, the internal of the silk fiber generates the porous structure, and the silk fiber swells and increases the volume, thereby achieving the purpose of swelling. However, the expansion porosity of the prior art can cause the performance of the mulberry silk with weak mechanical properties to further reduce, which is different from that of tussah silk, and is also the reason for the expansion porosity research of the mulberry silk rarely; on one hand, the invention adopts a new expansion pore-forming process and on the other hand adopts a modifier to obtain the expanded porous mulberry silk with the mechanical property equivalent to that before pore-forming.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the invention has positive practical significance, and experiments prove that the porous bulked mulberry silk floss quilt obtained by the invention has better bulkiness and heat preservation rate, the antibacterial rate is also greatly improved, and the wearability is greatly improved.
2. The raw materials added in the preparation process are safe, and the preparation method is beneficial to preparing household products.
3. The invention ultrasonic-treats the silk in the mixed solution of turmeric extract, acetic acid and carboxymethyl cellulose, so that the silk has good antibacterial property, and is a method using natural green antibacterial agent.
4. The mulberry silk is treated for the first time, so that the mulberry silk has good surface performance, and the mulberry silk has the advantages of keeping warm and fluffy.
5. The preparation method is simple, has low cost and good application prospect.
Drawings
FIG. 1 is a schematic view of a combination structure of an expanded dry mulberry silk cotton sheet and an tussah silk cotton sheet;
wherein, 1 is an expanded dry mulberry silk cotton sheet, and 2 is a tussah silk cotton sheet.
Detailed Description
The invention is further described below with reference to the following examples:
example one
A preparation method of an expanded silk floss quilt comprises the following steps:
(1) using mulberry silk as a raw material, removing impurities, rinsing, adding water, and soaking for 50min at a bath ratio of 15: 1; then dehydrating and finishing cleaning; degumming the cleaned silk at high temperature and high pressure; after degumming, discharging the degumming silk cellulose solution from the reaction kettle; the pressure of high-temperature high-pressure degumming is 0.15MPa, the temperature is 118 ℃, and the degumming time is 8 minutes; the mass concentration of the degummed mulberry silk cellulose fiber solution is 58 percent;
(2) adding the mixed solution of the turmeric extract, acetic acid and carboxymethyl cellulose into the degummed mulberry silk fibroin fiber solution, carrying out ultrasonic treatment for 2 hours, adding the polyureaformaldehyde and selenocysteine hydrochloride, and carrying out ultrasonic treatment for 1 hour; then dehydrating and drying in the sun to obtain the processed mulberry silk; the mass ratio of the degummed silk fiber, the turmeric extract, the acetic acid, the carboxymethyl cellulose, the polyurea formaldehyde and the selenocysteine hydrochloride is 100: 5: 4: 5: 2;
the chemical structural formula of the selenocysteine hydrochloride (CAS No. 3542-13-0) is as follows:
(3) heating the processed mulberry silk at 160 ℃ for 40 seconds, and then heating at 200 ℃ for 25 seconds to obtain the silk with holes; preparing silk with holes into a mulberry silk cotton sheet by adopting a conventional method, and then soaking the mulberry silk cotton sheet into an amino polyethylene glycol aqueous solution to obtain a treated mulberry silk cotton sheet; the mass ratio of the mulberry silk floss piece to the amino polyethylene glycol is 100: 6;
(4) placing the processed mulberry silk floss piece into a rotary closed container with a rupture membrane for swelling to obtain a swelling wet silk floss quilt; when puffing, the saturated steam pressure in the closed container is 0.08 Mpa; the closed container rotates at 12 r/min; when the saturated steam pressure in the closed container is increased to 0.5Mpa, the rupture disk is ruptured; the bursting disk arranged on the bursting port cover of the closed container is broken, the silk floss sheet is suddenly decompressed instantly and is subjected to air explosion, and then the silk floss sheet is punched out of the bursting port, so that the mulberry silk is bulked and the silk fiber is porous;
(5) dehydrating the expanded wet silk floss sheet, manually loosening and drying to obtain an expanded dry mulberry silk floss sheet; the drying is carried out for 25 seconds at 185 ℃ and then 135 seconds at 105 ℃;
(6) removing impurities from tussah silk, rinsing, adding water, and soaking for 50min at a bath ratio of 15: 1; then dehydrating and finishing cleaning; degumming the cleaned silk at high temperature and high pressure; after degumming, discharging the degumming silk cellulose solution from the reaction kettle; the pressure of high-temperature high-pressure degumming is 0.25MPa, the temperature is 130 ℃, and the degumming time is 16 minutes; the mass concentration of the degummed tussah silk fibroin fiber solution is 75 percent; adding trimethylsilanol into the degummed tussah silk fibroin fiber solution, carrying out conventional ultrasonic treatment for 2.5 hours, and then dehydrating and drying in the sun to obtain treated tussah silk; preparing the processed tussah silk into tussah silk cotton sheets by adopting a conventional method (silk wadding quilt knowledge);
(7) combining the expanded dry mulberry silk cotton sheets with the tussah silk cotton sheets, and sewing by adopting a conventional method to obtain the expanded silk cotton quilt based on the mulberry silk, wherein the combination is that the expanded dry mulberry silk cotton sheets and the tussah silk cotton sheets are stacked at intervals, and referring to the attached figure 1, wherein 1 is the expanded dry mulberry silk cotton sheets, and 2 is the tussah silk cotton sheets; the volume ratio of the expanded dry silk cotton sheet to the tussah silk cotton sheet is 100: 18, and the volume is the total volume.
The mulberry silk fiber prepared by the invention and single fiber void ratio and diameter are measured and compared with common silk, and the results are shown in the following table:
in the prepared expanded filament, the single fiber void ratio is 23.33 percent without adding the polyureaformaldehyde; and (3) directly preparing a silk floss sheet without preparing the silk with holes, wherein in the prepared expanded silk floss quilt, the single fiber void ratio is 26.66%.
In addition, the mechanical properties of silk were also measured and the results are shown in the following table:
as seen from the above table, the obtained expanded silk has higher breaking strength than common tussah silk, and is higher than mulberry silk; the core technology for developing the porous mulberry silk is realized through the crosslinking action of the polyethylene glycol and the curcuma extract, silk fibers are high in elasticity, the initial modulus is an indirect index for measuring the softness of the silk fibers, and the fact that the expanded mulberry silk disclosed by the invention is easy to deform and has better softness than common silk is shown. The breaking strength is 1.6 CN/dtex without adding amino polyethylene glycol; the breaking strength is 1.7 CN/dtex without adding selenocysteine hydrochloride, the bacteriostasis rate of the prepared swelling dry mulberry silk cotton sheet is 95.86 percent, and the bacteriostasis rate of the tussah silk cotton sheet is 72.26 percent.
The common tussah silk is not treated by trimethylsilanol, and the mechanical property of the tussah silk is basically not influenced by the trimethylsilanol treatment; before and after trimethylsilanol treatment, the water contact angles of the tussah silk cotton piece are 135.8 degrees and 156.6 degrees respectively.
Meanwhile, the wearability of the silk floss quilt prepared by the invention is also considered and compared with the common tussah silk, and the result is shown in the following table:
if the mixture is dried at 105 ℃ for 3 minutes, the bulk is 45 cm3(ii)/g; if no tussah silk cotton piece is added, the heat transfer coefficient is 0.923w/m2DEG C; the table shows that the porous mulberry silk floss quilt has better bulkiness and heat preservation rate than the common tussah silk floss quilt, the bacteriostasis rate is greatly improved, the strength of the silk floss sheet prepared from the expanded mulberry silk is improved by adding the tussah silk floss sheet, the shape retention rate of the silk floss quilt for 24 hours is improved by 70% by adding 35% of the tussah silk floss sheet, no organic volatile matter is detected, the wearability is greatly improved, and the porous mulberry silk floss quilt has remarkable progress.
Claims (2)
1. A preparation method of an expanded silk wadding quilt based on mulberry silk comprises the following steps:
(1) degumming the cleaned mulberry silk at high temperature and high pressure to obtain a degummed mulberry silk cellulose fiber solution; the pressure of the high-temperature high-pressure degumming is 0.1-0.2 MPa, the temperature is 110-135 ℃, and the degumming time is 6-8 minutes;
(2) adding a mixed solution of a turmeric extract, acetic acid and carboxymethyl cellulose into a degummed mulberry silk cellulose fiber solution, carrying out ultrasonic treatment for 2-3 hours, adding polyurea formaldehyde and selenocysteine hydrochloride, and carrying out ultrasonic treatment for 1-1.5 hours; then dehydrating and drying in the sun to obtain the processed mulberry silk; the mass ratio of the degummed mulberry silk cellulose fiber, the turmeric extract, the acetic acid, the carboxymethyl cellulose, the polyurea formaldehyde and the selenocysteine hydrochloride is 100: 5: 4: 5: 2;
the chemical structural formula of the selenocysteine hydrochloride is as follows:
(3) heating the processed mulberry silk at 160 ℃ for 40 seconds, and then heating at 200 ℃ for 25 seconds to obtain the mulberry silk with holes; preparing mulberry silk with holes into a mulberry silk floss sheet, and then soaking the mulberry silk floss sheet into an amino polyethylene glycol aqueous solution to obtain a treated mulberry silk floss sheet; the mass ratio of the mulberry silk floss piece to the amino polyethylene glycol is 100: 6;
(4) placing the processed mulberry silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain a swelling wet mulberry silk floss sheet; when puffing, the saturated steam pressure in the closed container is 0.08 Mpa; the closed container rotates at 12 r/min; when the saturated steam pressure in the closed container is increased to 0.5Mpa, the rupture disk is ruptured;
(5) dehydrating the expanded wet mulberry silk floss sheet, manually loosening the sheet, and drying the sheet to obtain an expanded dry mulberry silk floss sheet;
(6) degumming the washed tussah silk at high temperature and high pressure to obtain a degummed tussah silk fibroin fiber solution; adding trimethylsilanol into the degummed tussah silk fibroin fiber solution, carrying out ultrasonic treatment for 2-3 hours, and then dehydrating and drying in the sun to obtain the treated tussah silk; preparing the treated tussah silk into a tussah silk cotton sheet; the mass ratio of the degummed tussah silk fibroin fiber to the trimethylsilanol is 100: 18;
(7) combining and sewing the expanded dry mulberry silk floss piece and the tussah silk floss piece to obtain the expanded silk floss quilt based on the mulberry silk;
in the step (2), the mass concentration of the degummed mulberry silk cellulose fiber solution is 55-62%;
in the step (5), the drying is carried out for 25 seconds at 185 ℃ and then 135 seconds at 105 ℃;
in the step (6), the pressure of the high-temperature high-pressure degumming is 0.15-0.3 MPa, the temperature is 110-135 ℃, and the degumming time is 10-20 minutes; the mass concentration of the degummed tussah silk fibroin fiber solution is 75-78%;
in the step (7), the volume ratio of the expanded dry mulberry silk floss piece to the tussah silk floss piece is 100: 35.
2. The preparation method according to claim 1, wherein in the step (1), mulberry silk is used as a raw material, after impurity removal and rinsing, water is added to soak for at least 30min, the bath ratio is 10-20: 1, and then dehydration is carried out to complete cleaning; in the step (6), tussah silk is used as a raw material, impurities are removed, rinsing is carried out, water is added to soak for at least 30min, the bath ratio is 10-20: 1, and then dehydration is carried out to finish cleaning.
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| CN101543366A (en) * | 2009-04-27 | 2009-09-30 | 苏州大学 | Porous and bulked tussah silk floss quilt and preparation method thereof |
| CN104073907A (en) * | 2014-06-06 | 2014-10-01 | 江苏鹰翔化纤股份有限公司 | Polyester fiber and preparation method thereof |
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| CN107083569B (en) * | 2017-05-10 | 2018-07-10 | 安徽三利丝绸集团有限公司 | A kind of high-quality processing and treating method of mulberry silk |
| CN108085973B (en) * | 2018-01-13 | 2020-04-28 | 广州多美生物科技有限公司 | Freckle-removing silk mask with high water retention property |
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| CN101543366A (en) * | 2009-04-27 | 2009-09-30 | 苏州大学 | Porous and bulked tussah silk floss quilt and preparation method thereof |
| CN104073907A (en) * | 2014-06-06 | 2014-10-01 | 江苏鹰翔化纤股份有限公司 | Polyester fiber and preparation method thereof |
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