CN109023931B - Flame-retardant expanded silk floss sheet and preparation method thereof - Google Patents
Flame-retardant expanded silk floss sheet and preparation method thereof Download PDFInfo
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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Abstract
The invention discloses a flame-retardant expanded silk floss sheet and a preparation method thereof, wherein the preparation method comprises the following steps: (1) degumming the cleaned silk at high temperature and high pressure to obtain a degummed fibroin fiber solution; (2) adding mixed solution of Curcuma rhizome extract, acetic acid and carboxymethyl cellulose into degummed fibroin fiber solution, performing ultrasonic treatment, adding polyurea formaldehyde, selenocysteine hydrochloride and cyclotripolyphosphate, performing ultrasonic treatment, adding sucrose, and performing ultrasonic treatment; then dehydrating and drying in the sun to obtain the treated silk; (3) heating the treated silk at 180 ℃ for 30 seconds, and then heating at 210 ℃ for 20 seconds to obtain the silk with holes; 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; (4) and (3) putting the treated silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain the flame-retardant expanded silk floss sheet. The invention successfully prepares the porous bulked tussah silk floss sheet with excellent wearability, has good antibacterial property and flame retardance, and has practical positive significance.
Description
Technical Field
The invention relates to a preparation method of silk floss, in particular to a flame-retardant expanded silk floss sheet 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 foreign research on porous bulked real silk begins in the eighties of the last century, and the processing method mainly comprises two types of bulking treatment and dividing filament yarn, wherein the bulking treatment is carried out on common raw silk by using a medicament, and the dividing filament yarn is carried out by changing the process and the method in the silk reeling process so as to achieve the purpose of bulking the real silk. For example, Chinese invention patent CN1059248C discloses a method for producing bulk elastic silk, which combines silk twisted in different directions with silk not twisted, and puts the combined silk into concentrated calcium salt solution for salt condensation treatment, thereby successfully realizing the elasticity and expansion of silk.
However, the above preparation method is not effective; in addition, the preparation method needs to use a large amount of chemical reagents, and does not meet the theme of green environmental protection. Therefore, the development of the flame-retardant expanded silk floss sheet and the preparation method thereof have practical positive significance.
Disclosure of Invention
The invention aims to provide a flame-retardant expanded silk floss sheet and a preparation method thereof, so as to obtain the flame-retardant expanded silk floss sheet with excellent performance.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of a flame-retardant expanded silk floss sheet comprises the following steps:
(1) degumming the cleaned silk at high temperature and high pressure to obtain a degummed fibroin fiber solution;
(2) adding a mixed solution of a turmeric extract, acetic acid and carboxymethyl cellulose into a degummed fibroin fiber solution, carrying out ultrasonic treatment for 2-3 hours, adding polyurea formaldehyde, selenocysteine hydrochloride and cyclotripolyphosphate, carrying out ultrasonic treatment for 0.5-1 hour, adding sucrose, and carrying out ultrasonic treatment for 0.5-1 hour; then dehydrating and drying in the sun to obtain the treated silk;
the chemical structural formula of the selenocysteine hydrochloride is as follows:
(3) heating the treated silk at 180 ℃ for 30 seconds, and then heating at 210 ℃ for 20 seconds to obtain the silk with holes; 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;
(4) and (3) putting the treated silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain the flame-retardant expanded silk floss sheet.
In the technical scheme, 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, silk is used as a raw material, impurities are removed, rinsing is carried out, and water is added for soaking for at least 30min, wherein the bath ratio is 10-20: 1; then dehydrating and finishing the cleaning.
In the technical scheme, the mass ratio of the degummed fibroin fiber, the turmeric extract, the acetic acid, the carboxymethyl cellulose, the polyurea formaldehyde, the selenocysteine hydrochloride, the cyclotripolyphosphate and the sucrose is 100: 15: 5: 10: 11: 7: 6: 2. The cyclotripolyphosphate and the sucrose are existing products, and can provide good flame retardance and certain antibacterial ability.
In the technical scheme, the mass concentration of the degummed silk fibroin fiber solution is 75-78%, and the reactivity of the treatment reagent and the silk fibroin fiber can be improved.
In the technical scheme, the mass ratio of the silk floss sheet to the amino polyethylene glycol is 100: 15, 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, when the puffing is carried out, the saturated steam pressure in the closed container is 0.08 Mpa; the closed container rotates at 15 r/min; when the saturated steam pressure in the closed container is increased to 0.5Mpa, the rupture disk is ruptured.
The flame-retardant expanded silk floss sheet is obtained according to the preparation method.
As described above, the step (2) serves to form a coating layer on the surface of silk to impart antibacterial and flame-retardant properties, and is a method using a natural green antibacterial agent, and carboxymethyl cellulose can improve the adhesion of turmeric extract to the surface of a 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 working principle of the invention is as follows: the tussah silk floss sheet is put into a rotary closed container provided with a bursting membrane, then high-pressure saturated steam is introduced into the container, the pressure of the container is kept for a certain period of time, under the action of the high-temperature and high-pressure saturated steam, the silk fibroin of the tussah silk floss sheet begins to be rapidly converted into a swelling stage from swelling, when sudden pressure reduction occurs, the pressure of the tussah silk floss sheet is instantly reduced from high pressure to normal pressure, the energy accumulated in the silk fiber is promoted to be suddenly released, a porous structure is generated in the silk fiber, and the silk fiber is swelled and increased in volume, so that the purpose of swelling is achieved.
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 tussah 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 degumming process of the invention does not add any chemical raw materials or auxiliary agents, so the degumming waste liquid has little content of other impurities except sericin, thereby being beneficial to the purification and recovery of sericin and conforming to the theme of environmental protection.
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 preparation method is simple, has low cost and good application prospect.
Detailed Description
The invention is further described below with reference to the following examples:
example one
A preparation method of a flame-retardant expanded silk floss sheet comprises the following steps:
(1) taking tussah silk as a raw material, removing impurities, rinsing, adding water, and soaking for at least 30min at a bath ratio of 15: 1; then dehydrating and finishing cleaning; degumming the cleaned silk at high temperature and high pressure to obtain a degummed fibroin fiber solution; the pressure of high-temperature high-pressure degumming is 0.2MPa, the temperature is 125 ℃, and the degumming time is 15 minutes; the mass concentration of the degummed silk fibroin fiber solution is 75 percent;
(2) adding a mixed solution of turmeric extract, acetic acid and carboxymethyl cellulose into the degummed fibroin fiber solution, carrying out ultrasonic treatment for 2 hours, adding polyurea formaldehyde, selenocysteine hydrochloride and cyclotripolyphosphate, carrying out ultrasonic treatment for 0.5 hour, adding sucrose, and carrying out ultrasonic treatment for 1 hour; then dehydrating and drying in the sun to obtain the treated silk; the mass ratio of the degummed silk fiber, the turmeric extract, the acetic acid, the carboxymethyl cellulose, the polyurea formaldehyde, the selenocysteine hydrochloride, the cyclotripolyphosphate and the cane sugar is 100: 15: 5: 10: 11: 7: 6: 2;
the chemical structural formula of the selenocysteine hydrochloride is as follows:
(3) heating the treated silk at 180 ℃ for 30 seconds, and then heating at 210 ℃ for 20 seconds to obtain the silk with holes; preparing silk with holes into a silk floss sheet by a conventional method, and then soaking the silk floss sheet in an amino polyethylene glycol aqueous solution to obtain a treated silk floss sheet; the mass ratio of the silk floss sheet to the amino polyethylene glycol is 100: 15;
(4) placing the treated silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain a flame-retardant expanded silk floss sheet; when puffing, the saturated steam pressure in the closed container is 0.08 Mpa; the closed container rotates at 15 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 opening 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 opening, so that the silk is bulked and the silk fiber is porous.
The porosity and diameter of the silk fiber and single fiber prepared by the invention are measured and compared with the common tussah silk, and the results are shown in the following table:
| item | Silk fiber diameter (micrometer) measured from optical microscope | Longitudinal width of silk fiber (micrometer) measured by electron microscope | Single fiber void fraction (%) |
| The invention relates to an expanded silk | 38.28 | 43.98 | 38.78 |
| Common silk | 26.38 | 30.52 | 8.94 |
In the prepared flame-retardant expanded silk floss sheet, the single fiber void ratio is 26.12 percent without adding the polyureaformaldehyde; and (3) directly preparing the silk floss sheet without preparing the silk with holes, wherein the single fiber void ratio of the prepared flame-retardant expanded silk floss sheet is 29.02 percent.
In addition, the mechanical properties of tussah silk were also measured and the results are shown in the following table:
| item | Breaking strength (CN/dtex) | Elongation at Break (%) | Initial modulus (CN/dtex) |
| The invention relates to an expanded silk | 3.2 | 32.81 | 1.39 |
| Common tussah silk | 2.2 | 23.45 | 1.87 |
The results show that the obtained expanded silk has higher breaking strength than common tussah silk, the core technology for developing porous tussah silk is realized due to the crosslinking effect of polyethylene glycol and a turmeric extract, silk fiber is high in elasticity, and the initial modulus is an indirect index for measuring the softness of the silk fiber, so that the tussah silk is easy to deform and has better softness than the common tussah silk. The breaking strength is 2.8 CN/dtex without adding amino polyethylene glycol; the breaking strength is 2.9 CN/dtex without adding selenocysteine hydrochloride, the prepared quilt bacteriostasis rate is 92.08 percent, and the oxygen index of the silk floss piece is 25; no cyclotripolyphosphate and sucrose are added, and the oxygen index of the silk floss piece is 15; the oxygen index of the silk floss sheet of the invention is 30.
Meanwhile, the wearability of the silk floss quilt prepared by the silk floss piece prepared by the invention according to the conventional method is considered and compared with the common tussah silk, and the results are shown in the following table:
| item | The invention relates to a silk wadding quilt | Common tussah silk floss quilt |
| Elastic recovery (%) | 97.1 | 89.2 |
| Bulk (cm)3/g) | 40 | 26 |
| Coefficient of heat transfer (w/m)2. ℃) | 1.130 | 2.299 |
| Heat insulation Rate (%) | 93.98 | 81.95 |
| Bacteriostatic ratio (%) | 97.2 | 65.8 |
The porous tussah silk floss quilt has better bulkiness and heat preservation rate than the common tussah silk floss quilt, the antibacterial rate is greatly improved, the wearability is greatly improved, and the porous tussah silk floss quilt has remarkable progress.
Claims (6)
1. A preparation method of a flame-retardant expanded silk floss sheet is characterized by comprising the following steps:
(1) degumming the cleaned silk at high temperature and high pressure to obtain a degummed fibroin fiber solution;
(2) adding a mixed solution of a turmeric extract, acetic acid and carboxymethyl cellulose into a degummed fibroin fiber solution, carrying out ultrasonic treatment for 2-3 hours, adding polyurea formaldehyde, selenocysteine hydrochloride and cyclotripolyphosphate, carrying out ultrasonic treatment for 0.5-1 hour, adding sucrose, and carrying out ultrasonic treatment for 0.5-1 hour; then dehydrating and drying in the sun to obtain the treated silk;
the chemical structural formula of the selenocysteine hydrochloride is as follows:
(3) heating the treated silk at 180 ℃ for 30 seconds, and then heating at 210 ℃ for 20 seconds to obtain the silk with holes; 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;
(4) placing the treated silk floss sheet into a rotary closed container with a rupture membrane for swelling to obtain a flame-retardant expanded silk floss sheet;
the mass ratio of the degummed silk fiber, the turmeric extract, the acetic acid, the carboxymethyl cellulose, the polyurea formaldehyde, the selenocysteine hydrochloride, the cyclotripolyphosphate and the cane sugar is 100: 15: 5: 10: 11: 7: 6: 2; the mass concentration of the degummed silk fibroin fiber solution is 75-78%.
2. The preparation method according to claim 1, wherein 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.
3. The preparation method according to claim 1, wherein silk is used as a raw material, impurities are removed, rinsing is carried out, and then water is added to soak for at least 30min, wherein the bath ratio is 10-20: 1; then dehydrating and finishing the cleaning.
4. The method according to claim 1, wherein the mass ratio of the silk floss sheet to the aminopolyethylene glycol is 100: 15.
5. The method according to claim 1, wherein the pressure of saturated steam in the closed vessel is 0.08 MPa; the closed container rotates at 15 r/min; when the saturated steam pressure in the closed container is increased to 0.5Mpa, the rupture disk is ruptured.
6. A flame-retardant expanded silk floss sheet obtained by the production method according to claim 1.
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| CN201810990514.4A CN109023931B (en) | 2018-08-28 | 2018-08-28 | Flame-retardant expanded silk floss sheet and preparation method thereof |
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| CN109023931B true CN109023931B (en) | 2021-02-26 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342790A (en) * | 2001-07-26 | 2002-04-03 | 屈清辉 | Process and apparatus for removing sericin from silkworm cocoon |
| CN101543366A (en) * | 2009-04-27 | 2009-09-30 | 苏州大学 | Porous and bulked tussah silk floss quilt and preparation method thereof |
| CN102127862A (en) * | 2010-12-20 | 2011-07-20 | 南通那芙尔服饰有限公司 | Color 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 |
| CN104278336A (en) * | 2014-10-28 | 2015-01-14 | 南通那芙尔服饰有限公司 | Method for manufacturing bassinas silk quilt |
-
2018
- 2018-08-28 CN CN201810990514.4A patent/CN109023931B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342790A (en) * | 2001-07-26 | 2002-04-03 | 屈清辉 | Process and apparatus for removing sericin from silkworm cocoon |
| CN101543366A (en) * | 2009-04-27 | 2009-09-30 | 苏州大学 | Porous and bulked tussah silk floss quilt and preparation method thereof |
| CN102127862A (en) * | 2010-12-20 | 2011-07-20 | 南通那芙尔服饰有限公司 | Color 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 |
| CN104278336A (en) * | 2014-10-28 | 2015-01-14 | 南通那芙尔服饰有限公司 | Method for manufacturing bassinas silk quilt |
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