CN109730497A - 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 a kind of expansion silk wadding quilt and preparation method thereof based on mulberry silk, include the following steps: for the mixed solution of Turmeric P.E, acetic acid and carboxymethyl cellulose to be added in degumming fibroin fiber solution, ultrasonic treatment, adds uramit, selenocystamine hydrochloride, is ultrasonically treated；Amino-polyethyleneglycols aqueous solution is impregnated after silk with holes is prepared into silk floss sheet, obtains processing silk floss sheet；Processing silk floss sheet is put into equipped with extruding is carried out in the rotatable closed container of rupture disk, obtains expanding wet silk floss sheet；It will be dried after wet silk floss sheet dehydration, manual garnetting will be expanded, obtains the expansion dry silk floss sheet of silkworm；Dry mulberry silk piece will be expanded to combine, sew with processing tussah silk cotton piece, obtain expansion silk wadding quilt.The present invention is successfully prepared the excellent porous varicosity silk floss sheet of wearability, and has good antibiotic property, has the positive effect of reality.
Description
Technical field
The present invention relates to a kind of preparation methods of silk floss, and in particular to a kind of expansion silk wadding quilt and its system based on mulberry silk
Preparation Method.
Background technique
As the improvement of people's living standards, people increasingly advocate back to nature, the dosage of pure natural silk wadding quilt increases severely,
Consumption market expands year by year.The raw material of silk wadding quilt is various silks, wherein the silk wadding quilt made of porous varicosity silk is than common
Silk wadding quilt has the wearability such as superior elasticity, warmth retention property, softness.Porous varicosity silk refers to inside silk fiber with more
The silk of pore structure can save a large amount of static sky since the porous structure can form the short space of many stored airs
Gas, therefore there is good warmth retention property, and gas permeability, penetrability are good, it gets the attention and increasingly in-depth study.
Mulberry silk is soft, widely applies preparing silk wadding quilt field, but its poor mechanical property, after especially expanding,
Therefore the prior art is almost without the report about porous expansion mulberry silk.
Existing expansion thread preparation method is ineffective, needs not meeting environmentally protective master using a large amount of chemical reagent
Topic.Therefore, a kind of expansion silk wadding quilt and preparation method thereof is developed, there is the positive effect of reality.
Summary of the invention
The object of the present invention is to provide a kind of expansion silk wadding quilt and preparation method thereof based on mulberry silk, it is excellent to obtain performance
Good expansion silk wadding quilt.
To achieve the above object of the invention, the technical solution adopted by the present invention is that:
A kind of expansion silk wadding quilt based on mulberry silk, which is characterized in that the preparation side of the expansion silk wadding quilt based on mulberry silk
Method includes the following steps:
(1) mulberry silk after cleaning is subjected to high temperature and pressure degumming, obtains degummed mulberry silk cellulose fiber solution；
(2) mixed solution of Turmeric P.E, acetic acid and carboxymethyl cellulose is added in degummed mulberry silk cellulose fiber solution,
Ultrasonic treatment 2~3 hours adds uramit, selenocystamine hydrochloride, is ultrasonically treated 1~1.5 hour；Then it is dehydrated, shines
It is dry, obtain processing mulberry silk；
The chemical structural formula of the selenocystamine hydrochloride is as follows:
(3) processing mulberry silk is heated 40 seconds in 160 DEG C, is then heated 25 seconds in 200 DEG C, obtains mulberry silk with holes；It will be with holes
Mulberry silk impregnates amino-polyethyleneglycols aqueous solution after being prepared into mulberry silk piece, obtains processing mulberry silk piece；
(4) processing mulberry silk floss sheet is put into equipped with extruding is carried out in the rotatable closed container of rupture disk, obtains expansion watered mulberry leaf silkworm
Silk floss sheet；
(5) it will be dried after wet mulberry silk piece dehydration, manual garnetting will be expanded, obtains expanding dry mulberry silk piece；
(6) tussah silk after cleaning is subjected to high temperature and pressure degumming, obtains degumming tussah silk peptide fiber solution；Then by front three
Base silanol is added in degumming tussah silk peptide fiber solution, is ultrasonically treated 2~3 hours, is then dehydrated, dries, and obtains processing tussah
Silk；Processing tussah silk is prepared into tussah silk cotton piece；
(7) dry mulberry silk piece will be expanded to combine, sew with tussah silk cotton piece, obtain the expansion silk wadding quilt based on mulberry silk.
A kind of preparation method of the expansion silk wadding quilt based on mulberry silk, includes the following steps:
(1) mulberry silk after cleaning is subjected to high temperature and pressure degumming, obtains degummed mulberry silk cellulose fiber solution；
(2) mixed solution of Turmeric P.E, acetic acid and carboxymethyl cellulose is added in degummed mulberry silk cellulose fiber solution,
Ultrasonic treatment 2~3 hours adds uramit, selenocystamine hydrochloride, is ultrasonically treated 1~1.5 hour；Then it is dehydrated, shines
It is dry, obtain processing mulberry silk；
The chemical structural formula of the selenocystamine hydrochloride is as follows:
(3) processing mulberry silk is heated 40 seconds in 160 DEG C, is then heated 25 seconds in 200 DEG C, obtains mulberry silk with holes；It will be with holes
Mulberry silk impregnates amino-polyethyleneglycols aqueous solution after being prepared into mulberry silk piece, obtains processing mulberry silk piece；
(4) processing mulberry silk floss sheet is put into equipped with extruding is carried out in the rotatable closed container of rupture disk, obtains expansion watered mulberry leaf silkworm
Silk floss sheet；
(5) it will be dried after wet mulberry silk piece dehydration, manual garnetting will be expanded, obtains expanding dry mulberry silk piece；
(6) tussah silk after cleaning is subjected to high temperature and pressure degumming, obtains degumming tussah silk peptide fiber solution；Then by front three
Base silanol is added in degumming tussah silk peptide fiber solution, is ultrasonically treated 2~3 hours, is then dehydrated, dries, and obtains processing tussah
Silk；Processing tussah silk is prepared into tussah silk cotton piece；
(7) dry mulberry silk piece will be expanded to combine, sew with tussah silk cotton piece, obtain the expansion silk wadding quilt based on mulberry silk.
In above-mentioned technical proposal, in step (1), the pressure of the high temperature and pressure degumming is 0.1~0.2MPa, and temperature is
110~135 DEG C, usually time is 6~8 minutes；In step (6), the pressure of the high temperature and pressure degumming is 0.15~0.3MPa,
Temperature is 110~135 DEG C, and usually time is 10~20 minutes.
In above-mentioned technical proposal, in step (1), using mulberry silk as raw material, after removal of impurities, rinsing, water is added and impregnates at least
30min, bath raio are 10~20: 1, are then dehydrated, complete cleaning；In step (6), using tussah silk as raw material, after removal of impurities, rinsing,
Water is added and impregnates at least 30min, bath raio is 10~20: 1, is then dehydrated, completes cleaning.
In above-mentioned technical proposal, in step (2), degummed mulberry silk cellulose fiber, Turmeric P.E, acetic acid, carboxymethyl cellulose
Element, uramit, selenocystamine hydrochloride mass ratio be 100: 5: 5: 4: 5: 2；In step (6), degumming tussah silk peptide fiber,
The mass ratio of trimethyl silanol is 100: 18.
In above-mentioned technical proposal, in step (2), the mass concentration of the degummed mulberry silk cellulose fiber solution is 55~62%；
In step (6), the mass concentration of the degumming tussah silk peptide fiber solution is 75~78%.Reagent treatment and fibroin can be improved
The reactivity of fiber.
In above-mentioned technical proposal, in step (3), mulberry silk piece, amino-polyethyleneglycols mass ratio be 100: 6, not only
So that silk floss sheet is soft and smooth, affine, mainly to be in that hole is uniform when expansion, hole is avoided to cross fast diffusion.
In above-mentioned technical proposal, in step (4), when carrying out extruding, the saturation vapor pressure in closed container is
0.08Mpa；Closed container is rotated with 12 revs/min；Rupture disk is broken when saturation vapor pressure in closed container rises to 0.5Mpa
It splits.
In above-mentioned technical proposal, in step (5), dry in 185 DEG C dry 25 seconds after then at 105 DEG C dry 135 seconds；First with compared with
High-temperature expands the hole of silk floss sheet, and then low temperature removes moisture content, has both reached drying effect, has in turn avoided organic volatile
Residual, and improve silk wadding quilt bulkiness.
In above-mentioned technical proposal, trimethyl silanol improves the surface property of tussah silk as modified component, such as hydrophobic；This
Inorganic agent is added in fibroin fiber solution for invention, and process uniformity and stability can be improved；It can be improved using drying
Inorganic agent avoids directly drying the dry uneven problem of caused reaction in the reaction uniformity on mulberry silk surface.
The invention also discloses the expansion silk wadding quilts based on mulberry silk obtained according to above-mentioned preparation method；Expand dry silkworm
The volume ratio of silk floss sheet and tussah silk cotton piece is 100: 18, and mulberry silk can increase the gap of silk wadding quilt, while provide good
Heat preservation, but its mechanical property is relatively low, can be mended using the physical action between tussah silk cotton piece and the dry mulberry silk piece of expansion
By force, group is combined into the dry mulberry silk piece of expansion and tussah silk cotton piece stacked spaced apart, and preferably first layer and the last layer is all that expansion is dry
Mulberry silk piece.
Above, the effect of the step (2) is to form coating on silk surface, makes it have antibiotic property heat preservation, is one
The method that kind uses natural green antibacterial agent；Turmeric P.E can be improved in the carboxymethyl cellulose and other compounds exist
The adhesion on silk floss sheet surface.Uramit can provide porous performance, cooperate the place of selenocystamine hydrochloride and step (3)
Science and engineering skill can form certain aperture on fibroin fiber surface, and not influence the preparation and mechanical property of silk floss sheet, swollen
When swollen, pore and reaming are much better than pure expansion bring technical effect simultaneously, to obtain.Dosage is controlled, is on the one hand kept away
Exempt from the influence to fibre property, the excellent product of the available antibacterial of two aspects, mechanical property, porous performance.
Mulberry silk piece is put into equipped in the rotatable closed container of rupture disk by the present invention, and height is then passed through into container
Saturated steam is pressed, keeps its pressure by certain time, under the action of the saturated steam of high temperature and pressure, mulberry silk piece
Fibroin fiber start to be quickly converted to the extruding stage by swelling, when gas explosion occurs for unexpected decompression, tussah silk wadding piece moment is by high pressure
It is down to normal pressure state, promotes silk fiber to put aside energy and discharges suddenly, makes to generate porous structure inside silk fiber, therewith silk fiber
Extruding occurs, volume increases, to achieve the purpose that extruding.But prior art expanded porous will lead to mechanical property natively
Weak mulberry silk performance further declines, this is different with tussah silk, this be also it is existing it is rarely found mulberry silk is expanded it is more
The reason of hole is studied；The new expansion pore technique of one aspect of the present invention, two aspects use modifying agent, obtain expanded porous silkworm
Before silk mechanical property and non-pore quite.
Due to the adoption of the above technical solution, compared with prior art, the present invention has the advantage that
1. the present invention has the positive effect of reality, test proves that the porous varicosity mulberry silk wadding quilt that the present invention obtains has more preferable
Bulkiness and heat preservation rate, and bacteriostasis rate also improves a lot, and wearability is substantially improved.
2. preparation process adding raw materials safety of the present invention, advantageous to household products are prepared.
3. the present invention carries out silk at ultrasound in the mixed solution of Turmeric P.E, acetic acid and carboxymethyl cellulose
Reason, makes it have good antibiotic property, is a kind of method using natural green antibacterial agent.
4. the present invention is for the first time handled mulberry silk, make it have it is good show performance, while mulberry silk being kept to protect
Warm, fluffy advantage.
5. preparation method of the invention is simple and cost is relatively low, have a good application prospect.
Detailed description of the invention
Fig. 1 is to expand dry mulberry silk piece and tussah silk cotton piece combining structure schematic diagram；
Wherein, 1 is expands dry mulberry silk piece, and 2 be tussah silk cotton piece.
Specific embodiment
The present invention will be further described below with reference to examples:
Embodiment one
A kind of preparation method expanding silk wadding quilt, includes the following steps:
(1) using mulberry silk as raw material, after removal of impurities, rinsing, water is added and impregnates 50min, bath raio 15: 1；Then it is dehydrated, completes clear
It washes；Silk after cleaning is subjected to high temperature and pressure degumming；After degumming, degumming fibroin fiber solution is released from reaction kettle；High temperature
The pressure of high pressure degumming is 0.15MPa, and temperature is 118 DEG C, and usually time is 8 minutes；The matter of degummed mulberry silk cellulose fiber solution
Measuring concentration is 58%；
(2) degummed mulberry silk cellulose fiber solution is added in the mixed solution of Turmeric P.E, acetic acid and carboxymethyl cellulose, surpassed
Sonication 2 hours, uramit, selenocystamine hydrochloride are added, is ultrasonically treated 1 hour；Then it is dehydrated, dries, obtain everywhere
Manage mulberry silk；Degumming fibroin fiber, Turmeric P.E, acetic acid, carboxymethyl cellulose, uramit, selenocystamine hydrochloride
Mass ratio is 100: 5: 5: 4: 5: 2；
The chemical structural formula of the selenocystamine hydrochloride (CAS 3542-13-0) is as follows:
(3) processing mulberry silk is heated 40 seconds in 160 DEG C, is then heated 25 seconds in 200 DEG C, obtains silk with holes；By silkworm with holes
Silk impregnates amino-polyethyleneglycols aqueous solution after being prepared into mulberry silk piece using conventional method, obtains processing mulberry silk piece；Mulberry
Silkworm silk floss sheet, amino-polyethyleneglycols mass ratio be 100: 6；
(4) processing mulberry silk piece is put into equipped with extruding is carried out in the rotatable closed container of rupture disk, obtains expanding wet silk
Cotton quilt；When carrying out extruding, the saturation vapor pressure in closed container is 0.08Mpa；Closed container is rotated with 12 revs/min；It is close
Rupture disk ruptures when the saturation vapor pressure closed in container rises to 0.5Mpa；The explosion being equipped in the explosion lid of closed container
Film rupture, silk floss sheet moment depressurize suddenly, and gas explosion occurs, goes out explosion mouth therewith, make mulberry silk that extruding occur with silk fiber and are in
It is existing porous；
(5) it will be dried after wet silk floss sheet dehydration, manual garnetting will be expanded, obtains expanding dry mulberry silk piece；Drying is in 185 DEG C
It is dried 135 seconds after drying 25 seconds then at 105 DEG C；
(6) by after tussah silk removal of impurities, rinsing, water is added and impregnates 50min, bath raio 15: 1；Then it is dehydrated, completes cleaning；It will be clear
Silk after washing carries out high temperature and pressure degumming；After degumming, degumming fibroin fiber solution is released from reaction kettle；High temperature and pressure degumming
Pressure be 0.25MPa, temperature be 130 DEG C, usually time be 16 minutes；The mass concentration of degumming tussah silk peptide fiber solution is
75%；Then trimethyl silanol being added in degumming tussah silk peptide fiber solution, conventional Ultrasound is handled 2.5 hours, be then dehydrated,
It dries, obtains processing tussah silk；Conventional method (silk wadding quilt knowledge) is used to be prepared into tussah silk cotton piece processing tussah silk；
(7) dry mulberry silk piece will be expanded to combine with tussah silk cotton piece, sew using conventional method, obtained based on mulberry silk
Silk wadding quilt is expanded, wherein group is combined into the dry mulberry silk piece of expansion and tussah silk cotton piece stacked spaced apart, with reference to attached drawing 1, wherein 1 is swollen
Swollen dry mulberry silk piece, 2 are tussah silk cotton piece；The volume ratio for expanding dry mulberry silk piece and tussah silk cotton piece is 100: 18, body
Product is total volume.
Mulberry silk fiber and single fiber voidage prepared by the present invention, measuring diameter, and compared with common silk,
As a result as shown in the table:
It is added without uramit, in the expansion thread of preparation, single fiber voidage 23.33%；It is straight that step (3) does not prepare silk with holes
It connects and prepares silk floss sheet, in the expansion silk wadding quilt of preparation, single fiber voidage 26.66%.
In addition, the mechanical property of silk also measured were, as a result as shown in the table:
From upper table as it can be seen that the obtained expansion silk of the present invention is higher than the breaking strength of common tussah silk, more it is higher than mulberry silk；
Due to polyethylene glycol and Turmeric P.E crosslinked action, this is to develop the core technology of porous mulberry silk, and silk fiber is rich
There is high resiliency, initial modulus is the indirect indexes for measuring silk fiber flexibility, illustrates that present invention expansion mulberry silk is easy to happen change
Shape has better flexibility than common silk.Amino-polyethyleneglycols are added without, breaking strength is 1.6 CN/dtex；It is added without
Selenocystamine hydrochloride, breaking strength are 1.7 CN/dtex, and the dry mulberry silk piece bacteriostasis rate of the expansion of preparation is 95.86%, toothed oak
Silk cotton piece bacteriostasis rate is 72.26%.
Common tussah silk is without the tussah silk by trimethyl silanol processing, and trimethyl silanol processing is for tussah silk power
Learn performance does not influence substantially；Trimethyl silanol before and after the processing, the water contact angle of tussah silk cotton piece is respectively 135.8 °,
156.6°。
The wearability of silk wadding quilt prepared by the present invention has also been investigated simultaneously, and has been compared with common tussah silk, has been tied
Fruit is as shown in the table:
If dried 3 minutes when drying using 105 DEG C, fluffy degree is 45 cm3/g；If being added without tussah silk cotton piece, heat transfer coefficient
For 0.923w/m2. ℃；From upper table as it can be seen that porous mulberry silk quilt of the invention than common tussah silk floss quilt have preferably it is bulk
Degree and heat preservation rate, and bacteriostasis rate also improves a lot, and the addition of tussah silk cotton piece improves expansion mulberry silk preparation
The intensity of silk floss sheet, the addition of 35% tussah silk cotton piece is so that 24 hours shape conservation rates of silk wadding quilt improve 70%, and do not examine
Organic volatile out, wearability are substantially improved, and have significant progress.
Claims (10)
1. a kind of expansion silk wadding quilt based on mulberry silk, which is characterized in that the preparation of the expansion silk wadding quilt based on mulberry silk
Method includes the following steps:
(1) mulberry silk after cleaning is subjected to high temperature and pressure degumming, obtains degummed mulberry silk cellulose fiber solution；
(2) mixed solution of Turmeric P.E, acetic acid and carboxymethyl cellulose is added in degummed mulberry silk cellulose fiber solution,
Ultrasonic treatment 2~3 hours adds uramit, selenocystamine hydrochloride, is ultrasonically treated 1~1.5 hour；Then it is dehydrated, shines
It is dry, obtain processing mulberry silk；
The chemical structural formula of the selenocystamine hydrochloride is as follows:
(3) processing mulberry silk is heated 40 seconds in 160 DEG C, is then heated 25 seconds in 200 DEG C, obtains mulberry silk with holes；It will be with holes
Mulberry silk impregnates amino-polyethyleneglycols aqueous solution after being prepared into mulberry silk piece, obtains processing mulberry silk piece；
(4) processing mulberry silk floss sheet is put into equipped with extruding is carried out in the rotatable closed container of rupture disk, obtains expansion watered mulberry leaf silkworm
Silk floss sheet；
(5) it will be dried after wet mulberry silk piece dehydration, manual garnetting will be expanded, obtains expanding dry mulberry silk piece；
(6) tussah silk after cleaning is subjected to high temperature and pressure degumming, obtains degumming tussah silk peptide fiber solution；Then by front three
Base silanol is added in degumming tussah silk peptide fiber solution, is ultrasonically treated 2~3 hours, is then dehydrated, dries, and obtains processing tussah
Silk；Processing tussah silk is prepared into tussah silk cotton piece；
(7) dry mulberry silk piece will be expanded to combine, sew with tussah silk cotton piece, obtain the expansion silk wadding quilt based on mulberry silk.
2. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that in step (1), the high temperature is high
The pressure of pressure-off glue is 0.1~0.2MPa, and temperature is 110~135 DEG C, and usually time is 6~8 minutes；It is described in step (6)
The pressure of high temperature and pressure degumming is 0.15~0.3MPa, and temperature is 110~135 DEG C, and usually time is 10~20 minutes.
3. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that in step (1), be with mulberry silk
Raw material after removal of impurities, rinsing, is added water and impregnates at least 30min, and bath raio is 10~20: 1, is then dehydrated, completes cleaning；Step (6)
In, using tussah silk as raw material, after removal of impurities, rinsing, water is added and impregnates at least 30min, bath raio is 10~20: 1, is then dehydrated, complete
At cleaning.
4. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that in step (2), degummed mulberry silk
Cellulose fiber, Turmeric P.E, acetic acid, carboxymethyl cellulose, uramit, selenocystamine hydrochloride mass ratio be 100: 5: 5:
4:5:2；In step (6), degumming tussah silk peptide fiber, trimethyl silanol mass ratio be 100: 18.
5. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that in step (2), the degumming mulberry
The mass concentration of silk cellulose fiber solution is 55~62%；In step (6), the quality of the degumming tussah silk peptide fiber solution is dense
Degree is 75~78%.
6. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that in step (3), mulberry silk
Piece, amino-polyethyleneglycols mass ratio be 100: 6.
7. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that in step (4), carry out extruding
When, the saturation vapor pressure in closed container is 0.08Mpa；Closed container is rotated with 12 revs/min；Saturation in closed container
Rupture disk ruptures when water vapour pressure rises to 0.5Mpa.
8. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that in step (5), dry in
185 DEG C dry 25 seconds after then at 105 DEG C dry 135 seconds.
9. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that expand dry mulberry silk piece and toothed oak
The volume ratio of silk cotton piece is 100: 18.
10. the expansion silk wadding quilt based on mulberry silk according to claim 1, which is characterized in that group is combined into the dry mulberry silk of expansion
Continuous piece and tussah silk cotton piece stacked spaced apart.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110820333A (en) * | 2019-11-19 | 2020-02-21 | 河南民兴生物科技股份有限公司 | Preparation method for improving tussah silk fiber strength |
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| CN110820333A (en) * | 2019-11-19 | 2020-02-21 | 河南民兴生物科技股份有限公司 | Preparation method for improving tussah silk fiber strength |
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