阅读说明：本技术 一种蚕丝绵的制备方法 (Preparation method of silk floss ) 是由 杨祖根 于 2021-07-30 设计创作，主要内容包括：本发明涉及一种蚕丝绵的制备方法,其包括将蚕茧置于中性溶液中进行脱胶,以及使脱胶后的蚕茧在活性酶及泡化碱的作用下进行发酵腐化。本发明通过脱胶工艺、发酵腐化工艺的设计,降低了对蚕丝绵的损伤,能够高效脱胶与有效去除蚕丝纤维的异味,使得制备得到的蚕丝绵具有强度好、蓬松度佳、光泽度好以及无异味的优点。(The invention relates to a preparation method of silk floss, which comprises the steps of placing silkworm cocoons into neutral solution for degumming and fermenting and decaying the degummed silkworm cocoons under the action of active enzyme and sodium silicate. According to the invention, through the design of the degumming process and the fermentation and decomposition process, the damage to the silk floss is reduced, the degumming can be carried out efficiently, and the peculiar smell of the silk fiber can be effectively removed, so that the prepared silk floss has the advantages of good strength, excellent bulkiness, good glossiness and no peculiar smell.)

1. A preparation method of silk floss is characterized by comprising the steps of putting silkworm cocoons into a neutral solution, cooking at a first temperature, and then preserving heat at a second temperature to degum the silkworm cocoons; then, fermenting and decaying the degummed silkworm cocoons under the action of active enzyme and sodium silicate;

wherein the neutral solution is an aqueous solution containing a surfactant, and the first temperature > the second temperature.

2. The method for producing silk floss according to claim 1, wherein the method comprises controlling the first temperature to 98 to 100 ℃ and/or the second temperature to 95 to 97 ℃ and/or the temperature of fermentation and decay to 40 to 45 ℃ under normal pressure.

3. The method for preparing silk floss according to claim 1 or 2, wherein the cooking time is controlled to be 20-40 min and/or the heat preservation time is controlled to be 1.5-2.5 h and/or the fermentation time is controlled to be 40-56 h.

4. The method for preparing silk floss of claim 1, wherein the surfactant comprises anionic surfactant and/or nonionic surfactant, and/or the anionic surfactant comprises one or more of sodium dioctyl sulfosuccinate, sodium dodecyl benzene sulfonate, sodium glycocholate, sodium lauryl sulfate, and sodium dodecyl sulfate; and/or the nonionic surfactant comprises one or more of alkyl glucoside, fatty glyceride, sorbitan fatty acid, polysorbate, polyoxyethylene polyoxypropylene.

5. The method for producing silk floss according to claim 4, wherein the surfactant comprises Pluronic F-127 and/or sodium glycocholate.

6. The method for preparing silk floss as claimed in claim 1, wherein the mass content of the surfactant in the neutral solution is 1.3-2%, and/or the mass ratio of the silkworm cocoon to the neutral solution is 1: (9-11).

7. The method for producing silk floss according to claim 1, wherein the active enzyme is neutral lipase.

8. The method for producing silk floss as claimed in claim 1 or 7, wherein the mass ratio of the active enzyme to the silkworm cocoon is (0.1-0.25): 1 and/or the feeding mass ratio of the sodium silicate to the silkworm cocoons is (0.15-0.3): 1.

9. the method for producing silk floss according to claim 1, further comprising a step of taking out the silk cocoon after the fermentation and decay step is completed, and beating, washing, dehydrating and drying the silk floss to obtain the silk floss; and/or the preparation method further comprises the step of filtering, removing impurities, centrifugally removing impurities, concentrating and freeze-drying the treatment liquid of the silkworm cocoons after the silkworm cocoons are degummed so as to obtain the finished fibroin product.

10. The method for preparing silk floss according to claim 1, wherein the method comprises the steps of:

(1) placing the silkworm cocoons in a neutral solution, cooking at the temperature of 98-100 ℃, and then preserving heat at the temperature of 95-97 ℃ to degum the silkworm cocoons, wherein the cooking time is controlled to be 20-40 min, and the heat preservation time is controlled to be 1.5-2.5 h;

(2) cooling the system in the step (1) to 40-45 ℃, and adding the active enzyme and the sodium silicate to ferment and decompose the degummed silkworm cocoons, wherein the mass ratio of the active enzyme to the silkworm cocoons is (0.1-0.25): 1. the feeding mass ratio of the sodium silicate to the silkworm cocoons is (0.15-0.3): 1, controlling the fermentation time to be 40-56 hours and the temperature to be 40-45 ℃;

(3) taking out the fermented and decayed silkworm cocoons, and performing cotton beating, washing, dewatering and drying to obtain the silk floss;

(4) and filtering the treated liquid after the silkworm cocoons are taken out to remove impurities, centrifugally removing the impurities, concentrating and freeze-drying to obtain a finished fibroin product.

Technical Field

The invention relates to a preparation method of silk floss.

Background

Silk is a fiber obtained by spinning and spinning silk liquid in a silkworm body and then solidifying the silk liquid. The silk is mainly composed of silk fibroin, sericin wrapped on the outer layer of the silk fibroin, pigment, oil wax and inorganic matters. In order to ensure the fluffiness, cleanness and softness of silk floss, most of impurities such as sericin, grease, wax and the like on the silk floss need to be removed.

Chinese patent CN200610050727.6 discloses elastic silk floss fiber is obtained by soaking silkworm cocoon in boiling soda solution, then opening cocoon, removing impurities, opening cotton, and high temperature steam touch steaming. Although this method can obtain a silk floss fiber having a certain elasticity, the use of soda ash reduces the glossiness and fiber strength of the silk floss fiber. Chinese patent CN201811085845.X utilizes immobilized microorganism strains to carry out fermentation deoiling and impurity removal treatment on mulberry silk byproducts, then utilizes the combination of hydrogen peroxide, percarbamide and alkaline ionic liquid to carry out degumming on the mulberry silk byproducts, then utilizes reagents such as hydrogen peroxide, TAED, sodium perborate and oxalic acid to bleach the degummed mulberry silk byproducts, and finally utilizes puffing liquid and finishing agent to carry out treatment to obtain the elastic fluffy silk floss. The method is also to degum under alkaline condition, which has certain damage to silk fiber, and in order to effectively remove oil and impurities, an additional alternating magnetic field needs to be applied in the fermentation process, the preparation process is complex, and the operation is difficult in the actual process.

Disclosure of Invention

The invention aims to solve the technical problem of providing a preparation method of silk floss, which has mild preparation conditions, simple steps and easy operation.

In order to achieve the purpose, the invention adopts the technical scheme that:

the invention provides a preparation method of silk floss, which comprises the steps of putting silkworm cocoons into neutral solution, cooking at a first temperature, and then preserving heat at a second temperature to degum the silkworm cocoons; then, fermenting and decaying the degummed silkworm cocoons under the action of active enzyme and sodium silicate;

wherein the neutral solution is an aqueous solution containing a surfactant, and the first temperature > the second temperature.

Preferably, the preparation method comprises the step of controlling the first temperature to be 98-100 ℃ under normal pressure.

Further preferably, the second temperature is controlled to be 95-97 ℃.

Still more preferably, the fermentation decomposition temperature is controlled to be 40-45 ℃.

Preferably, the cooking time is controlled to be 20-40 min, and further 25-35 min.

Further preferably, the heat preservation time is controlled to be 1.5-2.5 hours, and further to be 1.8-2.2 hours.

Further preferably, the fermentation time is controlled to be 40-56 hours, and further 45-51 hours.

Preferably, the surfactant comprises an anionic surfactant and/or a nonionic surfactant.

Further preferably, the anionic surfactant comprises one or more of sodium dioctyl succinate, sodium dodecyl benzene sulfonate, sodium glycocholate, sodium lauryl sulfate and sodium dodecyl sulfate.

Further preferably, the nonionic surfactant comprises one or more of alkyl glucoside, fatty acid glyceride, sorbitan fatty acid, polysorbate, polyoxyethylene polyoxypropylene.

Even more preferably, the surfactant comprises Pluronic F-127 and/or sodium hepatocholate.

Preferably, the mass content of the surfactant in the neutral solution is 1.3-2%.

Further preferably, when the surfactant is an anionic surfactant, the mass content of the surfactant in the neutral solution is 1.4-1.6%; when the surfactant is a nonionic surfactant, the mass content of the surfactant in the neutral solution is 1.8-2.0%.

Preferably, the feeding mass ratio of the silkworm cocoons to the neutral solution is 1: (9-11), further 1: (9.5-10.5).

Preferably, the active enzyme is a neutral lipase. The use of the active enzyme can not only shorten the fermentation time and improve the fermentation efficiency, but also effectively remove the grease components in the silkworm cocoons and the residual sericin which is not removed completely, so that the prepared silkworm silk floss has natural fragrance and no odor.

Further preferably, the feeding mass ratio of the active enzyme to the silkworm cocoons is (0.1-0.25): 1, further (0.1-0.2): 1, further (0.15 to 0.2): 1.

preferably, the feeding mass ratio of the sodium silicate to the silkworm cocoons is (0.15-0.3): 1, further (0.2-0.25): 1.

preferably, the preparation method further comprises the step of taking out the silkworm cocoons after the fermentation and the decay are finished, and then beating, washing, dehydrating and drying the silkworm cocoons to obtain the silk floss.

Further preferably, after the silkworm cocoons are degummed, the step of filtering and removing impurities, centrifuging and removing impurities, concentrating and freeze-drying the processing liquid of the silkworm cocoons to obtain the finished fibroin product.

According to some preferred embodiments, the preparation method comprises the steps of:

(1) placing the silkworm cocoons in a neutral solution, cooking at the temperature of 98-100 ℃, and then preserving heat at the temperature of 95-97 ℃ to degum the silkworm cocoons, wherein the cooking time is controlled to be 20-40 min, and the heat preservation time is controlled to be 1.5-2.5 h;

(2) cooling the system in the step (1) to 40-45 ℃, and adding the active enzyme and the sodium silicate to ferment and decompose the degummed silkworm cocoons, wherein the mass ratio of the active enzyme to the silkworm cocoons is (0.1-0.25): 1. the feeding mass ratio of the sodium silicate to the silkworm cocoons is (0.15-0.3): 1, controlling the fermentation time to be 40-56 hours and the temperature to be 40-45 ℃;

(3) taking out the fermented and decayed silkworm cocoons, and performing cotton beating, washing, dewatering and drying to obtain the silk floss;

(4) and filtering the treated liquid after the silkworm cocoons are taken out to remove impurities, centrifugally removing the impurities, concentrating and freeze-drying to obtain a finished fibroin product.

Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:

according to the invention, the neutral solution is adopted for degumming, so that the damage to silk fibers is reduced; through the design of the degumming process and the fermentation decomposition process, the degumming, degreasing and impurity removal can be carried out efficiently, so that the prepared silk floss has the advantages of good strength, excellent bulkiness, good glossiness and no peculiar smell;

the preparation method disclosed by the invention is simple in steps and strong in operability.

Detailed Description

The present invention will be further described with reference to the following examples. However, the present invention is not limited to the following examples. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions not mentioned are conventional conditions in the industry. The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.

The following examples and comparative examples were carried out under normal pressure without specific reference, and the opening, rinsing, dewatering and drying processes of the examples are conventional in the art.

The active enzymes referred to in the following examples and comparative examples are commercially available neutral lipases.

Example 1

(1) Taking silkworm cocoons for cocoon opening to remove silkworm chrysalis in the silkworm cocoons;

(2) placing silkworm cocoon (100 g) after cocoon opening in 1000g neutral aqueous solution, heating to 100 ℃, keeping 100 ℃ and boiling for 30min, then cooling to 96 ℃, and keeping the temperature for 2 hours to ensure that the fibroin is degummed and decomposed on the silkworm cocoon; wherein the neutral aqueous solution is prepared by dissolving 15g of Pluronic F-127 surfactant in 985g of water;

(3) cooling to 40-45 ℃, adding 15g of active enzyme and 20g of sodium silicate into the system in the step (2), and preserving heat for 48 hours to carry out fermentation and decomposition;

(4) after fermentation and decay are finished, silk fiber is drawn out, and silk floss can be obtained after opening, washing, dewatering and drying; filtering the solution with the silk fiber taken out, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain the fibroin.

In the present embodiment, when the silk fiber after fermentation and decay is drawn, the drawing is smooth, and the silk fiber is not broken, wherein, 2g of fibroin and 56g of silk floss are obtained in the present embodiment, the oil content of the silk floss is 1.4%, the color of the silk floss is milk white, and the silk floss has toughness, no peculiar smell, and good filling power when being torn.

Example 2

(1) Taking silkworm cocoons for cocoon opening to remove silkworm chrysalis in the silkworm cocoons;

(2) placing silkworm cocoon (total 100 g) after cocoon opening in 1000g neutral aqueous solution, heating to 100 ℃, keeping 100 ℃ and boiling for 30min, then cooling to 96 ℃, and keeping the temperature for 2 hours to ensure that the fibroin is degummed and decomposed on the silkworm cocoon; wherein the neutral aqueous solution is prepared by dissolving 20g of sodium glycocholate surfactant in 980g of water;

(3) cooling to 40-45 ℃, adding 20g of active enzyme and 20g of sodium silicate into the system in the step (2), and preserving heat for 48 hours to carry out fermentation and decomposition;

(4) after fermentation and decay are finished, silk fiber is drawn out, and silk floss can be obtained after opening, washing, dewatering and drying; filtering the solution with the silk fiber taken out, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain the fibroin.

In the present embodiment, when the silk fiber after fermentation and decay is drawn, the drawing is smooth, and the silk fiber is not broken, wherein, in the present embodiment, 1.6g of silk protein is obtained, 53g of silk floss, the oil content of the silk floss is 1.2%, the color of the silk floss is milk white, and the silk floss has toughness, no peculiar smell, and good bulkiness when being torn.

Comparative example 1

(1) Taking silkworm cocoons for cocoon opening to remove silkworm chrysalis in the silkworm cocoons;

(2) placing silkworm cocoon (100 g) after cocoon opening in 1000g neutral aqueous solution, heating to 100 ℃, keeping 100 ℃ and boiling for 30min, then cooling to 96 ℃, and keeping the temperature for 2 hours to ensure that the fibroin is degummed and decomposed on the silkworm cocoon; wherein the neutral aqueous solution is prepared by dissolving 15g of Pluronic F-127 surfactant in 985g of water;

(3) cooling to 40-45 ℃, drawing out silk fibers, and opening, washing, dehydrating and drying the silk fibers to obtain silk floss; filtering the solution with the silk fiber taken out, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain silk protein;

the silk fiber of this example is not smooth when being drawn, wherein, silk protein 1.5g, silk floss 60g are obtained in this example, the color and luster of silk floss is cream yellow, the oil content of silk floss is 2%, silk floss has peculiar smell, fluffy degree is poor, silk floss does not meet the raw material requirement of silk quilt.

Comparative example 2

(1) Taking silkworm cocoons for cocoon opening to remove silkworm chrysalis in the silkworm cocoons;

(2) placing silkworm cocoon (100 g) after cocoon opening in 1000g of aqueous alkali, heating to 100 ℃, keeping the temperature of 100 ℃ for boiling for 30min, then cooling to 96 ℃, and preserving the temperature for 2 hours to ensure that the fibroin is degummed and decomposed on the silkworm cocoon; wherein the alkali solution is prepared by dissolving 15g of sodium carbonate in 985g of water;

(3) cooling to 40-45 ℃, adding 15g of active enzyme and 20g of sodium silicate into the system in the step (2), and preserving heat for 48 hours to carry out fermentation and decomposition;

(4) after fermentation and decay are finished, silk fiber is drawn out, and silk floss can be obtained after opening, washing, dewatering and drying; filtering the solution with the silk fiber taken out, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain the fibroin.

In the present example, when silk fibers after fermentation and decay are subjected to wiredrawing, the wiredrawing is not smooth, and the silk fibers are broken, wherein 2.3g of silk protein and 50g of silk floss are obtained in the present example, the oil content of the silk floss is 1.05%, the color of the silk floss is milk white, and the toughness and the strength of the silk floss are poor.

Comparative example 3

(1) Taking silkworm cocoons for cocoon opening to remove silkworm chrysalis in the silkworm cocoons;

(2) placing the silkworm cocoon (100 g) after cocoon opening in 1000g of neutral aqueous solution, heating to 96 ℃, and preserving heat for 2.5 hours to ensure that the fibroin is degummed and decomposed on the silkworm cocoon; wherein the neutral aqueous solution is prepared by dissolving 15g of Pluronic F-127 surfactant in 985g of water;

(3) cooling to 40-45 ℃, adding 15g of active enzyme and 20g of sodium silicate into the system in the step (2), and preserving heat for 48 hours to carry out fermentation and decomposition;

(4) after fermentation and decay are finished, silk fiber is drawn out, and silk floss can be obtained after opening, washing, dewatering and drying; filtering the solution with the silk fiber taken out, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain the fibroin.

When the silk fiber after fermentation and decay is subjected to wire drawing, the wire drawing is not smooth, and the silk fiber has viscosity and is easy to wind; in the example, 1.3g of silk fibroin and 58g of silk floss with oil content of 1.6% are obtained, the color of the silk floss is cream yellow, the silk floss has no peculiar smell but poor filling power, and the produced silk floss does not meet the requirements of raw materials of the silk quilt.

The present invention has been described in detail in order to enable those skilled in the art to understand the invention and to practice it, and it is not intended to limit the scope of the invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the present invention.