A fragrance-releasing silk quilt inner tube and a preparation method thereof

Abstract

The present application belongs to the field of silk weaving, and particularly relates to a fragrance-releasing silk quilt inner and a preparation method thereof. The present application uses a gelatin and sericin blend as a microcapsule wall material, and uses 'Chinese mother flower' - xiancao flower fragrance as a core material to prepare a fragrance-releasing microcapsule with good mechanical properties of the wall material. The present application provides a fragrance-releasing silk quilt inner, and the fragrance-releasing microcapsule forms a chemical cross-linking bond with the surface of the silk fiber through a chemical reaction, has high adhesion, pleasant and long-lasting fragrance, and helps people to fall asleep in a warm and comfortable atmosphere.

Description

Technical Field

[0001] This invention belongs to the field of silk weaving, specifically relating to a fragrance-releasing silk quilt inner core and its preparation method. Background Technology

[0002] As early as the Middle Stone Age, five to six thousand years ago, archaeologists discovered that ancient people had already begun to study silkworm cocoon raising, silk extraction, and silk weaving techniques. To this day, research on silk continues to deepen because silk possesses a unique luster, a soft feel, excellent mechanical strength, and high toughness, earning it the title of "Queen of Fibers." Silk is primarily used in textiles and clothing. As a natural high-molecular-weight material, silk has good biocompatibility and relatively good environmental stability, leading to its widespread chemical modification into silk fibers with special properties, such as antibacterial, moisture-wicking, easy dyeing, and antistatic properties, thus meeting the growing demand for functional silk fibers.

[0003] We spend a third of our lives sleeping, but sometimes rough bedding makes us toss and turn, and sometimes lack of skin hydration affects sleep quality. To enjoy a good night's sleep, you need a quilt that has been meticulously crafted in every aspect, and silk quilts have been favored by consumers for many years. To give silk quilts more functionality, a method for preparing a long-lasting, slow-release fragrant silk quilt (CN201811129355.5) discloses a method for preparing a long-lasting, slow-release fragrant silk quilt, using a fragrance solution to soften and scent the silk. The fragrance mixture includes the following components by weight percentage: 8-12% hydrophilic amino silicone oil, 3-5% penetrant, 5-10% glacial acetic acid, 10-20% fragrance microcapsules, 20-40% deionized water, and the balance being water. However, it does not provide a solution on how to improve the adhesion between the fragrance microcapsules and the silk, and cannot ensure that the microcapsules will not fall off during long-term use, thus preventing the silk quilt from retaining its fragrance for a long time.

[0004] To address the adhesion strength issue of microcapsules, CN202210259038 discloses a self-adhesive microcapsule for controllable fragrance addition to textiles, its preparation, and its application. This microcapsule utilizes dopamine-modified fragrance microcapsules and employs Fe... 3+ Controlling its adhesion to fabrics increases the binding force between microcapsules and fabrics, enabling the preparation of scented fabrics. However, this method first requires chitosan microcapsules to be modified by carboxymethyl β-cyclodextrin grafting in the presence of dopamine before it can be processed by Fe... 3+ The chelation process, which uses coordination to bond microcapsules to fabrics, is a complex method that is difficult to industrialize. Summary of the Invention

[0005] To address the aforementioned issues, this invention provides a method for preparing a fragrance-releasing silk quilt inner lining. The fragrance-releasing microcapsules form chemical cross-linking bonds with the surface of silk fibers through a chemical reaction, resulting in high adhesion strength, a pleasant and long-lasting fragrance, and helping people fall asleep peacefully in a warm and comfortable atmosphere.

[0006] To address the aforementioned technical problems, this application provides the following technical solution:

[0007] This invention provides a method for preparing the inner filling of a scented silk quilt, comprising the following steps:

[0008] S1: Mix gelatin aqueous solution, sericin aqueous solution and emulsifier to obtain a homogeneous emulsion;

[0009] A fragrance-releasing microcapsule with good mechanical properties was prepared by using a blend of gelatin and sericin as the microcapsule wall material and daylily fragrance, known as the "Chinese Mother Flower," as the core material.

[0010] S2: Add daylily essential oil to the homogeneous emulsion, mix, and then shear and stir to obtain an emulsion containing aroma-releasing microcapsules;

[0011] S3: Silkworm cocoons are reeled into silk rolls, centrifuged, dehydrated, and then degummed to obtain silk sheets;

[0012] S4: Centrifuge and dehydrate the silk floss sheets;

[0013] S5: Soak the silk flakes dehydrated by centrifugation in step S4 in the finishing solution for 2-4 minutes and then dry them at 65-85℃ until the moisture regain is not higher than 12%; the finishing solution is obtained by mixing an emulsion containing fragrance-releasing microcapsules with a protein crosslinking agent;

[0014] S6: Stretch and cut the dried silk floss sheet from step S5 to obtain silk floss strips;

[0015] S7: The silk strips are stretched into a thin layer of silk mesh and then layered in multiple layers to obtain the inner core of the fragrance-releasing silk quilt.

[0016] Preferably, the concentrations of both the gelatin aqueous solution and the sericin aqueous solution are 0.8-1.5 wt%, and the volume ratio of the gelatin aqueous solution to the sericin aqueous solution is 1-3:1.

[0017] Preferably, the emulsifier is selected from quaternary ammonium salt emulsifiers, and its content in the homogeneous emulsion is 1-2 wt%. Its residue on the surface of silk can exert its own antibacterial and other functions.

[0018] Preferably, in step S3, the degumming process takes 5-10 minutes.

[0019] Preferably, in step S3, the degumming process is carried out by placing the sample in a weak alkaline aqueous solution at a temperature of 85-95°C, wherein the concentration of the solute in the weak alkaline aqueous solution is 0.3-0.7 g / L.

[0020] After the above degumming process, the residual sericin on the surface of the silk is higher than that of the traditional silk reeling process, with a residual sericin rate of 7-9%. This facilitates further intermolecular diffusion and cross-linking with the wall material of the microcapsules, thereby improving the adhesion strength of the microcapsules to the surface of the silk.

[0021] Furthermore, the weak base is an alkaloid, selected from berberine or quaternary ammonium bases. On one hand, this weakens the degumming reaction, increasing the residual sericin rate on the silk surface. On the other hand, the organic base remaining on the silk surface can exert its own antibacterial and other functions.

[0022] Preferably, the particle size of the aroma-releasing microcapsules in the aroma-releasing microcapsule emulsion is 0.1-30 μm.

[0023] Preferably, in the finishing solution, the protein cross-linking agent is transglutaminase, and the mass of transglutaminase is 15-35% of the total mass of gelatin and sericin.

[0024] In step S5, during drying in the oven, under the action of the protein crosslinking agent, the gelatin and sericin of the microcapsule wall material undergo chemical crosslinking with the sericin remaining on the silk surface. The gelatin and sericin macromolecules in the microcapsule wall material diffuse into each other simultaneously with the sericin macromolecules on the silk surface, thereby improving the adhesion of the microcapsules to the silk surface.

[0025] Preferably, in step S6, the length of the stretch is 3-6 times the original length.

[0026] Specifically, the preparation method of the scented silk quilt inner lining includes the following steps:

[0027] (1) Preparation of aroma-releasing microcapsule emulsion

[0028] A mixed aqueous solution of gelatin and sericin with a concentration of 0.8-1.5 wt% was prepared by mixing them in a certain proportion. An emulsifier was added to the mixed aqueous solution and stirred at high speed to form a homogeneous emulsion.

[0029] Add daylily essential oil to the above emulsion at a flow rate of 60-100 drops (approximately 0.07g per drop) / min according to the specified ratio, and mix thoroughly. Then, after high-speed shearing and stirring, form a fragrance-releasing microcapsule emulsion with a particle size of 0.1-30μm.

[0030] (2) Preparation of high-colloid-content silk floss sheets

[0031] The silkworm cocoons are reeled into silk rolls using a silk reeling machine. After centrifugation and dehydration, the rolls are placed in a weak alkaline aqueous solution at a temperature of 85-95℃ and a weight percentage concentration of 0.3-0.7 g / L for degumming for 5-10 minutes. The rolls are then removed and centrifuged again for further dehydration.

[0032] (3) Finishing after silk floss floss release microcapsule emulsion

[0033] The aroma-releasing microcapsule emulsion was mixed with a protein cross-linking agent to form an aroma-releasing microcapsule emulsion finishing solution. The dehydrated silk floss sheets were then immersed in the finishing solution for 2-4 minutes, and then dried in an oven at 65-85℃ to obtain the silk floss sheets.

[0034] The preferred protein cross-linking agent is transglutaminase, and the amount of transglutaminase added is 15-35% of the mass of the two proteins in the gelatin and sericin aqueous solution.

[0035] (4) Preparation of silk quilt inner filling

[0036] The dried silk floss sheets are stretched to 3-6 times their original length along a direction perpendicular to the silk fibers. Then, they are cut into sections according to the length of the silk quilt to obtain silk floss strips. These strips are then stretched into thin layers of silk mesh by hand and shaken by four people. These layers are then stacked in sequence to obtain the inner filling of the silk quilt.

[0037] The present invention also provides a fragrance-releasing silk quilt inner core prepared by the above preparation method.

[0038] The technical solution of the present invention has the following advantages compared with the prior art:

[0039] This invention provides a fragrance-releasing silk quilt inner filling, in which the surface of the silk fibers is cross-linked with fragrance-releasing microcapsules, which have a pleasant and long-lasting fragrance, helping people fall asleep peacefully in a warm and comfortable atmosphere.

[0040] After the degumming process, the residual sericin on the surface of the silk is slightly higher than that of the traditional silk reeling process, which is conducive to further cross-linking with the wall material of the microcapsules and thus improving the adhesion strength of the microcapsules.

[0041] In the oven, under the action of the transglutaminase crosslinking agent, the gelatin of the microcapsule wall material undergoes chemical crosslinking with the sericin remaining on the silk surface, thereby improving the adhesion strength between the microcapsules and the silk surface of the silk quilt. Attached Figure Description

[0042] Figure 1 Image of silk flakes in aroma-releasing microcapsule emulsion.

[0043] Figure 2 This image shows a silk floss sheet with fragrance-releasing microcapsules stretched to three times its original length along a direction perpendicular to the length of the silk fibers. Detailed Implementation

[0044] The present invention will be further described below with reference to specific embodiments, so that those skilled in the art can better understand and implement the present invention, but the embodiments are not intended to limit the present invention.

[0045] Example 1

[0046] After silkworm cocoons are reeled into silk floss rolls using a reeling machine, the silk floss sheets are centrifuged to remove water and then placed in a berberine aqueous solution at 90℃ and a weight percentage concentration of 0.5 g / L for degumming treatment for 8 minutes. The silk is then removed, centrifuged again to remove water, and a residual glue rate of 7% is obtained.

[0047] 5 L of each of the following solutions, containing 1.5% by weight, were taken and mixed to prepare a mixed protein aqueous solution. 100 g of hexadecyltrimethylammonium chloride emulsifier was added to the protein mixture, and the mixture was stirred at at least 8000 rpm for 5 min to form a homogeneous emulsion. 100 g of daylily essential oil was added dropwise to the emulsion at a rate of 60 drops / min, followed by high-speed shearing and stirring at at least 12000 rpm for 3 min to form a fragrance-releasing microcapsule emulsion with a particle size of 0.1–20 μm.

[0048] Add 20g of transglutaminase crosslinking agent to the above-mentioned aroma-releasing microcapsule emulsion, and add 400g of silk reeling while stirring. Stir and soak for 2 minutes, then remove and dry in a drying room at 75℃ until the moisture regain is 10% to obtain aroma-releasing microcapsule silk floss sheets.

[0049] The dried silk floss sheets are stretched to three times their original length along a direction perpendicular to the silk fibers. Then, they are cut into sections according to the length of the silk quilt to obtain silk floss strips. These strips are then stretched into thin layers of silk mesh by hand and shaken by four people. These layers are then stacked in sequence to obtain the inner filling of the silk quilt.

[0050] Example 2

[0051] After silkworm cocoons are reeled into silk floss rolls using a reeling machine, the silk floss sheets are centrifuged to remove water and then placed in a berberine aqueous solution at 90℃ and a weight percentage concentration of 0.3 g / L for degumming treatment for 5 minutes. The silk is then removed, centrifuged again to remove water, and a residual glue rate of 9% is obtained.

[0052] 7 L and 30 mL of 1.5% (w / w) gelatin and sericin aqueous solutions were taken separately and stirred to prepare a mixed protein aqueous solution. 200 g of hexadecyltrimethylammonium chloride emulsifier was added to the protein mixed aqueous solution, and the mixture was stirred at at least 8000 rpm for 5 min to form a homogeneous emulsion. 150 g of daylily essential oil was added dropwise to the above emulsion at a rate of 60 drops / min, and then the mixture was subjected to high-speed shear stirring at at least 15000 rpm for 3 min to form a fragrance-releasing microcapsule emulsion with a particle size of 0.1–15 μm.

[0053] Add 52g of glutamine transaminase crosslinking agent to the above-mentioned aroma-releasing microcapsule emulsion, and add 500g of silk reeling silk while stirring. Stir and soak for 4 minutes, take it out, and then put it in a drying room at a temperature of 85℃ to dry until the moisture regain is 9%, to obtain aroma-releasing microcapsule silk floss sheets.

[0054] The dried silk floss sheets are stretched to four times their original length along a direction perpendicular to the silk fibers. Then, they are cut into sections according to the length of the silk quilt to obtain silk floss strips. Four people manually open and shake the silk floss strips to stretch them into thin layers of silk mesh. These layers are then stacked one after another to obtain the inner filling of the silk quilt.

[0055] Example 3

[0056] After silkworm cocoons are reeled into silk floss rolls using a reeling machine, the silk floss sheets are centrifuged to remove water and then placed in a berberine aqueous solution at 95℃ and a weight percentage concentration of 0.7 g / L for degumming treatment for 10 minutes. The silk is then removed, centrifuged again to remove water, and a residual glue rate of 7% is obtained.

[0057] 5 L of each of the following solutions, containing 1.5% by weight, were taken and mixed to prepare a mixed protein aqueous solution. 100 g of hexadecyltrimethylammonium bromide emulsifier was added to the protein mixture, and the mixture was stirred at at least 8000 rpm for 5 min to form a homogeneous emulsion. 200 g of daylily essential oil was added dropwise to the emulsion at a rate of 100 drops / min, followed by high-speed shearing and stirring at at least 12000 rpm for 3 min to form a fragrance-releasing microcapsule emulsion with a particle size of 0.1–30 μm.

[0058] Add 20g of glutamine transaminase crosslinking agent to the above-mentioned aroma-releasing microcapsule emulsion, and add 450g of silk reeling while stirring. Stir and soak for 2 minutes, then remove and dry in an oven at 85℃ until the moisture regain is 11% to obtain aroma-releasing microcapsule silk floss sheets.

[0059] The dried silk floss sheets are stretched to six times their original length along a direction perpendicular to the silk fibers. Then, they are cut into sections according to the length of the silk quilt to obtain silk floss strips. These strips are then stretched into thin layers of silk mesh by hand and shaken by four people. These layers are then stacked in sequence to obtain the inner filling of the silk quilt.

[0060] Example 4

[0061] After silkworm cocoons are reeled into silk floss rolls using a reeling machine, the silk floss sheets are centrifuged to remove water and then placed in a benzalkonium bromide aqueous solution at 90℃ and a weight percentage concentration of 0.3 g / L for degumming treatment for 7 minutes. The silk is then removed, centrifuged again to remove water, and a residual glue rate of 8% is obtained.

[0062] 7.5 L and 2.5 L of 1.5% (w / w) gelatin and sericin aqueous solutions were taken separately and stirred to prepare a mixed protein aqueous solution. 150 g of hexadecyltrimethylammonium chloride emulsifier was added to the protein mixed aqueous solution, and the mixture was stirred at at least 8000 rpm for 5 min to form a homogeneous emulsion. 150 g of daylily essential oil was added dropwise to the above emulsion, and then the mixture was subjected to high-speed shear stirring at at least 12000 rpm for 3 min to form a fragrance-releasing microcapsule emulsion with a particle size of 0.1–30 μm.

[0063] Add 40g of transglutaminase crosslinking agent to the above-mentioned aroma-releasing microcapsule emulsion, and add 500g of silk reeling while stirring. Stir and soak for 4 minutes, then remove and dry in a drying room at 75℃ until the moisture regain is 7%, to obtain aroma-releasing microcapsule silk floss sheets.

[0064] The dried silk floss sheets are stretched to three times their original length along a direction perpendicular to the silk fibers. Then, they are cut into sections according to the length of the silk quilt to obtain silk floss strips. These strips are then stretched into thin layers of silk mesh by hand and shaken by four people. These layers are then stacked in sequence to obtain the inner filling of the silk quilt.

[0065] Example 5

[0066] After silkworm cocoons are reeled into silk floss rolls using a reeling machine, the silk floss sheets are centrifuged to remove water and then placed in a benzalkonium bromide aqueous solution at 90℃ and a weight percentage concentration of 0.7 g / L for degumming treatment for 10 minutes. The silk is then removed, centrifuged again to remove water, and a residual glue rate of 7% is obtained.

[0067] 5 L of each of the following solutions, containing 1.5% by weight, were taken and mixed to prepare a mixed protein aqueous solution. 200 g of hexadecyltrimethylammonium bromide emulsifier was added to the protein mixed aqueous solution, and the mixture was stirred at at least 8000 rpm for 5 min to form a homogeneous emulsion. 100 g of daylily essential oil was added dropwise to the above emulsion, and the mixture was then subjected to high-speed shear stirring at at least 12000 rpm for 3 min to form a fragrance-releasing microcapsule emulsion with a particle size of 0.1–20 μm.

[0068] Add 30g of transglutaminase crosslinking agent to the above-mentioned aroma-releasing microcapsule emulsion, and add 480g of silk reeling while stirring. Stir and soak for 2 minutes, then remove and dry in a drying room at 75℃ until the moisture regain is 10% to obtain aroma-releasing microcapsule silk floss sheets.

[0069] The dried silk floss sheets are stretched to five times their original length along a direction perpendicular to the silk fibers. Then, they are cut into sections according to the length of the silk quilt to obtain silk floss strips. Four people manually open and shake the silk floss strips to stretch them into thin layers of silk mesh. These layers are then stacked one after another to obtain the inner filling of the silk quilt.

[0070] Effect Evaluation 1

[0071] Test method:

[0072] (1) Residual glue content

[0073] Take two samples, each with a mass of 3.0g ± 0.3g. First, remove the grease according to the method specified in FZ / T 40006, and then conduct the test according to FZ / T40004. Calculate the residual gum rate according to formula (1), and round the result to 0.1 according to GB / T 8170.

[0074]

[0075] In the formula:

[0076] P—Residual glue content:

[0077] m c0 —Dry weight of the sample before degumming, in grams (g);

[0078] m c1 —Dry weight of the sample after degumming, in grams (g).

[0079] (2) Evaluation of fragrance release

[0080] The aroma release evaluation was conducted by a sensory evaluation group of 5 people. The aroma release was tested, and the average score of the 5 people was calculated. The highest score was 5 points: 0 points, no perceptible aroma; 1 point, aroma is barely perceptible; 2 points, general aroma; 3 points, obvious aroma; 4 points, rich aroma; 5 points, strong aroma.

[0081] (3) Fragrance longevity

[0082] Referring to GB / T 457, the determination of folding endurance of paper and paperboard was performed using a PY-H608 paperboard folding endurance tester. The samples were first subjected to 1000 folds, followed by a sensory evaluation of aroma release, with a maximum score of 5 points. The sample width was 15 mm, tension was 14.72 N, folding angle was 135°±2°, and folding speed was 175±10 folds / min.

[0083] For ease of explanation, the concentrations of gelatin and silk fibroin aqueous solutions in the above examples are both 1.5%. The performance of the samples obtained from the above examples was tested, and the results are shown in Table 1.

[0084] Table 1. Sensory Evaluation Scoring Table for Aroma

[0085] project Example 1 Example 2 Example 3 Example 4 Example 5 Residual glue content (%) 8 9 7 8 7 Fragrance release score 4.5 4.9 4.8 4.9 4.8 Fragrance longevity 4.0 4.9 3.5 4.8 4.0 Remark* have have have have have

[0086] *Note: Does the sample release a burst of aroma after being kneaded?

[0087] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A method for preparing a scented silk quilt inner filling, characterized in that, Includes the following steps: S1: Mix gelatin aqueous solution, sericin aqueous solution and emulsifier to obtain a homogeneous emulsion; S2: Add daylily essential oil to the homogeneous emulsion, mix, and then shear and stir to obtain an emulsion containing aroma-releasing microcapsules; S3: Reel silkworm cocoons into silk rolls, centrifuge and dehydrate them, then degumme them to obtain silk floss sheets; in step S3, the degumming time is 5-10 min; in step S3, the degumming method is to place the silk floss sheets in a weak alkaline aqueous solution at a temperature of 85-95℃, wherein the concentration of the solute in the weak alkaline aqueous solution is 0.3-0.7 g / L; the weak alkaline is an alkaloid, and the alkaloid is selected from berberine or quaternary ammonium alkaloids; the residual glue rate of the silk floss sheets is 7-9%; S4: Centrifuge and dehydrate the silk floss sheets; S5: After centrifugation and dehydration in step S4, the silk flakes are soaked in the finishing solution for 2-4 minutes and then dried at 65-85℃ until the moisture regain is no higher than 12%; the finishing solution is obtained by mixing an emulsion containing aroma-releasing microcapsules with a protein cross-linking agent; in the finishing solution, the protein cross-linking agent is transglutaminase, and the mass of transglutaminase is 15-35% of the total mass of gelatin and sericin; S6: Stretch and cut the dried silk floss sheet from step S5 to obtain silk floss strips; S7: The silk strips are stretched into a thin layer of silk mesh and then layered in multiple layers to obtain the inner core of the fragrance-releasing silk quilt.

2. The preparation method according to claim 1, characterized in that, The concentrations of the gelatin aqueous solution and the sericin aqueous solution are both 0.8-1.5 wt%, and the volume ratio of the gelatin aqueous solution to the sericin aqueous solution is 1-3:

1.

3. The preparation method according to claim 1, characterized in that, The aroma-releasing microcapsule emulsion contains aroma-releasing microcapsules with a particle size of 0.1-30 μm.

4. The preparation method according to claim 1, characterized in that, In step S6, the length of the stretch is 3-6 times the original length.

5. A fragrance-releasing silk quilt inner lining prepared by any one of claims 1-4.

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