Preparation method of non-polluted absorbent cotton paper
Patent Information
- Application Number
- CN202411432164.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-14
- Publication Date
- 2026-09-25
- Estimated Expiration
- 2044-10-14
AI Technical Summary
[0004]然而上述现有技术在制备得到脱脂棉棉纸后,需要在无菌环境内对其进行迅速消毒及包装,否则脱脂棉棉纸容易受到外部环境的污染,此外脱脂棉棉纸在长期存储过程中容易受到光照和环境温度的影响出现老化,从而导致脱脂棉纤维出现断裂和吸水性降低,因此亟需提供一种方案解决上述问题
[0023]可选地,所述脱脂棉的制备方法包括:将除杂后的棉纤维进行梳棉后制得棉短绒;将棉短绒在碱液内脱脂后漂白制得脱脂棉。如此对棉纤维进行除杂和梳棉后能够取出纤维内的杂质并对纤维进行梳理,使其更加均匀和整齐,能够极大地提高棉纤维的纯净度和纤维均匀性,而对棉短绒进行脱脂和漂白,能够去除棉纤维中的天然油脂、蜡质和色素,通过皂化反应将脂肪酸盐和甘油从纤维表面去除,进一步提高纤维的纯净度和亲水性,漂白还能够提高脱脂棉纤维的白度和化学吸附性能。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of degreased cotton technology, and in particular to a method for preparing degreased cotton paper that is not easily contaminated. Background Technology
[0002] After cotton fibers are chemically treated to remove oil components, degreased cotton, whose main component is cellulose, is obtained. It has good water absorption, flexibility and breathability. After degreased cotton fibers are made into degreased cotton paper, the application of degreased cotton in the fields of medical care, hygiene and personal care can be greatly improved.
[0003] Existing technologies mainly use degreased cotton as raw material in the process of preparing degreased cotton paper. The degreased cotton is combed into a uniform fiber web, and pressure is applied to form the fiber web into a thin sheet. The moisture in the fiber web is removed by drying, thereby forming degreased cotton paper.
[0004] However, the existing technology requires rapid sterilization and packaging of the degreased cotton paper after it is prepared in a sterile environment. Otherwise, the degreased cotton paper is easily contaminated by the external environment. In addition, the degreased cotton paper is easily affected by light and ambient temperature during long-term storage, which can lead to aging, resulting in breakage of the degreased cotton fibers and reduced water absorption. Therefore, there is an urgent need to provide a solution to the above problems. Summary of the Invention
[0005] The purpose of this invention is to provide a method for preparing degreased cotton paper that is not easily contaminated.
[0006] The present invention provides a method for preparing non-contaminated degreased cotton paper, comprising the following steps: pulping degreased cotton in a modified solution to form fiber pulp; filtering primary cotton paper from the fiber pulp using a forming screen, and drying the primary cotton paper to obtain secondary cotton paper with a moisture content of 10-20%; soaking the secondary cotton paper in pine leaf extract for modification, then removing and drying it to obtain degreased cotton paper with a moisture content of 3-8%.
[0007] The preparation method provided by this invention, by soaking and pulping degreased cotton in a modified solution, facilitates the full surface modification of the degreased cotton fibers. This process forms a uniform and dense protective film on the surface of the degreased cotton fibers, inhibiting microbial growth and improving fiber stability and storage performance. Furthermore, the surface modification treatment facilitates the adhesion of pine needle extract to the surface of the degreased cotton fibers, thereby forming a composite film structure with the pine needle extract and the protective film. This improves the water absorption and water retention properties of the degreased cotton fibers and further enhances the overall corrosion resistance and structural stability of the degreased cotton paper.
[0008] Optionally, the preparation method of the dwarf pine leaf extract includes: steaming dwarf pine leaf powder in boiling water for 1-2 hours to obtain a cooked powder; mixing the cooked powder with a compound bacterial solution and then fermenting and sterilizing; collecting the fermentation liquid and fermentation residue; keeping the fermentation residue in deionized water at 90-100℃ for 1-2 hours and then separating the aqueous extract; combining the aqueous extract and the fermentation liquid and concentrating under an inert atmosphere to obtain the dwarf pine leaf extract.
[0009] Optionally, when the matured powder is mixed with the compound bacterial solution, the compound bacterial solution includes a fermentation base liquid and a mixed fermentation bacteria inoculated in the fermentation base liquid, and the mixed fermentation bacteria include lactic acid bacteria and yeast.
[0010] Optionally, the fermentation base liquid includes a sugar source, and the sugar source includes at least one of glucose and maltose.
[0011] Optionally, the lactobacillus is Lactobacillus CGMCC NO.0843.
[0012] Optionally, the yeast strain is CGMCC NO.27154.
[0013] Optionally, the inoculation concentration of the fermentation mixed bacteria in the fermentation base liquid is 10. 6 -10 7 CFU / mL.
[0014] Optionally, the ratio of viable lactobacilli to viable yeast in the fermentation mixture is (0.5-1):1.
[0015] Optionally, the matured powder is mixed with the compound bacterial solution and fermented in an anaerobic environment at 25-37°C and pH 5-6 for 70-74 hours, followed by sterilization; the sterilization includes at least one of high-temperature sterilization and ultraviolet sterilization.
[0016] Optionally, the pine needle powder is sieved through a 100-200 mesh sieve and then steamed in boiling water.
[0017] Optionally, the moisture content of the pine needle powder is 5-10%.
[0018] Optionally, the mixing ratio of the viable bacteria count in the composite bacterial solution to the cooked powder is 10:1. 6 -10 7 CFU / g.
[0019] Optionally, the volume of the pine leaf extract is 1 / 4 to 1 / 3 of the volume of the water extract and the fermentation broth.
[0020] Optionally, when the degreased cotton is pulped in a modified solution, the modified solution includes 5-10% by mass of active polyphenols, and the active polyphenols include at least one of tea polyphenols, anthocyanins, resveratrol, and curcumin.
[0021] Optionally, after ultrasonically mixing the degreased cotton in the modified solution for 10-15 minutes, it is then pulped for 30-45 minutes at a speed of 2000-3000 rpm and a gap of 0.1-0.5 mm to prepare a fiber slurry.
[0022] Optionally, the secondary cotton paper is soaked in pine leaf extract at 30-35℃ for 15-20 minutes, then dried to a moisture content of 20-25% to obtain the tertiary cotton paper. The tertiary cotton paper is then bleached in a bleaching solution and dried to a moisture content of 3-8% to obtain the degreased cotton paper.
[0023] Optionally, the method for preparing the degreased cotton includes: carding the cotton fibers after impurity removal to obtain cotton linters; and degreasing and bleaching the cotton linters in an alkaline solution to obtain degreased cotton. This process of removing impurities and carding the cotton fibers removes these impurities and makes the fibers more uniform and neat, greatly improving the purity and uniformity of the cotton fibers. Degreasing and bleaching the cotton linters remove natural oils, waxes, and pigments from the cotton fibers, and through saponification, removes fatty acid salts and glycerol from the fiber surface, further improving the purity and hydrophilicity of the fibers. Bleaching also improves the whiteness and chemical adsorption properties of the degreased cotton fibers. Detailed Implementation
[0024] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Unless otherwise defined, the technical or scientific terms used herein should have the ordinary meaning understood by those skilled in the art to which this invention pertains.
[0025] This invention provides a method for preparing degreased cotton paper that is not easily contaminated, comprising the following steps:
[0026] S1. The degreased cotton is pulped in a modified solution to produce fiber pulp;
[0027] S2. Use a forming screen to filter primary cotton paper from the fiber pulp;
[0028] S3. The primary cotton paper is dried to obtain secondary cotton paper with a moisture content of 10-20%.
[0029] S4. After soaking and modifying the secondary cotton paper in pine leaf extract, remove and dry it to obtain degreased cotton paper with a moisture content of 3-8%.
[0030] In some embodiments, the method for preparing the absorbent cotton used in step S1 includes:
[0031] S0.1. The cotton fibers after impurity removal are carded to obtain cotton linters;
[0032] S0.2 Degreased cotton is obtained by degreasing cotton linters in an alkaline solution and then bleaching them.
[0033] In fact, during the execution of step S0.1, mechanical impurity removal can be used to remove impurities from cotton fibers. First, a cotton cleaning machine is used to perform preliminary treatment on the cotton fibers. The beaters inside the cotton cleaning machine rotate at high speed to beat and tear the cotton fibers, thereby separating impurities from the cotton fibers. The dust grid plays a preliminary screening role for impurities.
[0034] In fact, during the execution of step S0.1, after the cotton fiber is initially screened and impurities removed by the cotton cleaning machine, the cotton fiber can be further cleaned and combed by the carding machine. This can further remove smaller impurities and short fibers from the cotton fiber, significantly improving the efficiency and cleanliness of the cotton fiber cleaning process. In addition, the card cloth on the cylinder of the carding machine can comb and shape the cotton fiber.
[0035] In fact, during the execution of step S0.1, when using a cotton cleaner and a carding machine to remove impurities and card cotton fibers, those skilled in the art can adaptively and reasonably adjust the parameters of the cotton cleaner and carding machine according to the processing conditions. For example, they can adjust the speed of the beaters in the cotton cleaner, the spacing between the dust grids, and the spacing between the cylinder and the cover plate of the cotton cleaner. In addition, the parameters can be adjusted according to the processing volume and impurity content of the cotton fibers to achieve the necessary removal and carding of the cotton fibers.
[0036] Specifically, in step S0.2, the cotton linters are soaked in an alkaline solution, causing a saponification reaction between the alkali and the oils in the cotton linters. This converts the water-insoluble oils into water-soluble fatty acid salts, thereby degreasing the cotton linters. Specifically, the alkaline solution used includes at least one of sodium hydroxide solution and potassium hydroxide solution, and the mass fraction of the solute in the alkaline solution is 5-10%.
[0037] Specifically, during step S0.2, after soaking the cotton linters in the alkaline solution, a surfactant can be added to the alkaline solution to reduce the surface tension, making it easier for the oil in the cotton linters to detach from the surface of the cotton fibers. In addition, when dealing with some dense cotton linters with deep oil penetration, adding a surfactant can significantly improve the degreasing efficiency and degreasing rate.
[0038] Specifically, in step S0.2, cotton linters are soaked in an alkaline solution and stirred at 50-80°C for 0.5-2 hours for degreasing. In fact, heating during the degreasing process effectively increases the rate of saponification, allowing for better decomposition of oil components and thus improving the degreasing rate of the cotton linters.
[0039] Specifically, in step S0.2, after degreasing the cotton linters in an alkaline solution, the degreased cotton linters are removed and their surface is rinsed with deionized water to remove residual alkaline solution and generated fatty acid salts from the surface of the cotton linters. In fact, during the surface rinsing with deionized water, the rinsing continues until the washing solution is neutral, ensuring that the pH value of the cotton linters returns to near neutral.
[0040] Specifically, in step S0.2, the degreased cotton linters are bleached in a bleaching solution. This helps improve the whiteness of the cotton linters after degreasing, enhancing their safety in medical and hygiene applications. Furthermore, the white appearance enhances visual cleanliness. The bleaching process also removes impurities and dirt from the surface of the degreased cotton, making the pores of the cotton fibers more open and improving the cotton's absorbency.
[0041] Specifically, in step S0.2, the degreased cotton linters are stirred and reacted in the bleaching solution to improve bleaching efficiency and uniformity. Furthermore, the bleaching time is controlled to be 30-60 minutes to avoid over-bleaching of the cotton linters. In practice, the temperature of the bleaching solution can be controlled at 20-30℃ during the bleaching process. Within this temperature range, the reaction efficiency can be effectively balanced, and damage to the cotton linters and over-bleaching can be avoided.
[0042] Specifically, in step S0.2, when bleaching the degreased cotton linters in a bleaching solution, the bleaching solution includes at least one of hydrogen peroxide and sodium hypochlorite. Specifically, the concentration of hydrogen peroxide and sodium hypochlorite in the bleaching solution can be 1-5 wt%. Specifically, after bleaching the cotton linters with the bleaching solution, the cotton linters are rinsed with deionized water to remove residual bleaching components and decomposition products, thereby stabilizing the bleaching effect.
[0043] In some embodiments, during step S1, the modified solution used includes 5-10% by mass of active polyphenols, and the solute in the modified solution is deionized water. By immersing the absorbent cotton in the modified solution, the active polyphenols can penetrate into the interior and surface of the absorbent cotton fibers, forming a uniform and dense polyphenol protective layer on the surface of the absorbent cotton fibers, effectively improving the protection of the cotton fibers. Furthermore, the active polyphenols also have good antibacterial and antioxidant properties, which can greatly improve the storage stability and anti-fouling properties of the absorbent cotton paper.
[0044] Specifically, the active polyphenols in the modification solution include at least one of tea polyphenols, anthocyanins, resveratrol, and curcumin. In fact, by selecting different active polyphenols and controlling the mixing ratio of active polyphenols in the modification solution, the structure of the polyphenol protective layer on the surface of the absorbent cotton fibers can be regulated, thereby controlling the storage performance and anti-fouling properties of the absorbent cotton paper. More specifically, the active polyphenols in the modification solution are a mixture of tea polyphenols and anthocyanins in a 1:1 mass ratio.
[0045] In some embodiments, during step S1, the degreased cotton is ultrasonically mixed in the modified solution for 10-15 minutes, and then beaten at a speed of 2000-3000 rpm and a gap of 0.1-0.5 mm for 30-45 minutes to produce a fiber slurry. In fact, by ultrasonically mixing the degreased cotton with the modified solution, the cavitation effect of ultrasound can be utilized to promote the adsorption of active polyphenols on the surface of the active cotton fibers, while also improving the mixing uniformity, which is beneficial for beating.
[0046] Specifically, the pulping process needs to be carried out in a disc pulper, and the feed pressure needs to be controlled at 0.1-0.3 MPa. In fact, by pulping the degreased cotton, the active polyphenols can be further combined with the degreased cotton fibers. Furthermore, during the pulping process, the degreased cotton fibers are subjected to mechanical forces, resulting in physical changes such as cutting, which is beneficial for the preparation of cotton paper.
[0047] In some embodiments, during step S2, an 80-120 mesh forming screen is used to filter the fiber slurry. After the cotton fibers completely cover the surface of the forming screen, the forming screen is removed from the fiber slurry and allowed to stand until no more liquid flows down. Then, the primary cotton paper is peeled off the surface of the forming screen.
[0048] In some embodiments, during step S3, after the primary cotton paper is dried, the evaporation of moisture leads to enhanced hydrogen bonding between cotton fibers, thereby improving the mechanical strength and structural stability of the cotton paper. In addition, by controlling the moisture content of the resulting secondary cotton paper, shrinkage and deformation caused by severe water loss can be avoided.
[0049] In some embodiments, during step S3, the primary cotton paper is dried under a nitrogen atmosphere at 40-45°C. This avoids surface oxidation of the primary cotton paper caused by oxidizing gases, which is beneficial for improving the surface quality of the secondary cotton paper. Furthermore, controlling the drying at a lower temperature helps control the rate of water loss from the primary cotton paper.
[0050] In some embodiments, the preparation method of dwarf pine leaf extract during step S4 includes the following steps:
[0051] Y1. Steam the powdered pine needles in boiling water for 1-2 hours to obtain cooked powder;
[0052] Y2. After mixing the cooked powder with the compound bacterial solution, ferment and then sterilize, and collect the fermentation liquid and fermentation residue; Y3. After keeping the fermentation residue in deionized water at 90-100℃ for 1-2 hours, separate the water extract.
[0053] Y4. The aqueous extract and fermentation broth were combined and concentrated under an inert atmosphere to obtain the pine leaf extract.
[0054] In fact, after performing step Y1, steaming the pine leaf powder in boiling water is beneficial for activating and transforming the active substances in the pine leaf powder. In addition, it avoids the direct dissolution of active substances in the solvent environment, and can destroy the cell wall structure in the pine leaf powder. It can also sterilize the pine leaf powder at the same time.
[0055] In some embodiments, during step Y1, the dwarf pine leaf powder is sieved through a 100-200 mesh sieve and then steamed in boiling water. In fact, using dwarf pine leaf powder helps to increase its specific surface area, thereby increasing the soluble area and dissolution rate of the active ingredients, and also improving post-processing efficiency. Furthermore, the dwarf pine leaf powder used can be obtained by washing fresh dwarf pine leaves, then drying them naturally or mechanically to obtain dwarf pine leaves with a moisture content of 5-10%, before further pulverization.
[0056] In some embodiments, during step Y1, the pine needle powder is spread evenly in a steamer and the thickness of the pine needle powder is controlled to be 8-10 mm. The steamer containing the pine needle powder is placed on top of boiling water at 100°C and the boiling water is continuously heated to steam the pine needle powder.
[0057] In some embodiments, during step Y2, the compound bacterial solution includes a fermentation base liquid and a mixed fermentation bacteria inoculated in the fermentation base liquid, and the mixed fermentation bacteria include lactic acid bacteria and yeast. In fact, fermenting the mature powder with the mixed fermentation bacteria helps to degrade large molecules such as polysaccharides in dwarf pine leaves into smaller active molecules, and also further removes plant cell walls. Furthermore, the organic acids and alcohols produced during fermentation can esterify with the active substances in the dwarf pine leaves to obtain esterified products.
[0058] In some embodiments, during step Y2, the fermentation medium used includes a sugar source and deionized water for dissolving the sugar source, and the sugar source includes at least one of glucose and maltose. In fact, pre-preparing the fermentation medium can provide a nutrient substrate for the metabolic activities of the fermenting mixed bacteria, supporting their growth and metabolism.
[0059] In some embodiments, during step Y2, the lactobacillus is Lactobacillus CGMCC NO.0843 and the yeast is yeast CGMCC NO.27154. In practice, the inoculation concentration of the fermentation mixture in the fermentation base liquid is 10. 6 -10 7 CFU / mL, and the ratio of viable bacteria in the compound bacterial solution to the cooked powder is 10:1. 6 -10 7 CFU / g. Specifically, the ratio of viable lactobacilli to viable yeast in the fermentation mixture is (0.5-1):1.
[0060] In some embodiments, during step Y2, the cooked powder is mixed with the composite bacterial solution and fermented in an anaerobic environment at 25-37°C and pH 5-6 for 70-74 hours, followed by sterilization. Specifically, sterilization includes at least one of high-temperature sterilization and ultraviolet sterilization.
[0061] In some embodiments, during step Y4, the inert atmosphere used is argon, and the volume of the pine leaf extract is 1 / 4 to 1 / 3 of the volume of the water extract and the fermentation broth.
[0062] In some embodiments, during step S4, the secondary cotton paper is soaked in pine leaf extract at 30-35°C for 15-20 minutes, then removed and dried to a moisture content of 20-25% to become tertiary cotton paper. The tertiary cotton paper is then bleached in a bleaching solution and dried to a moisture content of 3-8% to become degreased cotton paper.
[0063] Preparation Example 1
[0064] Example 1 provides a method for preparing absorbent cotton, comprising the following steps:
[0065] S0.1. The cotton fibers are fed evenly into the feed port of the cotton cleaner. The beater speed in the cotton cleaner is set to 800 rpm, the dust grid spacing is set to 3 mm, and the distance between the cylinder and the cover plate is set to 0.18 mm. The cotton fibers that have passed through the cotton cleaner are fed into the carding machine. The licker-in roller in the carding machine rotates at a speed of 900 rpm, and the cylinder speed is 350 rpm. After opening and combing the cotton fibers, cotton linters are produced.
[0066] S0.2. The cotton linters are immersed in a 5% sodium hydroxide aqueous solution and stirred at 60°C for 1 hour. The cotton linters are then removed and continuously rinsed with deionized water until the pH of the rinsing solution is neutral. The degreased cotton linters are then immersed in a 3% sodium hypochlorite aqueous solution and stirred at 25°C for 40 minutes. The cotton linters are then removed and rinsed with deionized water to obtain degreased cotton.
[0067] Preparation Example 2
[0068] Example 2 of this preparation provides a method for preparing dwarf pine leaf extract, including the following steps:
[0069] Y1. Spread the pine needle powder (8wt% moisture content) that has passed through a 100-mesh sieve evenly in a steamer, and control the loose layer thickness of the pine needle powder to be 10mm. Then place the steamer 15cm away from the surface of boiling water and continue to heat the boiling water to boiling. After steaming the pine needle powder for 2 hours, remove the steamer and let it cool to room temperature to obtain cooked powder.
[0070] Y2. A compound bacterial culture was prepared by inoculating Lactobacillus CGMCC NO.0843 and yeast CGMCC NO.27154 into the fermentation base liquid (a 10 wt% glucose aqueous solution), with a viable count of 10⁻⁶ Lactobacillus CGMCC NO.0843 in the compound bacterial culture. 7 The viable count of yeast CGMCC NO.27154 was 10 CFU / mL. 7 CFU / mL; After uniformly mixing the matured powder and the compound bacterial solution at a mass-volume ratio of 1g / mL, fermentation was carried out in an anaerobic environment at 32℃ and pH 5 for 72h, followed by ultraviolet sterilization and separation of fermentation broth and fermentation residue.
[0071] Y3. After mixing the fermentation residue with deionized water at a volume ratio of 1:10, heat to 95°C and keep warm for 2 hours, then filter and separate. Wash the filtrate with deionized water and combine the washing liquid and filtrate to obtain an aqueous extract.
[0072] Y4. The aqueous extract and fermentation broth were combined and ultrasonically mixed, and then concentrated under an argon atmosphere at 60°C to obtain the dwarf pine leaf extract; the volume of the dwarf pine leaf extract was 1 / 4 of the volume of the aqueous extract and fermentation broth mixture.
[0073] Preparation Example 3
[0074] Example 3 of this preparation provides a method for preparing pine leaf extract, including the following steps:
[0075] Y1. Prepare pine needle powder that passes through a 100-mesh sieve and has a moisture content of 8%;
[0076] Y2. A compound bacterial culture was prepared by inoculating Lactobacillus CGMCC NO.0843 and yeast CGMCC NO.27154 into the fermentation base liquid (a 10 wt% glucose aqueous solution), with a viable count of 10⁻⁶ Lactobacillus CGMCC NO.0843 in the compound bacterial culture. 7 The viable count of yeast CGMCC NO.27154 was 10 CFU / mL. 7 CFU / mL; After uniformly mixing the pine leaf powder and the compound bacterial solution at a mass-volume ratio of 1g / mL, fermentation was carried out in an anaerobic environment at 32℃ and pH 5 for 72h, followed by ultraviolet sterilization and separation of fermentation broth and fermentation residue.
[0077] Y3. After mixing the fermentation residue with deionized water at a volume ratio of 1:10, heat to 95°C and keep warm for 2 hours, then filter and separate. Wash the filtrate with deionized water and combine the washing liquid and filtrate to obtain an aqueous extract.
[0078] Y4. The aqueous extract and fermentation broth were combined and ultrasonically mixed, and then concentrated under an argon atmosphere at 60°C to obtain the dwarf pine leaf extract; the volume of the dwarf pine leaf extract was 1 / 4 of the volume of the aqueous extract and fermentation broth mixture.
[0079] Preparation Example 4
[0080] Example 4 of this preparation provides a method for preparing a dwarf pine leaf extract, comprising the following steps:
[0081] Y1. Spread the pine needle powder (8% moisture content) that has passed through a 100-mesh sieve evenly in a steamer, and control the loose layer thickness of the pine needle powder to be 10mm. Then place the steamer 15cm away from the boiling water surface and continue to heat the boiling water to boiling. After steaming the pine needle powder for 2 hours, remove the steamer and let it cool to room temperature to obtain cooked powder.
[0082] Y2. A compound bacterial culture was prepared by inoculating Lactobacillus CGMCC NO.16136 and yeast CGMCC NO.27154 into the fermentation base liquid (10% glucose solution). The viable count of Lactobacillus CGMCC NO.16136 in the compound bacterial culture was 10-1. 7 The viable count of yeast CGMCC NO.27154 was 10 CFU / mL. 7CFU / mL; After uniformly mixing the matured powder and the compound bacterial solution at a mass-volume ratio of 1g / mL, fermentation was carried out in an anaerobic environment at 32℃ and pH 5 for 72h, followed by ultraviolet sterilization and separation of fermentation broth and fermentation residue.
[0083] Y3. After mixing the fermentation residue with deionized water at a volume ratio of 1:10, heat to 95°C and keep warm for 2 hours, then filter and separate. Wash the filtrate with deionized water and combine the washing liquid and filtrate to obtain an aqueous extract.
[0084] Y4. The aqueous extract and fermentation broth were combined and ultrasonically mixed, and then concentrated under an argon atmosphere at 60°C to obtain the dwarf pine leaf extract; the volume of the dwarf pine leaf extract was 1 / 4 of the volume of the aqueous extract and fermentation broth mixture.
[0085] Preparation Example 5
[0086] Example 5 of this preparation provides a method for preparing a dwarf pine leaf extract, comprising the following steps:
[0087] Y1. Spread the pine needle powder (8% moisture content) that has passed through a 100-mesh sieve evenly in a steamer, and control the loose layer thickness of the pine needle powder to be 10mm. Then place the steamer 15cm away from the boiling water surface and continue to heat the boiling water to boiling. After steaming the pine needle powder for 2 hours, remove the steamer and let it cool to room temperature to obtain cooked powder.
[0088] Y2. A compound bacterial culture was prepared by inoculating Lactobacillus CGMCC NO.0843 and yeast CGMCC NO.23732 into the fermentation base liquid (10% glucose solution). The viable count of Lactobacillus CGMCC NO.0843 in the compound bacterial culture was 10. 7 The viable count of yeast CGMCC NO.23732 was 10 CFU / mL. 7 CFU / mL; After uniformly mixing the matured powder and the compound bacterial solution at a mass-volume ratio of 1g / mL, fermentation was carried out in an anaerobic environment at 32℃ and pH 5 for 72h, followed by ultraviolet sterilization and separation of fermentation broth and fermentation residue.
[0089] Y3. After mixing the fermentation residue with deionized water at a volume ratio of 1:10, heat to 95°C and keep warm for 2 hours, then filter and separate. Wash the filtrate with deionized water and combine the washing liquid and filtrate to obtain an aqueous extract.
[0090] Y4. The aqueous extract and fermentation broth were combined and ultrasonically mixed, and then concentrated under an argon atmosphere at 60°C to obtain the dwarf pine leaf extract; the volume of the dwarf pine leaf extract was 1 / 4 of the volume of the aqueous extract and fermentation broth mixture.
[0091] Preparation Example 6
[0092] Example 6 of this preparation provides a method for preparing a dwarf pine leaf extract, comprising the following steps:
[0093] Y1. Spread the pine needle powder (8% moisture content) that has passed through a 100-mesh sieve evenly in a steamer, and control the loose layer thickness of the pine needle powder to be 10mm. Then place the steamer 15cm away from the boiling water surface and continue to heat the boiling water to boiling. After steaming the pine needle powder for 2 hours, remove the steamer and let it cool to room temperature to obtain cooked powder.
[0094] Y2. After mixing the aged powder with deionized water at a volume ratio of 1:10, heat to 95℃ and keep warm for 2 hours, then filter and separate. Wash the filtrate with deionized water, combine the washing liquid and the filtrate to obtain an aqueous extract, and concentrate the aqueous extract to 1 / 4 of the volume of the dwarf pine leaf extract under an argon atmosphere at 60℃.
[0095] Preparation Example 7
[0096] Example 7 of this preparation provides a method for preparing a dwarf pine leaf extract, comprising the following steps:
[0097] Y1. Pine leaf powder (8% moisture content) that has passed through a 100-mesh sieve is mixed with deionized water at a volume ratio of 1:10. The mixture is then heated to 95°C and kept at that temperature for 2 hours before being filtered. The filtrate is washed with deionized water, and the washing liquid and filtrate are combined to obtain an aqueous extract. The aqueous extract is then concentrated under an argon atmosphere at 60°C to a volume of 1 / 4 of the aqueous extract volume of pine leaf extract.
[0098] Example 1
[0099] This embodiment 1 provides a method for preparing degreased cotton paper, including the following steps:
[0100] S1. The degreased cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (8% by mass of tea polyphenol solution, with a mass ratio of degreased cotton to tea polyphenol of 1:0.3) for 10 min. Then, the mixture of degreased cotton and modified solution was beaten at 0.2 MPa for 40 min using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0101] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0102] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 15%.
[0103] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 2 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 22%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 5%.
[0104] Example 2
[0105] This embodiment 2 provides a method for preparing degreased cotton paper, including the following steps:
[0106] S1. The degreased cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (8% anthocyanin solution by mass, with a degreased cotton to anthocyanin mass ratio of 1:0.3) for 10 min. Then, the mixture of degreased cotton and modified solution was beaten at 0.2 MPa for 40 min using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0107] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0108] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 13%.
[0109] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 2 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 23%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 4%.
[0110] Example 3
[0111] This embodiment 3 provides a method for preparing degreased cotton paper, including the following steps:
[0112] S1. The defatted cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (4% anthocyanin and 4% tea polyphenols by mass, with a mass ratio of defatted cotton, anthocyanin, and tea polyphenols of 1:0.15:0.15) for 10 minutes. Then, the mixture of defatted cotton and modified solution was beaten at 0.2 MPa for 40 minutes using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0113] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0114] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 17%.
[0115] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 2 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 21%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 6%.
[0116] Example 4
[0117] This embodiment 4 provides a method for preparing degreased cotton paper, including the following steps:
[0118] S1. The defatted cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (4% anthocyanin and 4% tea polyphenols by mass, with a mass ratio of defatted cotton, anthocyanin, and tea polyphenols of 1:0.15:0.15) for 10 minutes. Then, the mixture of defatted cotton and modified solution was beaten at 0.2 MPa for 40 minutes using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0119] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0120] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 16%.
[0121] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 3 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 22%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 5%.
[0122] Example 5
[0123] This embodiment 5 provides a method for preparing degreased cotton paper, including the following steps:
[0124] S1. The defatted cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (4% anthocyanin and 4% tea polyphenols by mass, with a mass ratio of defatted cotton, anthocyanin, and tea polyphenols of 1:0.15:0.15) for 10 minutes. Then, the mixture of defatted cotton and modified solution was beaten at 0.2 MPa for 40 minutes using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0125] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0126] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 16%.
[0127] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 4 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 25%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 7%.
[0128] Example 6
[0129] This embodiment 6 provides a method for preparing degreased cotton paper, including the following steps:
[0130] S1. The defatted cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (4% anthocyanin and 4% tea polyphenols by mass, with a mass ratio of defatted cotton, anthocyanin, and tea polyphenols of 1:0.15:0.15) for 10 minutes. Then, the mixture of defatted cotton and modified solution was beaten at 0.2 MPa for 40 minutes using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0131] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0132] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 16%.
[0133] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 5 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 24%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 5%.
[0134] Example 7
[0135] This embodiment 7 provides a method for preparing degreased cotton paper, including the following steps:
[0136] S1. The defatted cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (4% anthocyanin and 4% tea polyphenols by mass, with a mass ratio of defatted cotton, anthocyanin, and tea polyphenols of 1:0.15:0.15) for 10 minutes. Then, the mixture of defatted cotton and modified solution was beaten at 0.2 MPa for 40 minutes using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0137] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0138] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 16%.
[0139] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 6 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 23%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 4%.
[0140] Example 8
[0141] This embodiment 8 provides a method for preparing degreased cotton paper, including the following steps:
[0142] S1. The defatted cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (4% anthocyanin and 4% tea polyphenols by mass, with a mass ratio of defatted cotton, anthocyanin, and tea polyphenols of 1:0.15:0.15) for 10 minutes. Then, the mixture of defatted cotton and modified solution was beaten at 0.2 MPa for 40 minutes using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0143] S2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0144] S3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 16%.
[0145] S4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 7 for 15 minutes, the secondary cotton paper is taken out and dried to the tertiary cotton paper with a moisture content of 21%. The tertiary cotton paper is then soaked in sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to the degreased cotton paper with a moisture content of 5%.
[0146] Comparative Example 1
[0147] Comparative Example 1 provides a method for preparing degreased cotton paper, comprising the following steps:
[0148] D1. The degreased cotton prepared in Preparation Example 1 was dispersed in deionized water and ultrasonically mixed for 10 min. Then, the mixture of degreased cotton and deionized water was pulped at 0.2 MPa for 40 min using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0149] D2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0150] D3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C in a nitrogen atmosphere to produce secondary cotton paper with a moisture content of 17%.
[0151] D4. After soaking the secondary cotton paper in the pine leaf extract (30°C) prepared in Preparation Example 2 for 15 minutes, the secondary cotton paper was removed and dried to a tertiary cotton paper with a moisture content of 20%. The tertiary cotton paper was then soaked in a sodium hypochlorite aqueous solution for 30 minutes for bleaching treatment, and then dried to a degreased cotton paper with a moisture content of 6%.
[0152] Comparative Example 2
[0153] Comparative Example 2 provides a method for preparing degreased cotton paper, comprising the following steps:
[0154] D1. The defatted cotton prepared in Preparation Example 1 was ultrasonically mixed in a modified solution (4% anthocyanin and 4% tea polyphenols by mass, with a mass ratio of defatted cotton, anthocyanin, and tea polyphenols of 1:0.15:0.15) for 10 min. Then, the mixture of defatted cotton and modified solution was beaten at 0.2 MPa for 40 min using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0155] D2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0156] D3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C under a nitrogen atmosphere to a secondary cotton paper with a moisture content of 17%. After bleaching the secondary cotton paper by soaking it in a sodium hypochlorite aqueous solution for 30 minutes, dry it again to a degreased cotton paper with a moisture content of 6%.
[0157] Comparative Example 3
[0158] Comparative Example 3 provides a method for preparing degreased cotton paper, comprising the following steps:
[0159] D1. The degreased cotton prepared in Preparation Example 1 was dispersed in deionized water and ultrasonically mixed for 10 min. Then, the mixture of degreased cotton and deionized water was pulped at 0.2 MPa for 40 min using a disc mill at a speed of 2500 rpm and a gap of 0.3 mm to obtain fiber pulp.
[0160] D2. Use a 100-mesh forming screen to filter from the fiber slurry. After the degreased cotton fibers completely cover the surface of the forming screen, remove the forming screen from the fiber slurry and let it stand until no liquid flows down. Then peel off the primary cotton paper from the surface of the forming screen.
[0161] D3. Transfer the primary cotton paper to an atmosphere furnace and dry it at 40°C under a nitrogen atmosphere to a secondary cotton paper with a moisture content of 17%. After bleaching the secondary cotton paper by soaking it in a sodium hypochlorite aqueous solution for 30 minutes, dry it again to a degreased cotton paper with a moisture content of 6%.
[0162] The degreased cotton paper prepared in Examples 1 to 8 and Comparative Examples 1 to 3 was subjected to the following tests:
[0163] Water absorption test: Weigh the degreased cotton paper before and after saturation water absorption, and calculate the saturation water absorption rate of the degreased cotton paper. Saturation water absorption rate = weight gain after saturation water absorption / mass after saturation water absorption. The results are shown in Table 1 below. After irradiating the degreased cotton paper with a 15W xenon lamp in a dust-free and transparent environment for 72 hours, the water absorption test was carried out again. The results are shown in Table 1 below.
[0164] Water absorption rate test: Prepare a red dye solution and insert degreased cotton paper into the dye solution at a 45° angle, controlling the side insertion depth of the degreased cotton paper to be 2 mm. The water absorption rate of the degreased cotton paper to the solution is calculated as shown in Table 2 below. After irradiating the degreased cotton paper with a 15W xenon lamp in a dust-free transparent environment for 72 hours, the water absorption rate test is carried out again, and the results are shown in Table 2 below.
[0165] Antibacterial performance test: Based on the method described in Part 3 of GB / T20944.3-2008 "Antibacterial properties of textiles", Staphylococcus aureus was selected as the test strain to test the antibacterial performance of the degreased cotton paper. The initial antibacterial rate of the degreased cotton paper was determined, and the results are shown in Table 3 below. After the degreased cotton paper was irradiated with a 15W xenon lamp in a dust-free transparent environment for 72 hours, the antibacterial performance test was carried out again, and the results are shown in Table 3 below.
[0166] Water-locking test: After the degreased cotton paper was saturated with red dye solution, the water was drained and a piece of cotton cloth of the same area as the degreased cotton paper was attached to the surface of the cotton paper. After applying a 1kg weight evenly for 10 minutes, the ratio of the red area on the surface of the cotton cloth to the side area of the cotton cloth was observed, as shown in Table 4 below. Then, the degreased cotton paper was irradiated with a 15W xenon lamp in a dust-free and transparent environment for 72 hours, and the water-locking test was carried out again. The results are shown in Table 4 below.
[0167] Each of the above tests was repeated three times and the average value was calculated.
[0168] Table 1. Water absorption test results
[0169]
[0170] Table 2 Results of water absorption rate test
[0171]
[0172] Table 3 Results of antibacterial test
[0173]
[0174] Table 4 Results of Water Retention Test
[0175]
[0176] While embodiments of the present invention have been described in detail above, it will be apparent to those skilled in the art that various modifications and variations can be made to these embodiments. However, it should be understood that such modifications and variations fall within the scope and spirit of the invention as set forth in the claims. Furthermore, the invention described herein may have other embodiments and can be implemented or carried out in various ways.
Claims
1. A method for preparing degreased cotton paper that is not easily contaminated, characterized in that, Includes the following steps: Fiber pulp is prepared by pulping degreased cotton in a modified solution; Primary cotton paper is filtered from the fiber pulp using a forming mesh; the primary cotton paper is dried to obtain secondary cotton paper with a moisture content of 10-20%; the secondary cotton paper is soaked in pine leaf extract for modification, then removed and dried to obtain degreased cotton paper with a moisture content of 3-8%. The preparation method of the dwarf pine leaf extract includes: steaming dwarf pine leaf powder in boiling water for 1-2 hours to obtain cooked powder; mixing the cooked powder with a compound bacterial solution, fermenting and then sterilizing; collecting the fermentation liquid and fermentation residue; keeping the fermentation residue in deionized water at 90-100℃ for 1-2 hours and then separating the aqueous extract; combining the aqueous extract and the fermentation liquid and concentrating under an inert atmosphere to obtain the dwarf pine leaf extract. When the matured powder is mixed with the compound bacterial solution, the compound bacterial solution includes a fermentation base liquid and a mixed fermentation bacteria inoculated in the fermentation base liquid, and the mixed fermentation bacteria include Lactobacillus CGMCC NO.0843 and Saccharomyces CGMCC NO.27154. When degreased cotton is pulped in a modified solution, the modified solution includes 5-10% by mass of active polyphenols, and the active polyphenols include at least one of tea polyphenols, anthocyanins, resveratrol, and curcumin. The solvent in the modified solution is deionized water.
2. The preparation method according to claim 1, characterized in that, The fermentation base liquid includes a sugar source, and the sugar source includes at least one of glucose and maltose; and / or, the inoculation concentration of the fermentation mixed bacteria in the fermentation base liquid is 10. 6 -10 7 CFU / mL; and / or, the ratio of viable lactobacilli to viable yeast in the fermentation mixture is (0.5-1):
1.
3. The preparation method according to claim 1, characterized in that, After mixing the matured powder with the compound bacterial solution, the mixture is fermented in an anaerobic environment at 25-37℃ and pH 5-6 for 70-74 hours and then sterilized; the sterilization includes at least one of high-temperature sterilization and ultraviolet sterilization.
4. The preparation method according to claim 1, characterized in that, The dwarf pine needle powder is sieved through a 100-200 mesh sieve and then steamed in boiling water; and / or, the moisture content of the dwarf pine needle powder is 5-10%; and / or, the mixing ratio of the viable bacteria in the compound bacterial solution to the cooked powder is 10:
1. 6 -10 7 CFU / g; and / or, the volume of the pine leaf extract is 1 / 4 to 1 / 3 of the volume of the water extract and the fermentation broth.
5. The preparation method according to claim 1, characterized in that, After ultrasonically mixing the degreased cotton in the modified solution for 10-15 minutes, it is then beaten at a speed of 2000-3000 rpm and a gap of 0.1-0.5 mm for 30-45 minutes to prepare a fiber slurry.
6. The preparation method according to claim 1, characterized in that, Secondary cotton paper is soaked in pine leaf extract at 30-35℃ for 15-20 minutes, then dried to a moisture content of 20-25% to produce tertiary cotton paper. Tertiary cotton paper is then bleached in bleaching solution and dried to a moisture content of 3-8% to produce degreased cotton paper.
7. The preparation method according to claim 1, characterized in that, The method for preparing the degreased cotton includes: carding the cotton fibers after removing impurities to obtain cotton linters; degreasing the cotton linters in an alkaline solution and then bleaching them to obtain degreased cotton.
Citation Information
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