CN109137133B - Preparation method of loofah sponge cellulose/chitosan composite fiber - Google Patents
Preparation method of loofah sponge cellulose/chitosan composite fiber Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
Abstract
The invention belongs to the technical field of deep processing of plant fibers, and particularly discloses an oil-absorbing hydrophobic silkA preparation method of melon collateral composite fiber. The invention uses pectase: laccase: enzymolysis of dried retinervus Luffae fructus fiber and chitosan after enzymolysis of cellulase and papain with complex enzyme composed of hemicellulase sequentially passes through NMMO & H2Performing O solution treatment, defoaming treatment and other steps to obtain modified loofah sponge fibers, mixing the modified loofah sponge fibers with chitosan subjected to enzyme treatment, and completely dissolving the modified loofah sponge fibers and the chitosan in a dimethylformamide solution at the temperature of 50 +/-5 ℃ to obtain a loofah sponge cellulose/chitosan electrostatic spinning solution; and finally, carrying out electrostatic spinning treatment and crosslinking heat treatment on the loofah sponge cellulose/chitosan to obtain the loofah sponge cellulose/chitosan composite fiber. The brand-new loofah sponge cellulose/chitosan composite fiber prepared by the invention has the characteristics of high oil absorption rate, low water absorption rate and the like, and has wide market prospect.
Description
Technical Field
The invention belongs to the technical field of deep processing of plant fibers, and particularly relates to a preparation method of an oil-absorbing hydrophobic loofah sponge composite fiber.
Background
The retinervus Luffae fructus is the vascular bundle of mature fruit of Cucurbitaceae plant retinervus Luffae fructus or Guangdong retinervus Luffae fructus. Has the effects of clearing and activating the channels and collaterals, and detoxifying and reducing swelling. In folk, the loofah sponge is often dried in the sun and then used for washing dishes, oil absorption components contained in the loofah sponge are utilized, however, cellulose, hemicellulose and lignin are contained in the loofah sponge, the loofah sponge is not storable and can often mildew, and the like, the oil absorption rate is not high, the oil absorption effect is not satisfactory, and a novel material is urgently needed to replace the traditional loofah sponge.
Chitosan is a natural cationic polymer, and is extracted from shells of crustaceans and arthropods and cell walls of lower plants such as fungi and algae. Has good film forming property, biocompatibility, biodegradability and excellent antibacterial and bacteriostatic effects, thus being widely applied to the fields of medicine, food, chemical industry, environmental protection and the like.
Cellulose is a natural renewable polymer material widely existing on the earth and has incomparable advantages compared with petroleum. Cellulose membrane materials have an important position in the membrane industry due to their good mechanical strength, air permeability, biodegradability and other properties. Loofah sponge is an important cellulose resource, is a three-dimensional reticular structure formed by companion substances such as cellulose, hemicellulose, lignin and the like, and in order to utilize the loofah sponge cellulose resource, the cellulose companion substances are required to be treated to remove the hemicellulose and the lignin so as to separate single fibers.
The literature reports that the natural loofah sponge fiber is pretreated by a combined treatment method of alkali and hydrogen peroxide. The results show that NaOH and H are used2O2The optimal process for treating the mixed solution is 10 percent of H2O2And 10% NaOH for 2 h. Under the process condition, the degumming rate of the loofah sponge fiber is 39%, the cellulose content is 80.51%, and the degumming rate is obviously improved compared with 66.19% before the treatment. The pretreatment process changes the thick fiber bundle (2000 μm) of the loofah sponge into single fiber with the diameter of about 20 μm, and the moisture regain of the loofah sponge fiber is improved to 12% from the original 9.25%.
If the loofah sponge fiber is used for oil absorption, the water absorption rate of the loofah sponge fiber needs to be reduced, and the oil absorption rate of the loofah sponge fiber needs to be improved.
Disclosure of Invention
The invention provides a preparation method of loofah sponge cellulose/chitosan composite fiber, aiming at overcoming the defects of natural loofah sponge fiber, reducing the water absorption rate and improving the oil absorption rate, and the specific preparation process is as follows:
(1) magnetically stirring retinervus Luffae fructus fiber in water solution, and oven drying at below 110 deg.C to obtain dry retinervus Luffae fructus fiber.
② using pectinase: laccase: performing enzymolysis treatment on the dried loofah sponge fibers by using a compound enzyme consisting of hemicellulase;
thirdly, preparing a suspension with the chitosan content of 5-15%, swelling with deionized water for 15-60 min, gradually adding an acetic acid solution with the concentration of 2-5% to dissolve the chitosan, and uniformly stirring at the temperature of 40 +/-5 ℃ to completely dissolve the chitosan to obtain a chitosan solution;
adding a complex enzyme of cellulase and papain into the chitosan solution, carrying out enzymolysis for 10-120 min, and evaporating water in the chitosan solution at 90-100 ℃ after the enzymolysis is finished to obtain enzyme-treated chitosan;
⑤ adding the enzymolyzed retinervus Luffae fructus fiber into NMMO. H2Adding 0.05-0.4% propyl gallate into the O solution, and reacting at 90 + -3 deg.C for 1-5H to obtain retinervus Luffae fructus cellulose/NMMO. H2O solution;
⑥ the obtained retinervus Luffae fructus cellulose/NMMO. H2Defoaming the O solution at the temperature of 80-95 ℃ and the vacuum degree of 0.1-0.6 MPa for 1-10 h;
⑦ defoaming retinervus Luffae fructus cellulose/NMMO. H2Adding 0.1-0.8% of boric acid and 0.5-2.5% of sodium acetate into the O solution, and placing the mixture in a water area at the temperature of 70-95 ℃ for mixing, stirring and reacting for 30-120 min to obtain a modified loofah sponge cellulose mixed solution;
eighthly, concentrating and drying the modified loofah sponge cellulose mixed solution to obtain modified loofah sponge cellulose;
ninthly, completely dissolving the modified loofah sponge cellulose and the chitosan after enzyme treatment in a dimethylformamide solution at the temperature of 50 +/-5 ℃ to obtain loofah sponge cellulose/chitosan electrostatic spinning solution;
(10) electrostatic spinning loofah sponge cellulose/chitosan to obtain loofah sponge cellulose/chitosan fiber;
⑪, placing the loofah sponge cellulose/chitosan fiber at 90 +/-3 ℃ for crosslinking and heat treatment for 5-8 h to obtain the loofah sponge cellulose/chitosan composite fiber.
Further, the enzymolysis treatment of the dried loofah sponge fiber is specifically carried out for 2-24 hours at the temperature of 55 ℃.
Further, the pectinase: laccase: the addition amount of the compound enzyme composed of the hemicellulase is 1-8% of the mass of the dried loofah sponge.
Further, the pectinase: laccase: in the compound enzyme composed of hemicellulase, pectinase: laccase: the proportion of the hemicellulase is 1:0.5: 0.5-1: 2: 2.
Further, the enzymolyzed retinervus Luffae fructus fiber is added with NMMO. H2The material-liquid ratio of the O solution mixture is 1: 2-1: 10 (m/V).
Further, the NMMO. H2In O solution, NMMO. H2The mass fraction of O is 11-17.5%.
Further, in the loofah sponge cellulose/chitosan electrostatic spinning solution, the content of the modified loofah sponge cellulose is 2-10%, the content of the chitosan after enzyme treatment is 0.5-5%,
further, the electrostatic spinning conditions are as follows: the spinning voltage is 5-20 kV, the solution flow rate is 0.5-2 mL/h, and the receiving distance of the roller is 5-15 cm.
Advantageous effects
The invention carries out modification treatment on the natural loofah sponge fiber on the basis of the natural loofah sponge fiber, removes substances which are easy to absorb water, mildew and rot from the natural loofah sponge fiber, adds complex enzyme treatment, can remove colloids such as hemicellulose, lignin and the like on the surface of the loofah sponge fiber by the complex enzyme treatment, and has clear and visible fibrous striations and exposed single cellulose fibers. The invention dissolves chitosan by acetic acid, then combines with modified loofah sponge fiber, and finally obtains a brand-new loofah sponge cellulose/chitosan composite fiber through electrostatic spinning, the loofah sponge cellulose/chitosan composite fiber not only does not contain colloid components in natural loofah sponge, but also enables the water absorption rate of the new fiber to be basically reduced to below 3% through chitosan and assistance, and the oil absorption rate of the new fiber can reach 12.86g +/-0.97 g/g, which far exceeds the oil absorption rate of similar fibers in markets.
The loofah sponge cellulose/chitosan composite fiber prepared by the invention can be used for preparing household washing article fibers, can quickly remove oil stains on washed articles, and is soft in texture and good in use comfort. Secondly, the invention can also be used as the adsorption fiber for offshore floating oil pollution, has large oil stain adsorption quantity, can be repeatedly used, and has high oil absorption efficiency and low cost.
Detailed Description
In this example, loofah sponge (naturally grown and mature in Anhui nest lake); the hemicellulase has an enzyme activity of 200u/mg, a temperature range of 30-60 ℃, and a pH value of: 4.0-5.5, wherein the laccase has an enzymatic activity of more than or equal to 10u/mg and a pH value: 3.0-5.5, the optimum temperature is 50 ℃, pectinase is used, the enzyme activity is 3 ten thousand u/g, NMMO with the mass fraction of 50% is purchased from Shanghai Jinsui Biotech Co., Ltd, and other reagents are analytically pure.
Example 1
A method for preparing loofah sponge cellulose/chitosan composite fiber comprises the following specific technical scheme:
1. cutting loofah sponge into fibers with the length of 0.5-3 cm, cooking in an electric heating constant-temperature water bath, magnetically stirring for 30min, filtering after stirring, and drying in a drying oven at 105 ℃ to obtain the dry loofah sponge fibers.
2. Treating the dried loofah sponge fibers with the complex enzyme: with pectinase: laccase: performing enzymolysis on a complex enzyme composed of hemicellulase for 12 hours at the temperature of 55 +/-3 ℃ to obtain the loofah sponge fiber after enzymolysis, wherein the addition amount of the complex enzyme is 5% of the mass of the dry loofah sponge, and in the complex enzyme, the mass ratio of pectinase: laccase: the ratio of the hemicellulase to the enzyme is 1:1: 1.
3. Preparing a suspension with the chitosan content of 10%, swelling with deionized water for 30min, gradually adding an acetic acid solution with the concentration of 3% to dissolve the chitosan, stirring uniformly at the temperature of 40 +/-5 ℃, and standing for 4h after the chitosan is completely dissolved to obtain a chitosan solution.
4. Adding complex enzyme of cellulase and papain into chitosan solution, performing enzymolysis for 30min, and evaporating water in the chitosan solution at 95 deg.C to obtain enzyme-treated chitosan; wherein the mixing ratio of the cellulase to the papain is 1:1, and the addition amount of the complex enzyme is 1% (mass ratio).
5. Adding the enzymolyzed retinervus Luffae fructus fiber into 13.3% NMMO H at a ratio of 1:5 (m/V)2Adding into O solution at the same time0.1% propyl gallate, reacting at 90 + -3 deg.C for 2 hr to obtain retinervus Luffae fructus cellulose/NMMO. H2And (4) O solution.
6. The prepared loofah sponge cellulose/NMMO H2And (3) placing the O solution into a vacuum drying oven, defoaming the O solution for 3 hours at the temperature of 90 ℃ and under the vacuum degree of 0.2MPa, and taking out the O solution to obtain uniform and transparent brown solution.
7. Defoaming loofah sponge cellulose/NMMO H2Adding 0.3% boric acid and 1% sodium acetate into the O solution, mixing and stirring for reaction at 85 deg.C in water for 60min to obtain modified retinervus Luffae fructus cellulose mixed solution.
8. Concentrating and drying the modified loofah sponge cellulose mixed solution to obtain the modified loofah sponge cellulose.
9. Mixing the modified loofah sponge cellulose and chitosan treated by enzyme to obtain a loofah sponge cellulose/chitosan mixture, and completely dissolving the loofah sponge cellulose/chitosan mixture in a dimethyl formamide solution at the temperature of 50 +/-5 ℃, wherein the content of the modified loofah sponge cellulose is 3%, and the content of the chitosan treated by enzyme is 1%, so as to obtain the loofah sponge cellulose/chitosan electrostatic spinning solution.
10. Electrostatic spinning is carried out on the loofah sponge cellulose/chitosan under the conditions that the liquid spinning voltage is 10 kV, the solution flow rate is 1mL/h and the roller receiving distance is 15cm, so as to obtain the loofah sponge cellulose/chitosan fiber.
11. Placing the loofah sponge cellulose/chitosan fiber at 90 ℃ for crosslinking heat treatment for 6 hours to obtain the loofah sponge cellulose/chitosan composite fiber.
Adopting a GB/T3903.33-2008 sheet static water absorption method, taking a sample, placing the sample in a constant temperature and humidity chamber for 24 hours, and weighing m0Immersing in distilled water for 6h, taking out the sample until no water drops, and weighing the weight m1。
Water absorption = (m)1-m0)/m0*100%（%）
The normal hexane (simulated oil substances) adsorption capacity of the loofah sponge cellulose/chitosan composite fiber prepared by the embodiment can reach 12.86g +/-0.97 g/g, and the loofah sponge cellulose/chitosan composite fiber has a strong oil absorption effect, and the water absorption rate is 1.56 +/-0.15%.
Example 2
A method for preparing loofah sponge cellulose/chitosan composite fiber comprises the following specific technical scheme:
1. cutting loofah sponge into fibers with the length of 0.5-3 cm, cooking in an electric heating constant-temperature water bath, magnetically stirring for 10min, filtering after stirring, and drying in a drying oven at 110 ℃ to obtain the dry loofah sponge fibers.
2. Treating the dried loofah sponge fibers with the complex enzyme: with pectinase: laccase: performing enzymolysis on a complex enzyme composed of hemicellulase at 55 ℃ for 2h to obtain the loofah sponge fiber after enzymolysis, wherein the addition amount of the complex enzyme is 1% of the mass of the dry loofah sponge, and in the complex enzyme, the mass ratio of pectinase: laccase: the hemicellulase ratio was 1:2: 2.
3. Preparing a suspension with the chitosan content of 5%, swelling with deionized water for 60min, gradually adding an acetic acid solution with the concentration of 5% to dissolve the chitosan, stirring uniformly at the temperature of 40 +/-5 ℃, and standing for 0.5h after the chitosan is completely dissolved to obtain a chitosan solution.
4. Adding complex enzyme of cellulase and papain into chitosan solution, performing enzymolysis for 10min, and evaporating water in the chitosan solution at 100 deg.C to obtain enzyme-treated chitosan; wherein the mixing ratio of the cellulase to the papain is 3:1, and the addition amount of the complex enzyme is 4% (mass ratio).
5. Adding the enzymolyzed retinervus Luffae fructus fiber into 17.5% NMMO H at a ratio of 1:2 (m/V)2Adding 0.4% propyl gallate into O solution, and reacting at 90 + -3 deg.C for 1 hr to obtain retinervus Luffae fructus cellulose/NMMO. H2And (4) O solution.
6. The prepared loofah sponge cellulose/NMMO H2And (3) placing the O solution into a vacuum drying oven, defoaming the O solution for 1 hour at the temperature of 80 ℃ and under the vacuum degree of 0.1MPa, and taking out the O solution to obtain uniform and transparent brown solution.
7. Defoaming loofah sponge cellulose/NMMO H2Adding into O solutionAdding 0.1% boric acid and 0.5% sodium acetate, mixing and stirring at 70 deg.C in water, and reacting for 30min to obtain modified retinervus Luffae fructus cellulose mixed solution.
8. Concentrating and drying the modified loofah sponge cellulose mixed solution to obtain the modified loofah sponge cellulose.
9. Mixing the modified loofah sponge cellulose and chitosan treated by enzyme to obtain a loofah sponge cellulose/chitosan mixture, and completely dissolving the loofah sponge cellulose/chitosan mixture in a dimethylformamide solution at the temperature of 50 +/-5 ℃, wherein the content of the modified loofah sponge cellulose is 2%, and the content of the chitosan treated by enzyme is 0.5%, so as to obtain the loofah sponge cellulose/chitosan electrostatic spinning solution.
10. Electrostatic spinning is carried out on the loofah sponge cellulose/chitosan under the conditions that the liquid spinning voltage is 5 kV, the solution flow rate is 0.5mL/h and the roller receiving distance is 15cm, so as to obtain the loofah sponge cellulose/chitosan fiber.
11. Placing the loofah sponge cellulose/chitosan fiber at the temperature of 90 +/-2 ℃ for crosslinking and heat treatment for 5 hours to obtain the loofah sponge cellulose/chitosan composite fiber.
Adopting a GB/T3903.33-2008 sheet static water absorption method, taking a sample, placing the sample in a constant temperature and humidity chamber for 24 hours, and weighing m0Immersing in distilled water for 6h, taking out the sample until no water drops, and weighing the weight m1。
Water absorption = (m)1-m0)/m0*100%（%）
The normal hexane (simulated oil substances) adsorption capacity of the loofah sponge cellulose/chitosan composite fiber prepared by the embodiment can reach 10.23g +/-0.18 g/g, and the loofah sponge cellulose/chitosan composite fiber has a strong oil absorption effect, and the water absorption rate is 0.18 +/-0.04%.
Example 3
A method for preparing loofah sponge cellulose/chitosan composite fiber comprises the following specific technical scheme:
1. cutting retinervus Luffae fructus into fibers with length of 3cm, steaming in electric heating constant temperature water bath, magnetically stirring for 50min, filtering, and oven drying at below 110 deg.C to obtain dry retinervus Luffae fructus fiber.
2. Treating the dried loofah sponge fibers with the complex enzyme: with pectinase: laccase: performing enzymolysis on a complex enzyme composed of hemicellulase for 24 hours at the temperature of 55 +/-3 ℃ to obtain the loofah sponge fiber after enzymolysis, wherein the addition amount of the complex enzyme is 8% of the mass of the dry loofah sponge, and in the complex enzyme, the mass ratio of pectinase: laccase: the hemicellulase ratio was 1:0.5: 0.5.
3. Preparing a suspension with the chitosan content of 15%, swelling with deionized water for 15min, gradually adding an acetic acid solution with the concentration of 2% to dissolve the chitosan, stirring uniformly at the temperature of 40 +/-5 ℃, and standing for 12h after the chitosan is completely dissolved to obtain a chitosan solution.
4. Adding complex enzyme of cellulase and papain into chitosan solution, performing enzymolysis for 120min, and evaporating water in the chitosan solution at 100 deg.C to obtain enzyme-treated chitosan; wherein the mixing ratio of the cellulase to the papain is 1:2, and the addition amount of the complex enzyme is 2% (mass ratio).
5. Adding the enzymolyzed retinervus Luffae fructus fiber into 11% of NMMO H at a material-liquid ratio of 1:10 (m/V)2Adding 0.05% propyl gallate into O solution, and reacting at 90 + -3 deg.C for 5 hr to obtain retinervus Luffae fructus cellulose/NMMO. H2And (4) O solution.
6. The prepared loofah sponge cellulose/NMMO H2And (3) placing the O solution into a vacuum drying oven, defoaming the O solution for 10 hours at the temperature of 95 ℃ and the vacuum degree of 0.6MPa, and taking out the O solution to obtain uniform and transparent brown solution.
7. Defoaming loofah sponge cellulose/NMMO H2Adding 0.8% boric acid and 2.5% sodium acetate into the O solution, mixing and stirring for reaction at 95 deg.C in water for 120min to obtain modified retinervus Luffae fructus cellulose mixed solution.
8. Concentrating and drying the modified loofah sponge cellulose mixed solution to obtain the modified loofah sponge cellulose.
9. Mixing the modified loofah sponge cellulose and chitosan treated by enzyme to obtain a loofah sponge cellulose/chitosan mixture, and completely dissolving the loofah sponge cellulose/chitosan mixture in a dimethyl formamide solution at the temperature of 50 +/-5 ℃, wherein the content of the modified loofah sponge cellulose is 10%, and the content of the chitosan treated by enzyme is 5%, so as to obtain the loofah sponge cellulose/chitosan electrostatic spinning solution.
10. Electrostatic spinning is carried out on the loofah sponge cellulose/chitosan under the conditions that the liquid spinning voltage is 20 kV, the solution flow rate is 2mL/h and the roller receiving distance is 10 cm, so as to obtain the loofah sponge cellulose/chitosan fiber.
11. Placing the loofah sponge cellulose/chitosan fiber at the temperature of 90 +/-3 ℃ for crosslinking and heat treatment for 8 hours to obtain the loofah sponge cellulose/chitosan composite fiber.
Adopting a GB/T3903.33-2008 sheet static water absorption method, taking a sample, placing the sample in a constant temperature and humidity chamber for 24 hours, and weighing m0Immersing in distilled water for 6h, taking out the sample until no water drops, and weighing the weight m1。
Water absorption = (m)1-m0)/m0*100%（%）
The normal hexane (simulated oil substances) adsorption capacity of the loofah sponge cellulose/chitosan composite fiber prepared by the embodiment can reach 11.08g +/-0.53 g/g, and the loofah sponge cellulose/chitosan composite fiber has a strong oil absorption effect, and the water absorption rate is 2.21 +/-0.03%.
Claims (8)
1. A preparation method of loofah sponge cellulose/chitosan composite fiber is characterized by comprising the following steps: the method comprises the following steps:
magnetically stirring loofah sponge fibers in an aqueous solution, and drying at the temperature of below 110 ℃ after stirring to obtain dry loofah sponge fibers;
② using pectinase: laccase: performing enzymolysis treatment on the dried loofah sponge fibers by using a compound enzyme consisting of hemicellulase;
thirdly, preparing a suspension with the chitosan content of 5-15%, swelling with deionized water for 15-60 min, gradually adding an acetic acid solution with the concentration of 2-5% to dissolve the chitosan, and uniformly stirring at the temperature of 40 +/-5 ℃ to completely dissolve the chitosan to obtain a chitosan solution;
adding a complex enzyme of cellulase and papain into the chitosan solution, carrying out enzymolysis for 10-120 min, and evaporating water in the chitosan solution at 90-100 ℃ after the enzymolysis is finished to obtain enzyme-treated chitosan;
⑤ adding the enzymolyzed retinervus Luffae fructus fiber into NMMO. H2Adding 0.05-0.4% propyl gallate into the O solution, and reacting at 90 + -3 deg.C for 1-5H to obtain retinervus Luffae fructus cellulose/NMMO. H2O solution;
⑥ the obtained retinervus Luffae fructus cellulose/NMMO. H2Defoaming the O solution at the temperature of 80-95 ℃ and the vacuum degree of 0.1-0.6 MPa for 1-10 h;
⑦ defoaming retinervus Luffae fructus cellulose/NMMO. H2Adding 0.1-0.8% of boric acid and 0.5-2.5% of sodium acetate into the O solution, and placing the mixture in a water bath at the temperature of 70-95 ℃ to mix and react for 30-120 min to obtain a modified loofah sponge cellulose mixed solution;
eighthly, concentrating and drying the modified loofah sponge cellulose mixed solution to obtain modified loofah sponge cellulose;
ninthly, completely dissolving the modified loofah sponge cellulose and the chitosan after enzyme treatment in a dimethylformamide solution at the temperature of 50 +/-5 ℃ to obtain loofah sponge cellulose/chitosan electrostatic spinning solution;
electrostatic spinning loofah sponge cellulose/chitosan to obtain loofah sponge cellulose/chitosan fiber;
⑪, placing the loofah sponge cellulose/chitosan fiber at 90 +/-3 ℃ for crosslinking and heat treatment for 5-8 h to obtain the loofah sponge cellulose/chitosan composite fiber.
2. The method for preparing loofah sponge cellulose/chitosan composite fiber according to claim 1, which is characterized in that: the enzymolysis treatment of the dried loofah sponge fiber is specifically carried out for 2-24 hours at the temperature of 55 ℃.
3. The method for preparing loofah sponge cellulose/chitosan composite fiber according to claim 1, which is characterized in that: the pectase is: laccase: the addition amount of the compound enzyme composed of the hemicellulase is 1-8% of the mass of the dried loofah sponge.
4. The method for preparing loofah sponge cellulose/chitosan composite fiber according to claim 1, which is characterized in that: the pectase is: laccase: in the compound enzyme composed of hemicellulase, pectinase: laccase: the proportion of the hemicellulase is 1:0.5: 0.5-1: 2: 2.
5. The method for preparing loofah sponge cellulose/chitosan composite fiber according to claim 1, which is characterized in that: adding the enzymolysis retinervus Luffae fructus fiber into NMMO. H2The material-liquid ratio of the O solution mixture is 1: 2-1: 10 (m/V).
6. The method for preparing loofah sponge cellulose/chitosan composite fiber according to claim 1, which is characterized in that: the NMMO. H2In O solution, NMMO. H2The mass fraction of O is 11-17.5%.
7. The method for preparing loofah sponge cellulose/chitosan composite fiber according to claim 1, which is characterized in that: in the loofah sponge cellulose/chitosan electrostatic spinning solution, the content of modified loofah sponge cellulose is 2-10%, and the content of chitosan after enzyme treatment is 0.5-5%.
8. The method for preparing loofah sponge cellulose/chitosan composite fiber according to claim 1, which is characterized in that: the electrostatic spinning conditions are as follows: the spinning voltage is 5-20 kV, the solution flow rate is 0.5-2 mL/h, and the receiving distance of the roller is 5-15 cm.
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| JPH07179649A (en) * | 1991-01-23 | 1995-07-18 | Snow Brand Milk Prod Co Ltd | Preparation of composite porous body made of vegetable fiber and chitosan |
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