Electrochemical and biological enzyme combined degumming method for industrial hemp fibers

Abstract

The invention belongs to the technical field of biological degumming, and particularly relates to an electrochemical combined biological enzyme degumming method for industrial hemp fibers, which comprises the following steps: forming a good pre-wetting effect by using a penetrant, and then carrying out primary degumming by using a biological enzyme compound liquid, and finally, forming a biological enzyme-electrolysis composite degumming system by using an alkaline pectinase-sodium carbonate buffer solution, and carrying out electrolysis degumming to realize gradient degumming, thereby obtaining the industrial hemp fiber with good degumming. According to the method, the problem that the degumming effect of the industrial hemp fibers is common is solved, an electrochemical-biological enzyme composite enzyme removal system is formed by utilizing preliminary degumming of the composite biological enzyme and a biological enzyme matched electrolysis system, and the enzyme removal effect is greatly improved.

Description

Technical Field

[0001] The invention belongs to the technical field of biological degumming, and in particular relates to an electrochemical combined with biological enzyme degumming method for industrial hemp fibers. Background Art

[0002] my country is the country with the richest hemp resources, with industrial hemp production ranking first in the world and one of the earliest hemp resources used by humans. Industrial hemp fiber is a green and ecological fiber with excellent properties such as moisture absorption, breathability, antibacterial properties, and mildew resistance. Furthermore, textiles made from industrial hemp fiber offer breathable, cooling, antibacterial, and antiseptic properties. However, industrial hemp fiber has an unpleasant feel and a certain itchiness, which seriously hinders its application. Therefore, a suitable degumming method is needed to reduce the discomfort of industrial hemp fiber.

[0003] Current degumming methods include physical degumming, chemical degumming, and biological degumming. Physical degumming can only degumming industrial hemp fiber to a certain extent, with average degumming effect and poor stability. Chemical degumming utilizes the difference in chemical properties between cellulose and colloid components and removes colloid in combination with chemical treatment. However, this treatment method has a long process flow, high energy consumption, high water consumption, high cost, and serious pollution. Although biological degumming has the advantages of being simple and easy to operate and pollution-free, the industrial hemp fiber after degumming still contains a large amount of colloid that has not been stripped off, and the product quality stability is poor. In view of the defects of existing processes, industrial hemp fiber needs a degumming method that can not only completely remove the colloid, but also maintain stable product quality. Summary of the Invention

[0004] In response to the problems in the prior art, the present invention provides a method for electrochemical combined with bio-enzymatic degumming of industrial hemp fiber, which solves the problem of general degumming effect of industrial hemp fiber. The method utilizes the preliminary degumming of composite bio-enzymes and the bio-enzyme combined electrolysis system to form an electrochemical-bio-enzyme composite degumming system, which greatly improves the degumming effect.

[0005] In order to achieve the above technical objectives, the technical solution of the present invention is: A method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber comprises the following steps: Step 1: placing industrial hemp fiber in water, adding a penetrant, and ultrasonically treating the fiber for 10-20 minutes, filtering, and air-drying to obtain pretreated industrial hemp fiber. The mass ratio of the industrial hemp fiber to water is 1:5-7. The penetrant is JFC, and the concentration of the penetrant in water is 0.05-0.08%. The ultrasonic treatment temperature is 30-40° C., the ultrasonic frequency is 80-100 kHz, and the concentration after drying is 20-30° C. This step utilizes the solubility and permeability of the penetrant in water to directly penetrate into the industrial hemp fiber, thereby ensuring a pre-wetting effect in the industrial hemp fiber and generating gaps in the industrial hemp fiber. Step 2: soaking the pretreated industrial hemp fiber in a bio-enzyme complex solution for 10-20 minutes to obtain preliminary degummed industrial hemp fiber, wherein the bio-enzyme complex solution is a bio-enzyme soaked in a sodium citrate buffer solution, and the mass ratio of the bio-enzyme is 3-5 parts of alkaline pectinase and 5-8 parts of xylanase, and the concentration of the bio-enzyme in the sodium citrate buffer solution is 50-100 g / L, and the sodium citrate buffer solution is a citric acid-sodium citrate buffer solution, and the pH is 5.5-6; the mass ratio of the industrial hemp fiber to the bio-enzyme mixture is 1:10-15, and the soaking temperature is 50-60° C.; this step utilizes the pH of the bio-enzyme complex solution and the mixing of the bio-enzyme to form a good preliminary degumming effect during the constant temperature soaking process, thereby forming a good biological degumming; Step 3, placing the preliminary degummed industrial hemp fiber in an alkaline pectinase buffer and performing a preliminary electrolysis for 5-10 minutes, then adding a mixed electrolyte for secondary electrolysis for 30-60 minutes, taking out the industrial hemp after standing for 1-3 hours, washing and drying to obtain industrial hemp fiber, wherein the mass ratio of the preliminary degummed industrial hemp fiber to the alkaline pectinase buffer is 1:10-13, the alkaline pectinase buffer solution adopts sodium bicarbonate buffer, and the pH is 10, the current of the preliminary electrolysis is 10-20mA, the mixed electrolyte adopts a mixed solution of sodium chloride and sodium thiosulfate, and the concentration of sodium thiosulfate is 20-40g / L, the concentration of sodium chloride is 5-10g / L, the volume ratio of the mixed electrolyte to the alkaline pectinase buffer is 1:1-2, and the current of the secondary electrolysis is 1-3 A, the temperature is 50-60°C; the standing temperature is 60-80°C, distilled water is used for washing, and the drying temperature is 110-120°C; this step utilizes alkaline pectinase and sodium carbonate to form an alkaline electrolysis system, utilizes the very small amount of electrons initially generated to promote the enzymatic action of the alkaline pectinase, and forms a continuous single enzymatic hydrolysis at an appropriate temperature, thereby opening the internal structure of the gel through the single enzymatic hydrolysis and improving the permeability of the solution; when the mixed electrolyte is added, the electrolytic intensity increases rapidly, forming a synergistic effect of the biological enzyme and the electrolytic system, the electrolytic system not only kills the alkaline pectinase, but also forms a stable and pure electrolytic system, at this time the sodium thiosulfate directly acts on the lignin under the electrolytic environment, thereby increasing the degumming amount and degumming efficiency, and the entire electrolytic system is a weak alkaline system, which causes minimal damage to the industrial hemp fiber.

[0006] It can be seen from the above description that the present invention has the following advantages: 1. The present invention solves the problem of general degumming effect of industrial hemp fiber, utilizes the preliminary degumming of composite biological enzymes and the combination of biological enzymes with an electrolytic system to form an electrochemical-biological enzyme composite degumming system, which greatly improves the degumming effect.

[0007] 2. The present invention utilizes alkaline pectinase and sodium carbonate buffer to form a synergistic degumming system of biological enzymes and electrochemistry, which not only completely opens the gum layer, but also utilizes electrochemical electrons to stimulate the enzymatic activity of pectinase, thereby improving the enzymatic hydrolysis efficiency of pectinase and providing a larger contact surface for subsequent electrolytic degumming.

[0008] 3. The present invention utilizes a high-efficiency electrolysis system formed by sodium thiosulfate and sodium chloride, which can quickly inactivate alkaline pectinase and utilize the enzymatic hydrolysis channel formed by pectinase to improve the penetration and contact of the electrolyte, thereby improving the degumming efficiency. DETAILED DESCRIPTION

[0009] The present invention is described in detail with reference to the embodiments, but no limitation is imposed on the claims of the present invention. Example 1

[0010] A method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber comprises the following steps: Step 1, placing industrial hemp fiber in water, adding a penetrant and ultrasonically treating it for 10 minutes, filtering and drying it to obtain pretreated industrial hemp fiber, wherein the mass ratio of the industrial hemp fiber to water is 1:7, the penetrant is JFC, and the concentration of the penetrant in water is 0.08%, the ultrasonic treatment temperature is 30°C, the ultrasonic frequency is 80kHz, and the drying concentration is 20°C; Step 2: soaking the pretreated industrial hemp fiber in a biological enzyme complex solution for 10 minutes to obtain a preliminary degummed industrial hemp fiber, wherein the biological enzyme complex solution is a biological enzyme soaked in a sodium citrate buffer solution, and the mass ratio of the biological enzyme is 5 parts of alkaline pectinase and 8 parts of xylanase, and the concentration of the biological enzyme in the sodium citrate buffer solution is 100 g / L, and the sodium citrate buffer solution is a citric acid-sodium citrate buffer solution with a pH of 5.5; the mass ratio of the industrial hemp fiber to the biological enzyme mixture is 1:15, and the soaking temperature is 50° C.; Step 3, placing the preliminary degummed industrial hemp fiber in an alkaline pectinase buffer and performing preliminary electrolysis for 5 minutes, then adding a mixed electrolyte for secondary electrolysis for 30 minutes, taking out the industrial hemp after standing for 1 hour, washing and drying to obtain industrial hemp fiber, the mass ratio of the preliminary degummed industrial hemp fiber to the alkaline pectinase buffer is 1:13, the alkaline pectinase buffer solution adopts sodium bicarbonate buffer, and the pH is 10, the current of the preliminary electrolysis is 10mA, the mixed electrolyte adopts a mixture of sodium chloride and sodium thiosulfate, and the concentration of sodium thiosulfate is 40g / L, the concentration of sodium chloride is 10g / L, the volume ratio of the mixed electrolyte to the alkaline pectinase buffer is 1:2, the current of the secondary electrolysis is 1A, and the temperature is 50°C; the standing temperature is 60°C, the washing adopts distilled water, and the drying temperature is 110°C. Example 2

[0011] A method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber comprises the following steps: Step 1, placing industrial hemp fiber in water, adding a penetrant and ultrasonically treating for 20 minutes, filtering and drying to obtain pretreated industrial hemp fiber, wherein the mass ratio of the industrial hemp fiber to water is 1:5, the penetrant is JFC, and the concentration of the penetrant in water is 0.05%, the ultrasonic treatment temperature is 40°C, the ultrasonic frequency is 100kHz, and the drying concentration is 30°C; Step 2: soaking the pretreated industrial hemp fiber in a biological enzyme complex solution for 20 minutes to obtain a preliminary degummed industrial hemp fiber, wherein the biological enzyme complex solution is a biological enzyme soaked in a sodium citrate buffer solution, and the mass ratio of the biological enzyme is 3 parts of alkaline pectinase and 5 parts of xylanase, and the concentration of the biological enzyme in the sodium citrate buffer solution is 50 g / L, and the sodium citrate buffer solution is a citric acid-sodium citrate buffer solution with a pH of 6; the mass ratio of the industrial hemp fiber to the biological enzyme mixture is 1:10, and the soaking temperature is 60°C; Step 3, placing the preliminary degummed industrial hemp fiber in an alkaline pectinase buffer and performing a preliminary electrolysis for 10 minutes, then adding a mixed electrolyte for secondary electrolysis for 360 minutes, taking out the industrial hemp after standing for 3 hours, washing and drying to obtain industrial hemp fiber, wherein the mass ratio of the preliminary degummed industrial hemp fiber to the alkaline pectinase buffer is 1:10, the alkaline pectinase buffer solution adopts sodium bicarbonate buffer, and the pH is 10, the current of the preliminary electrolysis is 20mA, the mixed electrolyte adopts a mixture of sodium chloride and sodium thiosulfate, and the concentration of sodium thiosulfate is 20g / L, the concentration of sodium chloride is 5g / L, the volume ratio of the mixed electrolyte to the alkaline pectinase buffer is 1:1, the current of the secondary electrolysis is 3A, and the temperature is 60°C; the standing temperature is 80°C, the washing adopts distilled water, and the drying temperature is 120°C. Example 3

[0012] A method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber comprises the following steps: Step 1, placing industrial hemp fiber in water, adding a penetrant and ultrasonically treating it for 15 minutes, filtering and drying it to obtain pretreated industrial hemp fiber, wherein the mass ratio of the industrial hemp fiber to water is 1:6, the penetrant is JFC, and the concentration of the penetrant in water is 0.06%, the ultrasonic treatment temperature is 35°C, the ultrasonic frequency is 90kHz, and the drying concentration is 25°C; Step 2: soaking the pretreated industrial hemp fiber in a biological enzyme complex solution for 15 minutes to obtain a preliminary degummed industrial hemp fiber, wherein the biological enzyme complex solution is a biological enzyme soaked in a sodium citrate buffer solution, and the mass ratio of the biological enzyme is 4 parts of alkaline pectinase and 7 parts of xylanase, and the concentration of the biological enzyme in the sodium citrate buffer solution is 80 g / L, and the sodium citrate buffer solution is a citric acid-sodium citrate buffer solution with a pH of 5.5; the mass ratio of the industrial hemp fiber to the biological enzyme mixture is 1:13, and the soaking temperature is 55° C.; Step 3, placing the preliminary degummed industrial hemp fiber in an alkaline pectinase buffer and performing preliminary electrolysis for 8 minutes, then adding a mixed electrolyte for secondary electrolysis for 50 minutes, taking out the industrial hemp after standing for 2 hours, washing and drying to obtain industrial hemp fiber, the mass ratio of the preliminary degummed industrial hemp fiber to the alkaline pectinase buffer is 1:12, the alkaline pectinase buffer solution adopts sodium bicarbonate buffer, and the pH is 10, the current of the preliminary electrolysis is 15mA, the mixed electrolyte adopts a mixture of sodium chloride and sodium thiosulfate, and the concentration of sodium thiosulfate is 30g / L, the concentration of sodium chloride is 8g / L, the volume ratio of the mixed electrolyte to the alkaline pectinase buffer is 1:1, the current of the secondary electrolysis is 2A, and the temperature is 55°C; the standing temperature is 70°C, the washing adopts distilled water, and the drying temperature is 115°C.

[0013] Comparative Example 1 A method for degumming industrial hemp fiber comprises the following steps: Step 1, placing industrial hemp fiber in water, adding a penetrant and ultrasonically treating it for 15 minutes, filtering and drying it to obtain pretreated industrial hemp fiber, wherein the mass ratio of the industrial hemp fiber to water is 1:6, the penetrant is JFC, and the concentration of the penetrant in water is 0.06%, the ultrasonic treatment temperature is 35°C, the ultrasonic frequency is 90kHz, and the drying concentration is 25°C; Step 2: soaking the pretreated industrial hemp fiber in a biological enzyme complex solution for 15 minutes to obtain a preliminary degummed industrial hemp fiber, wherein the biological enzyme complex solution is a biological enzyme soaked in a sodium citrate buffer solution, and the mass ratio of the biological enzyme is 4 parts of alkaline pectinase and 7 parts of xylanase, and the concentration of the biological enzyme in the sodium citrate buffer solution is 80 g / L, and the sodium citrate buffer solution is a citric acid-sodium citrate buffer solution with a pH of 5.5; the mass ratio of the industrial hemp fiber to the biological enzyme mixture is 1:13, and the soaking temperature is 55° C.; Step 3, adding the preliminary degummed industrial hemp fiber to the mixed electrolyte for electrolysis for 50 minutes, taking out the industrial hemp after standing for 2 hours, washing and drying to obtain industrial hemp fiber, wherein the mass ratio of the preliminary degummed industrial hemp fiber to the mixed electrolyte is 1:12, the mixed electrolyte adopts a mixture of sodium chloride and sodium thiosulfate, and the concentration of sodium thiosulfate is 30g / L, the concentration of sodium chloride is 8g / L, the current of the electrolysis is 2A, and the temperature is 55°C; the standing temperature is 70°C, the washing adopts distilled water, and the drying temperature is 115°C.

[0014] Comparative Example 2 A method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber comprises the following steps: Step 1, placing industrial hemp fiber in water, adding a penetrant and ultrasonically treating it for 15 minutes, filtering and drying it to obtain pretreated industrial hemp fiber, wherein the mass ratio of the industrial hemp fiber to water is 1:6, the penetrant is JFC, and the concentration of the penetrant in water is 0.06%, the ultrasonic treatment temperature is 35°C, the ultrasonic frequency is 90kHz, and the drying concentration is 25°C; Step 2, placing the industrial hemp fiber in an alkaline pectinase buffer, and performing a preliminary electrolysis for 8 minutes, then adding a mixed electrolyte for secondary electrolysis for 50 minutes, taking out the industrial hemp after standing for 2 hours, and washing and drying to obtain industrial hemp fiber, wherein the mass ratio of the industrial hemp fiber to the alkaline pectinase buffer is 1:12, the alkaline pectinase buffer solution adopts sodium bicarbonate buffer, and the pH is 10, the current of the preliminary electrolysis is 15mA, the mixed electrolyte adopts a mixture of sodium chloride and sodium thiosulfate, and the concentration of sodium thiosulfate is 30g / L, the concentration of sodium chloride is 8g / L, the volume ratio of the mixed electrolyte to the alkaline pectinase buffer is 1:1, the current of the secondary electrolysis is 2A, and the temperature is 55°C; the standing temperature is 70°C, the washing adopts distilled water, and the drying temperature is 115°C.

[0015] Comparative Example 3 A method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber comprises the following steps: Step 1: soaking the industrial hemp fiber in a biological enzyme complex solution for 15 minutes to obtain a preliminary degummed industrial hemp fiber, wherein the biological enzyme complex solution is a biological enzyme soaked in a sodium citrate buffer solution, and the mass ratio of the biological enzyme is 4 parts of alkaline pectinase and 7 parts of xylanase, and the concentration of the biological enzyme in the sodium citrate buffer solution is 80g / L, and the sodium citrate buffer solution is a citric acid-sodium citrate buffer solution with a pH of 5.5; the mass ratio of the industrial hemp fiber to the biological enzyme mixture is 1:13, and the soaking temperature is 55°C; Step 2, placing the preliminary degummed industrial hemp fiber in an alkaline pectinase buffer, and performing preliminary electrolysis for 8 minutes, then adding a mixed electrolyte for secondary electrolysis for 50 minutes, taking out the industrial hemp after standing for 2 hours, and washing and drying to obtain industrial hemp fiber, the mass ratio of the preliminary degummed industrial hemp fiber to the alkaline pectinase buffer is 1:12, the alkaline pectinase buffer solution adopts sodium bicarbonate buffer, and the pH is 10, the current of the preliminary electrolysis is 15mA, the mixed electrolyte adopts a mixture of sodium chloride and sodium thiosulfate, and the concentration of sodium thiosulfate is 30g / L, the concentration of sodium chloride is 8g / L, the volume ratio of the mixed electrolyte to the alkaline pectinase buffer is 1:1, the current of the secondary electrolysis is 2A, and the temperature is 55°C; the standing temperature is 70°C, the washing adopts distilled water, and the drying temperature is 115°C.

[0016] The industrial hemp fibers degummed in Examples 1-3 and Comparative Examples 1-3 were used as test samples for performance testing, and the results were as follows: Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Residual glue rate 8.83% 8.46% 8.71% 9.35% 9.24% 9.11% Breaking strength 28.45cN 23.67cN 27.16cN 29.98cN 29.58cN 29.39cN From the comparison of the above data, it can be seen that the degumming method provided by this technical solution can effectively reduce the glue content in industrial hemp fiber and greatly reduce the residual glue rate. At the same time, the change trend of the breaking strength also illustrates the synergistic effect of biological enzymes and electrochemistry, which not only improves the degumming efficiency, but also improves the degumming effect.

[0017] It is understood that the above specific description of the present invention is only used to illustrate the present invention and is not limited to the technical solutions described in the embodiments of the present invention. Those skilled in the art should understand that the present invention can still be modified or replaced with equivalents to achieve the same technical effects; as long as the use requirements are met, they are all within the scope of protection of the present invention.

Claims

1. A method for degumming industrial hemp fiber by electrochemical combined with bio-enzymatic degumming, characterized in that: The steps include: Step 1, placing industrial hemp fiber in water, adding a penetrant and ultrasonically treating for 10-20 minutes, filtering and drying to obtain pretreated industrial hemp fiber; Step 2: soaking the pretreated industrial hemp fiber in a bio-enzyme complex solution for 10-20 minutes to obtain preliminary degummed industrial hemp fiber; Step 3: Place the preliminarily degummed industrial hemp fiber in an alkaline pectinase buffer solution and perform a preliminarily electrolysis for 5-10 minutes, then add a mixed electrolyte for a secondary electrolysis for 30-60 minutes, let it stand for 1-3 hours, take out the industrial hemp, wash it, and dry it to obtain the industrial hemp fiber.

2. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 1, characterized in that: The mass ratio of industrial hemp fiber to water in step 1 is 1:5-7, the penetrant is JFC, and the concentration of the penetrant in water is 0.05-0.08%, the temperature of the ultrasonic treatment is 30-40°C, the ultrasonic frequency is 80-100kHz, and the concentration after drying is 20-30°C.

3. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 1, characterized in that: The biological enzyme complex solution in step 2 is biological enzymes soaked in sodium citrate buffer, and the mass ratio of the biological enzymes is 3-5 parts of alkaline pectinase and 5-8 parts of xylanase.

4. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 3, characterized in that: The concentration of the biological enzyme in sodium citrate buffer is 50-100 g / L.

5. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 3, characterized in that: The sodium citrate buffer is a citric acid-sodium citrate buffer with a pH of 5.5-6.

6. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 1, characterized in that: The mass ratio of the industrial hemp fiber to the biological enzyme mixture in step 2 is 1:10-15, and the soaking temperature is 50-60°C.

7. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 1, characterized in that: The mass ratio of the preliminary degummed industrial hemp fiber to the alkaline pectinase buffer in step 3 is 1:10-13, the alkaline pectinase buffer solution adopts sodium bicarbonate buffer and has a pH of 10, and the current of the preliminary electrolysis is 10-20 mA.

8. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 1, characterized in that: The mixed electrolyte in step 3 is a mixture of sodium chloride and sodium thiosulfate, with the concentration of sodium thiosulfate being 20-40 g / L, the concentration of sodium chloride being 5-10 g / L, the volume ratio of the mixed electrolyte to the alkaline pectinase buffer being 1:1-2, the current of the secondary electrolysis being 1-3 A, and the temperature being 50-60° C.

9. The method for electrochemical combined with bioenzymatic degumming of industrial hemp fiber according to claim 1, characterized in that: The standing temperature in step 3 is 60-80°C, distilled water is used for washing, and the drying temperature is 110-120°C.