CN116815334B - A kind of degumming method of apocynum venetum - Google Patents
A kind of degumming method of apocynum venetumInfo
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- CN116815334B CN116815334B CN202310891872.0A CN202310891872A CN116815334B CN 116815334 B CN116815334 B CN 116815334B CN 202310891872 A CN202310891872 A CN 202310891872A CN 116815334 B CN116815334 B CN 116815334B
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Abstract
本发明涉及一种罗布麻脱胶方法，属于罗布麻脱胶工艺技术领域。本发明提供的罗布麻脱胶方法包括预酸处理、预碱处理和温和氧化酶处理联合脱胶。本发明基于复合酶脱胶，配合温和氧化处理方法，可有效去除罗布麻纤维上的果胶、木质素、半纤维素等主要杂质，以及天然色素等其他杂质，并可增加罗布麻纤维白度，提高吸水和毛效，使织物表面光洁，手感柔软光滑；同时织物的亲水性，吸水扩散度均有明显增加，力学性能提升，可相应提高染色工序的上色率和匀染性。
The present invention relates to a method for degumming apocynum venetum, and belongs to the technical field of apocynum venetum degumming processes. The apocynum venetum degumming method provided by the present invention comprises a combined degumming process of pre-acid treatment, pre-alkali treatment and mild oxidase treatment. The present invention is based on composite enzyme degumming, combined with a mild oxidation treatment method, which can effectively remove major impurities such as pectin, lignin, hemicellulose, and other impurities on apocynum venetum fibers, as well as other impurities such as natural pigments, and can increase the whiteness of apocynum venetum fibers, improve water absorption and hair effect, make the surface of the fabric smooth, and feel soft and smooth; at the same time, the hydrophilicity and water absorption diffusion of the fabric are significantly increased, and the mechanical properties are improved, which can correspondingly improve the coloring rate and levelness of the dyeing process.
Description
Technical Field
The invention belongs to the technical field of a degumming process of apocynum venetum, and particularly relates to a degumming method of apocynum venetum.
Background
Apocynum venetum belongs to perennial wild herbal bast fiber plants of oleander, and is a characteristic plant resource in China. The bast fiber of the apocynum venetum is positioned in the bast tissue on the stems of the apocynum venetum plants, and the fiber is slender and is in a very loose fiber bundle. The apocynum venetum fiber has the characteristics of luster of silk, stiffness and smoothness of the apocynum venetum, spreadability of the velvet and softness of cotton, and the prepared textile has good air permeability and strong hygroscopicity, and simultaneously has the characteristics of softness, bacteriostasis, warmness in winter, coolness in summer and the like. Thus, apocynum venetum is referred to as "wild fiber king". However, compared with flax or ramie, the content of cellulose in the apocynum venetum is relatively low, and is only 45-55%. The gum layer of the apocynum venetum bast tissue is thicker, the fiber bundle structure is compact, the hydrophobicity is high, the accessibility is low, and meanwhile, the pectin content in the bast tissue is higher, so that the adhesion degree between wood and epidermal fibers is stronger. Therefore, the apocynum venetum must be degummed before being used for textile fibers, the degummed difficulty is high, and accordingly the degummed technology can have more direct influence on the fiber performance, and the apocynum venetum has become an important reason for restricting the apocynum venetum products to market.
Currently, the degumming methods of the apocynum venetum include chemical degumming, physical degumming, biological degumming and the like. The chemical degumming method is a mature degumming process, wherein the traditional chemical degumming process is mainly an alkali degumming process, and a large amount of chemical substances such as strong acid, strong alkali and the like are used, so that the environment is polluted, and the fiber is damaged. The degumming of apocynum fibers is more difficult than the rest of the several fibers, mainly because of the more pectic substances on the fibers. If the traditional secondary pre-alkali method is adopted, the dosage of chemicals is increased, and the environment is seriously damaged, which is contrary to the concept of green and sustainable development. Physical degumming mainly comprises methods of high temperature and high pressure, ultrasonic wave, microwave and the like. Although physical degumming is less environmentally friendly, its degumming efficiency is low. The biological degumming method is environment-friendly, but has the problems of low degumming efficiency, unstable quality of the finished dried hemp and the like. Biological degumming is divided into microbial degumming and biological enzyme degumming. In the aspect of microbial degumming, the microbial sources available for degumming the apocynum venetum are limited, and intensive research is needed. The biological enzyme degumming is to utilize biological enzyme to react with pectin in apocynum venetum so as to degrade pectin. Compared with chemical degumming, biological enzyme degumming has higher requirements on degumming conditions and limited degumming rate, and the residual gum content is higher than that of the chemical degumming.
The biological-chemical combined degumming method can achieve ideal degumming effect on the premise of reducing environmental pollution, and obtain the refined dry hemp with better quality. However, the report of Guan Luobu hemp biological-chemical combined degumming is relatively limited at present, and the existing degumming enzymes have single action, high price and high cost, and the added degumming enzymes have single performance, so that the problems of high requirements on degumming conditions, low degumming efficiency, low fiber whiteness, unstable quality of the prepared refined kendir and the like exist. Therefore, developing a mild degumming method capable of reducing the damage of the apocynum venetum, improving the whiteness of the apocynum venetum and reducing the viscosity of wastewater is a technical problem which needs to be solved urgently at present.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a method for degumming apocynum venetum, which has high degumming efficiency, good whiteness and low damage.
The invention is realized by the following technical scheme:
The invention provides a method for degumming apocynum venetum, which comprises the following steps:
(1) Adding herba Apocyni Veneti into acid solution, heating at 55-65deg.C for 55-75 min, and cleaning, wherein the bath ratio of herba Apocyni Veneti to the acid solution is 1 (20-50);
(2) Adding alkali liquor into the apocynum venetum cleaned in the step (1), and cleaning after heating for 95-105 min at 65-70 ℃, wherein the bath ratio of the apocynum venetum to the alkali liquor is 1 (20-50);
(3) Adding a mixed solution containing complex enzyme and oxidant into the apocynum venetum cleaned in the step (2), heating at 70-80 ℃ for 45-85 min, cleaning, and drying to obtain apocynum venetum refined dry fiber, wherein the bath ratio of the apocynum venetum to the mixed solution is 1 (20-50).
The degumming method of the invention adopts a chemical method of combination of complex enzyme and mild oxidation for degumming. Compared with the existing alkali-oxygen process, the method can reduce the strong damage to the apocynum venetum and reduce the sewage viscosity and the sewage treatment burden. The invention makes the outer layer of the fiber not be directly connected with the fiber or the colloid component with loose structure be primarily degraded through the pre-acid treatment and the pre-alkali treatment, and the non-fiber colloid is treated by one step by using the complex enzyme and the oxidant under the condition of not damaging the fiber structure so as to achieve the aim of complete degumming. The degumming method has good degumming effect on apocynum venetum, can obviously reduce the glue content of the fiber, improve the whiteness of the fiber, reduce the strong damage of the fiber and the like, and is environment-friendly in process.
In the step (1), the acid in the acid liquor is sulfuric acid, the mass of the sulfuric acid is 1.25% -2% of that of the apocynum, the heating temperature is 60-65 ℃ and the heating time is 55-60 min. The pretreatment of the sulfuric acid under the conditions of concentration and heating can effectively improve the whiteness of degummed apocynum and ensure that the apocynum has better mechanical strength.
As a preferred embodiment of the method for degumming apocynum venetum according to the present invention, in the step (1), the mass of the sulfuric acid is 1.75% -2% of the mass of apocynum venetum. When the concentration of sulfuric acid is 1.75% -2% of the mass of the apocynum venetum, the apocynum venetum after the pre-acid treatment has good whiteness and mechanical properties.
As a preferred embodiment of the method for degumming apocynum venetum according to the invention, in the step (2), the alkali liquor comprises, by mass, 4.5% -6.5% of sodium hydroxide, 4% -5% of sodium silicate, 2.5% -4.5% of sodium sulfite and 3% -3.5% of penetrating agent. According to the method, sodium hydroxide, sodium silicate, sodium sulfite and penetrating agent are compounded to serve as alkaline agents to pre-alkaline the apocynum venetum, so that colloid on the surface of the apocynum venetum is primarily degraded, and degumming is carried out by matching with pre-acid treatment and enzyme mild oxidation treatment to improve whiteness of the apocynum venetum refined dry apocynum venetum.
Preferably, the penetrant is an anionic alkali-resistant penetrant. The anionic alkali-resistant penetrating agent can better promote the alkali liquor to play a role, so that the pre-alkali treatment effect is better.
As a preferred embodiment of the method for degumming apocynum venetum according to the invention, in the step (2), the heating time is 100-105 min.
As a preferred embodiment of the degumming method for apocynum venetum according to the present invention, in the step (3), the complex enzyme includes pectase, hemicellulase, ligninase, laccase and xylanase. The complex enzyme obtained by adopting the compatibility of the various enzymes has better degumming effect.
As a preferred implementation mode of the apocynum degumming method, the compound enzyme comprises, by mass, 60-64 parts of pectase, 17-19 parts of hemicellulase, 10-13 parts of lignin enzyme, 3-5 parts of laccase and 4-5 parts of xylanase.
Preferably, the activity of pectase, hemicellulase, laccase and xylanase is more than or equal to 800U/mL, and the activity of lignin enzyme is more than or equal to 300U/mL.
The invention combines complex enzyme containing a plurality of biological enzyme species with the oxidant, and performs enzyme degumming under the oxidation condition, so that the gum on the surface of apocynum can be effectively removed, the degumming rate is high, and the gum residue is less.
Preferably, the compound enzyme comprises, by mass, 60 parts of pectase, 17 parts of hemicellulase, 13 parts of ligninase, 5 parts of laccase and 5 parts of xylanase.
Compared with other enzymes, the compound enzyme has better degumming effect, can obviously improve the whiteness of degummed apocynum, and has better fiber strength after degumping.
As a preferred embodiment of the method for degumming apocynum venetum according to the invention, in the step (3), the concentration of the complex enzyme in the mixed solution is 15g/L-25g/L. The enzyme concentration can influence the degumming efficiency and the degumming effect, and researches show that the compound enzyme concentration can effectively remove colloid on the surface of the apocynum venetum, improve the whiteness of the apocynum venetum refined dry hemp and reduce the damage of the apocynum venetum fibers.
In the step (3), the oxidant is hydrogen peroxide, and the concentration of hydrogen peroxide in the mixed solution is 4g/L-6g/L. The invention adopts hydrogen peroxide to provide a mild oxidation environment, combines with compound enzyme to degumm, has low degummed condition requirement and high degummed efficiency, and prepares refined dried apocynum with stable quality.
In the step (3), the washing is performed by hot water washing and then cold water washing. The invention adopts cold and hot water to alternately wash degummed apocynum, can sufficiently wash the surface colloid residue, and better maintains the strength of apocynum.
Preferably, the temperature of the hot water is 55-65 ℃ and the temperature of the cold water is 0-15 ℃.
The invention has the following beneficial effects:
(1) The degumming method adopts the combination of chemical degumming and biological degumming, combines the compound enzyme with oxidation environment for degumming, has less damage to the fiber, can replace the input of various auxiliary agents in the traditional apocynum degumming process, reduces the feeding variety and the feeding amount, simplifies the degumming process flow and operation, and effectively improves the degumming and impurity removing efficiency of the apocynum. Compared with the existing biological enzyme method, the gum residue rate of the apocynum venetum is about 5%, and the weight loss rate reaches 40%. Meanwhile, the viscosity of sewage is low, and the washing burden is light. (2) The degumming method is based on complex enzyme, and is matched with a mild oxidation and chemical treatment method, so that the tencel impurities, other various impurities, natural pigments and the like on the apocynum venetum fabrics can be effectively removed, whiteness can be increased, hair effect is improved, the surfaces of the fabrics are smooth and clean, the hand feeling is soft and smooth, meanwhile, the hydrophilia and water absorption diffusion of the fabrics are obviously increased, and the dyeing rate and the leveling property of dyeing procedures can be correspondingly improved. The degumming process flow and the operation are simple, and the damage to the apocynum venetum is small. The single yarn strength of the apocynum venetum reaches 8CN, the average breaking strength is 4.5cN/dtex, and the spinning requirement is met. In addition, the degumming method is a novel degumming process combining biological enzyme and mild oxidation, expands the adaptability of the biological-mild oxidation degumming process, and does not influence the degumming performance due to the differences in the production environment, the hemp skin state, the hemp peeling mode and the like of the apocynum venetum. The degumming method of the invention can be applied to the products after pilot plant test, and has stable degumming performance.
Drawings
FIG. 1 shows the effect of oxidation with hydrogen peroxide on the weight loss rate of apocynum;
FIG. 2 shows the effect of oxidation with hydrogen peroxide on the whiteness of apocynum;
FIG. 3 shows the effect of oxidation with hydrogen peroxide on the strength of a single fiber of Apocynum venetum;
FIG. 4 is a graph showing the effect of different enzyme treatment temperatures on the weight loss rate of apocynum;
FIG. 5 shows the effect of different enzyme treatment temperatures on the whiteness of apocynum;
FIG. 6 shows the effect of different enzyme treatment temperatures on the strength of apocynum venetum filaments;
FIG. 7 shows the results of testing the whiteness strength, elongation and breaking strength of apocynum venetum under different pre-acid treatment conditions;
FIG. 8 shows the results of testing the whiteness strength, elongation and breaking strength of apocynum under different pre-alkali treatment conditions;
FIG. 9 shows the results of testing the whiteness strength, elongation and breaking strength of apocynum venetum under different degelling agent treatment conditions;
Fig. 10 is a scanning electron microscope image of example 3 before and after degumming of apocynum venetum, wherein (a) is the apocynum venetum fiber before degumming and (b) is the apocynum venetum fiber after degumming.
Fig. 11 is an infrared spectrum of example 3 before and after degumming of apocynum venetum.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples. It will be appreciated by persons skilled in the art that the specific embodiments described herein are for purposes of illustration only and are not intended to be limiting.
The test methods used in the examples are conventional methods unless otherwise specified, and the materials, reagents, etc. used, unless otherwise specified, are commercially available.
Example 1
1.1 Selection of enzymes in Apocynum degumming Agents
The degummed effect of different enzyme types is analyzed and discussed by carrying out the combined degummed research of the compound biological enzyme and the hydrogen peroxide mild oxidation in the step (3) on the apocynum bast and taking the weight loss rate, the whiteness and the single fiber strength as evaluation indexes. Four different biological enzymes are respectively adopted to explore the degumming effect of degummed dried hemp, the oxidation conditions are 10g/L of enzyme, 2g/L of hydrogen peroxide, the bath ratio is 1:50, the temperature is 85 ℃ and the time is 30min, and the results are shown in Table 1. The enzyme types JS-369, HS-535, ZW-616 and YA-460 are all compound enzymes, and the compound enzymes JS-369 comprise, by mass, 60 parts of pectase, 17 parts of hemicellulase, 13 parts of lignin enzyme, 5 parts of laccase and 5 parts of xylanase. The composite enzyme HS-535 comprises 65 parts of pectase, 20 parts of hemicellulase, 8 parts of lignin enzyme, 2 parts of laccase and 5 parts of xylanase by mass. The compound enzyme ZW-616 comprises, by mass, 70-80 parts of pectase, 10-15 parts of hemicellulase and 10-15 parts of lignin enzyme. The compound enzyme YA-460 comprises, by mass, 70 parts of pectase, 25 parts of hemicellulase and 5 parts of lignin enzyme.
In this example, the whiteness test described below is referred to GB5881-86 "method for testing whiteness of Ramie fibers", the strength and breaking strength test is referred to GB5881-86 "method for testing breaking strength of Ramie fibers", and the length test is referred to GB5881-86 "method for testing length of Ramie fibers".
TABLE 1 comparison of Performance of degummed Sesamum with different Complex enzymes
As shown in the weight loss rate test results in Table 1, the weight loss rate of the apocynum venetum fibers obtained by degumming with the biological enzyme HS-535 is the largest, the weight loss rate of the apocynum venetum fibers obtained by degumming with the biological enzyme YA-460 is the smallest, the whiteness of the apocynum venetum bast is the best under the treatment of the composite biological enzyme JS-369 according to the whiteness test results, the whiteness of the refined apocynum venetum obtained by degumming with the biological enzyme YA-460 is the worst, the single fiber strength test results indicate that the single fiber strength of the apocynum venetum obtained by degumming with the biological enzyme HS-535 is the largest, and the next biological enzyme ZW-616 and the refined apocynum venetum obtained by degumming with the biological enzyme JS-369 is the smallest.
The comprehensive comparison can obtain that under the oxidation condition (10 g/L enzyme, 2g/L hydrogen peroxide, bath ratio of 1:50,85 ℃ and 30 min), the biological enzyme JS-369 has the highest whiteness, the larger weight loss rate and the best degumming effect, and the composite biological enzyme HS-535 has the lowest weight loss rate and whiteness of the degummed ramie obtained by using the composite biological enzyme YA-460 and the worst degumming effect.
1.2 Selection of the Condition in step (3) of the degumming Process
The influence of oxidation conditions and temperature on degumming effect is explored by the influence of the presence or absence of hydrogen peroxide and the difference of enzyme treatment temperature on the weight loss rate, whiteness and strength. Fig. 1 is an effect of whether hydrogen peroxide is added for oxidation on the weight loss rate of apocynum venetum, fig. 2 is an effect of whether hydrogen peroxide is added for oxidation on the whiteness of apocynum venetum, and fig. 3 is an effect of whether hydrogen peroxide is added for oxidation on the strength of apocynum venetum single fibers, and it can be seen from comprehensive fig. 1-3 that the introduction of oxidation conditions can improve the weight loss rate of apocynum venetum and can remarkably improve the whiteness of apocynum venetum, wherein the whiteness of refined apocynum venetum obtained by degumming with biological enzymes JS-369 and biological enzymes HS-535 is increased by more than twice when the oxidation conditions are not used. Fig. 4 shows the effect of different enzyme treatment temperatures on the weight loss rate of the apocynum venetum, fig. 5 shows the effect of different enzyme treatment temperatures on the whiteness of the apocynum venetum, and fig. 6 shows the effect of different enzyme treatment temperatures on the strength of the apocynum venetum single fibers, wherein as can be seen from fig. 4-6, the higher the enzyme treatment temperature is, the higher the refined whiteness and the weight loss rate of the apocynum venetum are, but the strength of the degummed apocynum venetum single fibers is damaged to some extent.
Through the exploration of the embodiment, the combination of enzyme-oxidation by combining biological enzyme and hydrogen peroxide is selected to degum the apocynum venetum.
Example 2
2.1 Investigation of the conditions for the Pre-acid treatment in step (1)
The weighed apocynum venetum is placed into a beaker, 98% sulfuric acid solution is added, the weighed apocynum venetum is placed into a water bath for heating treatment, the sulfuric acid concentration (1.25%, 1.75% and 2.25%) in the pre-acid condition, the temperature of the water bath (55 ℃, 65 ℃ and 75 ℃) and the heating time (55 min, 65min and 75 min) are subjected to factor analysis, and 9 groups of orthogonal experiments are carried out on the pre-acid treatment, wherein the orthogonal experiment scheme is shown in table 2.
TABLE 2 orthogonal protocol for Pre-acid treatment
| Numbering device | Sulfuric acid concentration (weight to fabric) | Temperature/°c | Time/min |
| A1 | 1.25% | 55 | 55 |
| A2 | 1.75% | 65 | 55 |
| A3 | 2.25% | 75 | 55 |
| A4 | 1.25% | 75 | 65 |
| A5 | 1.75% | 55 | 65 |
| A6 | 2.25% | 65 | 65 |
| A7 | 1.25% | 65 | 75 |
| A8 | 1.75% | 75 | 75 |
| A9 | 2.25% | 55 | 75 |
The effect of sulfuric acid concentration, pre-acid treatment temperature and time in step (1) on the performance of apocynum venetum was determined by 9 sets of orthogonal experiments. The whiteness, strength, elongation and strength of the apocynum venetum treated in the step (1) are tested, the test results are shown in fig. 7, the left graph of fig. 7 shows the whiteness test results of the apocynum venetum under different pre-acid treatment conditions, and as can be seen from the left graph of fig. 7, the lowest whiteness of the apocynum venetum fiber after pre-acid treatment is 68.38%, and the highest whiteness is 76.36%. And 5 groups of apocynum venetum with the best whiteness are selected from the whiteness test results, and the strength, elongation and breaking strength of the apocynum venetum are tested. The test results are shown in the right graph of FIG. 7, wherein the lowest average strength after the pre-acid treatment is 8.6cN, the highest average strength is 13cN, the minimum elongation is 0.23mm, the maximum elongation is 0.45mm, the minimum breaking strength is 4.29cN/dtex, and the maximum breaking strength is 6.53cN/dtex. Wherein, the mechanical strength and whiteness of the apocynum venetum after degumming of the groups A1 and A2 are better, the degumming effect of the A2 in the apocynum venetum is best, and the pre-acid condition is that the fabric weight is 1.75 percent of sulfuric acid solution, the temperature is 65 ℃ and the time is 55min.
2.2 Step (2) investigation of Pre-alkaline treatment conditions
Washing the pre-acid treated apocynum venetum with clear water, sequentially adding sodium hydroxide, sodium silicate, sodium sulfite and an anionic alkali-resistant penetrating agent, heating in a water bath kettle, and performing alkali boiling with alkali boiling as a single variable and pre-acid and enzyme treatment as quantification. Factor analysis was performed on sodium hydroxide concentration (4.5%, 5.5%, 6.5%), sodium silicate concentration (3%, 4%, 5%), sodium sulfite concentration (2.5%, 3.5%, 4.5%), anion type alkali-resistant penetrant concentration (1.5%, 2.5%, 3.5%), heating temperature (50 ℃,60 ℃, 70 ℃) and heating time (85 min, 95min, 105 min) in the alkali boiling condition to obtain 18 sets of orthogonal experiments, and the orthogonal experimental schemes are shown in table 3.
TABLE 3 orthogonal protocol for Pre-alkali treatment
And (3) determining the influence of the content of each component in the alkali liquor in the step (2), the pre-alkali treatment temperature and the pre-alkali treatment time on the performance of the apocynum venetum through 18 groups of orthogonal experiments. The whiteness, strength, elongation and strength of each group of treated apocynum venetum are tested, the test results are shown in fig. 8, the left graph of fig. 8 shows the whiteness test results of apocynum venetum under different pre-alkali treatment conditions, and as can be seen from the left graph of fig. 8, the lowest whiteness of the apocynum venetum fibers after pre-alkali treatment is 66.2%, and the highest whiteness is 75.9%. And selecting 10 groups of apocynum venetum with the best whiteness from the whiteness test results, and testing the strength, elongation and breaking strength of the apocynum venetum. The test results are shown in the right graph of FIG. 8, wherein the lowest average strength after the pre-alkali treatment is 6.1cN, the highest average strength is 10.46cN, the minimum elongation is 0.18mm, the maximum elongation is 0.44mm, the minimum breaking strength is 3.04cN/dtex, and the maximum breaking strength is 5.23cN/dtex. Wherein, the mechanical strength and whiteness of the apocynum venetum after degumming of the groups B3 and B18 are better, and the degumming effect of the B3 in the apocynum venetum is best, and the pre-alkali condition is that the weight of the fabric is 4.5 percent of sodium hydroxide, 4 percent of sodium silicate, 2.5 percent of sodium sulfite and 3.5 percent of penetrating agent, the temperature is 70 ℃ and the time is 105 minutes.
2.3 Step (3) enzyme combination Mild Oxidation treatment Condition exploration
Washing herba Apocyni Veneti subjected to pre-acid treatment and pre-alkali treatment with warm water, placing into a beaker, adding complex enzyme JS-369, controlling pH value at 9-11, adding hydrogen peroxide, measuring pH value of solution, controlling pH value at 9-11, heating to perform enzyme treatment, washing with warm water after finishing, washing with cold water, and oven drying to obtain refined herba Apocyni Veneti. Within this pH range, the enzyme combination mild oxidation treatment is optimal. Taking pre-acid treatment and alkali boiling as quantification, and taking enzyme treatment as single variables, performing factor analysis on the concentration (15 g/L, 20g/L and 25 g/L) of the compound enzyme JS-369, the concentration (4 g/L, 6g/L and 8 g/L) of hydrogen peroxide, the heating temperature (70 ℃, 85 ℃ and 100 ℃) and the heating time (45 min, 65min and 85 min) to obtain 9 groups of orthogonal experiments, wherein the orthogonal experimental scheme is shown in Table 4.
TABLE 4 orthogonal protocol for enzyme treatment
| Numbering device | Enzyme concentration (g/L) | Hydrogen peroxide concentration (g/L) | Temperature/°c | Time/min |
| C1 | 15 | 4 | 70 | 45 |
| C2 | 15 | 6 | 100 | 65 |
| C3 | 15 | 8 | 85 | 85 |
| C4 | 20 | 4 | 100 | 85 |
| C5 | 20 | 6 | 85 | 45 |
| C6 | 20 | 8 | 70 | 65 |
| C7 | 25 | 4 | 85 | 65 |
| C8 | 25 | 6 | 70 | 85 |
| C9 | 25 | 8 | 100 | 45 |
And (3) determining the influence of the compound enzyme dosage, the hydrogen peroxide dosage, the temperature and the time in the step (3) on the performance of the apocynum venetum through 9 groups of orthogonal experiments. The whiteness, strength, elongation and strength of the treated apocynum venetum are tested, the test results are shown in fig. 9, the left graph of fig. 9 shows the whiteness test results of apocynum venetum under different enzyme combination mild oxidation treatment conditions, and as can be seen from the left graph of fig. 9, the lowest whiteness of the apocynum venetum fiber after the enzyme combination mild oxidation treatment is 68.34%, and the highest whiteness is 75.06%. And 5 groups of apocynum venetum with the best whiteness are selected from the whiteness test results, and the strength, elongation and breaking strength of the apocynum venetum are tested. The results of the test are shown in the right graph of FIG. 9, in which the enzyme combination is mild and the average strength after oxidation treatment is 7.33cN, the average strength is 9.69cN, the elongation is 0.31mm, the elongation is 0.45mm, the breaking strength is 3.16cN/dtex, and the breaking strength is 4.84cN/dtex. Wherein, the mechanical strength and whiteness of the apocynum venetum after degumming in the groups C1 and C8 are better, the degumming effect of the C8 in the apocynum venetum is best, and the treatment condition of the degumming agent is 25g/L of the degumming agent, 6g/L of hydrogen peroxide at the temperature of 70 ℃ for 85min.
The pre-acid condition of the apocynum degumming step (1) is obtained through further researches, wherein the pre-acid condition of the apocynum degumming step (1) is that the temperature of a sulfuric acid solution with the weight of 1.25-2% is 55-65 ℃ and the time is 55-75 min, the pre-alkali condition of the apocynum degumming step (2) is that the temperature of a sodium hydroxide with the weight of 4.5-6.5% is 4-5% and sodium silicate with the weight of 2.5-4.5% is 3-3.5% and the temperature of 65-70 ℃ and the time is 95-105 min, and the enzyme combined mild oxidation treatment condition of the step (3) is that the temperature of a hydrogen peroxide with the weight of 15-25 g/L is JS-369 and the time is 4g/L-6g/L, and the temperature of the hydrogen peroxide is 70-80 ℃ and the time is 45-85 min.
Example 3
The embodiment provides a method for degumming apocynum venetum, which comprises the following steps:
(1) Adding herba Apocyni Veneti into sulfuric acid solution at bath ratio of 1:50, heating at 60deg.C for 60min, and cleaning with sulfuric acid of 2% owf;
(2) Adding the cleaned apocynum venetum in the step (1) into an alkali liquor with the bath ratio of 1:50, heating at 70 ℃ for 105min, and cleaning, wherein the alkali liquor comprises 4.5% of sodium hydroxide, 4% of sodium silicate, 2.5% of sodium sulfite and 3.5% of penetrating agent;
(3) Adding mixed solution of biological enzyme JS-369 and hydrogen peroxide into the apocynum venetum cleaned in the step (2), wherein the bath ratio is 1:50, the dosage of the apocynum venetum degumming agent is 25g/L, the mass fraction of the hydrogen peroxide is 30%, the dosage of the hydrogen peroxide is 6g/L, heating for 85min at 70 ℃, cleaning with hot water at 55 ℃ and then with cold water at 10 ℃, and drying at 60 ℃ to obtain the apocynum venetum refined dry fibrilum.
The average whiteness of the apocynum venetum treated by the degumming method in the embodiment reaches 77.34%, the average strength reaches 9.7cN, the average elongation reaches 0.57mm, and the average breaking strength reaches 4.91cN/dtex, which shows that the apocynum venetum treated by the degumming method has higher whiteness and mechanical property.
The surface morphology features of the apocynum venetum before and after degumming in the embodiment are observed by using a scanning electron microscope, the scanning electron microscope is shown in fig. 10, the diagram (a) is the apocynum venetum fiber before degumming, the surface is rough and uneven, the impurity is more, and a large number of colloid particles can be clearly seen to be wrapped on the surface of the apocynum venetum fiber. The degummed apocynum fiber has smooth and flat surface as shown in fig. 10 (b), which shows that the impurities on the surface of the apocynum fiber are basically removed, and the degummed agent and the degummed method can better remove the colloid on the surface of the apocynum fiber.
And (3) carrying out structural characterization on the apocynum fibers before and after degumming by using an infrared spectrum analyzer, wherein the scanning range is 4000-500 cm –1, and the resolution is 4cm –1. Fig. 11 is an infrared spectrum of a kendir fiber, wherein the treated kendir fiber is degummed in the present example. As can be seen from FIG. 11, the peak appearing at 3369cm –1 (the stretching vibration of-OH) is a characteristic absorption peak of cellulose and hemicellulose components, the peak appearing at 2898cm –1 (the stretching vibration of C-H) is a characteristic peak of cellulose and macromolecular gum, the absorption peaks at 1728cm –1 and 1643cm –1 are characteristic absorption peaks of lignin carbonyl and hemicellulose acetyl groups, the absorption peak at 1427cm –1、1369cm–1、1318cm–1、1157cm–1 is a characteristic absorption peak of galacturonic acid in pectin in a fingerprint region, and the peak appearing at 665cm –1 (the C-OH out-of-plane bending) is a main characteristic peak of cellulose. After the apocynum fiber is degummed, the absorption vibration peaks are weakened to a certain extent, which means that pectin, non-cellulose and other colloid in the apocynum fiber are basically removed after the degummed.
Example 4
A degumming method of apocynum venetum comprises the following steps:
(1) Adding herba Apocyni Veneti into sulfuric acid solution at bath ratio of 1:50, heating at 65deg.C for 55min, cleaning, and adding sulfuric acid with an amount of 1.75% owf;
(2) Adding the cleaned apocynum venetum in the step (1) into an alkali liquor with the bath ratio of 1:50, heating at 65 ℃ for 95min, and cleaning, wherein the alkali liquor comprises 6.5% of sodium hydroxide, 5% of sodium silicate, 4.5% of sodium sulfite and 3.5% of penetrating agent;
(3) Adding mixed solution of biological enzyme JS-369 and hydrogen peroxide into the apocynum venetum cleaned in the step (2), wherein the bath ratio is 1:50, the dosage of the apocynum venetum degumming agent is 15g/L, the mass fraction of the hydrogen peroxide is 30%, the dosage of the hydrogen peroxide is 4g/L, heating for 45min at 80 ℃, cleaning with 65 ℃ hot water and then with 15 ℃ cold water, and drying at 60 ℃ to obtain the apocynum venetum refined dry fibrilum.
The average whiteness of the apocynum venetum treated by the degumming method in the embodiment reaches 76.9%, the average strength reaches 9.2cN, the average elongation reaches 0.56mm, and the average breaking strength reaches 4.85cN/dtex, which shows that the apocynum venetum treated by the degumming method has higher whiteness and mechanical property.
Physical and chemical properties of apocynum venetum after pilot plant test in the enterprises of the degumming methods of example 3 and example 4 of the invention are shown in Table 5.
Table 5 physical and chemical properties of the pilot-tested Apocynum venetum fibers in enterprises
| Type of apocynum venetum | Example 3 | Example 4 |
| Weight loss ratio (%) | 46.5 | 46.0 |
| Whiteness degree | 76.5 | 74.2 |
| Single fiber strength (cN) | 8.5 | 8.2 |
| Pectin content (%) | 5.13 | 4.69 |
From the results in Table 5, it can be seen that the apocynum venetum degumming agent and the degumming method of the invention have stable pilot-scale performance, good degumming effect, good whiteness, good strength and low pectin residue.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The degumming method for the apocynum venetum is characterized by comprising the following steps of:
(1) Adding herba Apocyni Veneti into acid solution, heating at 55-65deg.C for 55-75 min, and cleaning, wherein the bath ratio of herba Apocyni Veneti to the acid solution is 1 (20-50);
(2) Adding alkali liquor into the apocynum venetum cleaned in the step (1), and cleaning after heating for 95-105 min at 65-70 ℃, wherein the bath ratio of the apocynum venetum to the alkali liquor is 1 (20-50);
(3) Adding a mixed solution containing complex enzyme and oxidant into the apocynum venetum cleaned in the step (2), heating at 70-80 ℃ for 45-85 min, cleaning, and drying to obtain apocynum venetum refined dry fiber, wherein the bath ratio of the apocynum venetum to the mixed solution is 1 (20-50);
In the step (2), the alkali liquor comprises, by mass, 4.5% -6.5% of sodium hydroxide, 4% -5% of sodium silicate, 2.5% -4.5% of sodium sulfite and 3% -3.5% of penetrating agent;
In the step (3), the compound enzyme comprises 60-64 parts of pectase, 17-19 parts of hemicellulase, 10-13 parts of lignin enzyme, 3-5 parts of laccase and 4-5 parts of xylanase.
2. The method for degumming a apocynum venetum according to claim 1, wherein in the step (1), the acid in the acid liquor is sulfuric acid, the mass of the sulfuric acid is 1.25% -2% of that of the apocynum venetum, the heating temperature is 60-65 ℃ and the heating time is 55-60 min.
3. The method for degumming a apocynum venetum according to claim 2, wherein in the step (1), the mass of the sulfuric acid is 1.75% -2% of the mass of the apocynum venetum.
4. The method for degumming a apocynum venetum according to claim 1, wherein in the step (2), the heating time is 100min-105min.
5. The method for degumming a apocynum venetum according to claim 1, wherein in the step (3), the concentration of the complex enzyme in the mixed solution is 15g/L to 25g/L.
6. The method for degumming a apocynum venetum according to claim 1, wherein in the step (3), the oxidant is hydrogen peroxide, and the concentration of the hydrogen peroxide in the mixed solution is 4g/L to 6g/L.
7. A method of degumming a kendir according to claim 3, wherein in step (3), the washing is a hot water washing followed by a cold water washing.
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