CN113373527B - Eutectic solvent and microorganism combined degumming method for flax roving - Google Patents
Eutectic solvent and microorganism combined degumming method for flax roving Download PDFInfo
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Abstract
The invention relates to a eutectic solvent and microorganism combined degumming method for flax roving, belonging to the technical field of biology. Adding the flax roving into an aqueous solution of a eutectic solvent, heating and then taking out, wherein the aqueous solution of the eutectic solvent enables fibers in the flax roving to be dispersed and destroys hydrogen bonds among hemicellulose and pectin molecules in the flax roving, thereby promoting the removal of colloid in the flax roving; and washing the taken flax roving to remove the residual eutectic solvent aqueous solution on the surface, and inoculating degumming microorganisms to carry out microbial degumming. According to the method, the flax roving is pretreated by using the eutectic solvent aqueous solution, and the eutectic solvent aqueous solution can effectively disperse the roving fiber and remove part of colloid, so that the subsequent biological degumming is facilitated. The process does not need acid-base pretreatment, is environment-friendly, has good degumming effect, and has good application prospect in flax roving degumming.
Description
Technical Field
The invention belongs to the technical field of biology, and particularly relates to a combined degumming method of a eutectic solvent and microorganisms of flax roving.
Background
The flax has a scientific name Linum usittissimum L, belongs to the Linaceae, linum, and can be classified into flax for fiber, flax for oil and flax for oil fiber according to the application. Currently, the flax fibers used in the flax textile industry worldwide are mainly derived from fiber flax. Flax fiber, the earliest natural fiber used by humans, was grown and used by ancient egyptians as early as two thousand years ago. The flax fiber has good moisture absorption and quick heat dissipation, has the functions of ultraviolet resistance and static resistance, and is widely applied to the textile field. In recent years, with the improvement of the living standard of consumers, the enhancement of the environmental protection concept and the change of the consumption concept, the consumption of textiles taking flax fibers as raw materials is remarkably increased. China has become one of the most important countries for flax textile consumption, and flax fiber products have wide market prospects.
Before spinning, the flax fiber can be processed in the subsequent process, wherein the roving scouring and bleaching process is a key link in the process, and the roving is chemically scoured to remove pectin, hemicellulose, lignin and other colloid components in the fiber, so that the fiber splitting degree is further improved, and the later-stage spinning is facilitated. In the prior art, a large amount of chemical reagents such as acid, alkali and sodium chlorite are used in the roving scouring process, so that the problems of more waste water, high energy consumption, poor fiber quality and the like exist. In order to solve the problems of chemical degumming, the biological degumming technology is gradually applied to the scouring process of the flax roving, but the biological degumming still has the problems of long degumming time and low efficiency, so the biological degumming technology is limited in the scouring process of the flax roving. The eutectic solvent (DES) is a two-component eutectic mixture formed by combining a hydrogen bond acceptor and a hydrogen bond donor, and the DES has the characteristics of wide raw material source, simple preparation, no toxicity and the like, so the DES is widely applied to the field of fiber processing in recent years.
Yu Wang et al, in patent publication No. CN110284200A, a method for the pretreatment of ramie degumming is disclosed. The method comprises the steps of mixing raw ramie with a eutectic solvent, heating, stirring, washing with water, and filtering to obtain the treated ramie. The method adopts the eutectic solvent to carry out degumming pretreatment on the ramie raw ramie, and has the advantages of simple process, easy synthesis of raw materials, low cost, no toxicity, biodegradability, no pollution and high degumming efficiency, but the pretreatment process needs to be carried out in an oil bath at 120 ℃, so the method has large energy consumption in mass production and certain difficulty in industrial popularization. Compared with ramie fibers, the flax fibers are shorter, a small amount of colloid is needed to be connected among the fibers, and the colloid cannot be completely removed, so that the application of the eutectic solvent in the flax fibers needs further research.
Xing Yanjun et al in patent publication No. CN104178527B, a method for the eutectic solvent pyrolysis of cellulosic feedstocks is disclosed. Adding alkali metal carbonate into high-polarity polyol according to a molar ratio of 5:1-10; then adding the cellulose raw material which is pretreated by mechanical shearing or physical and chemical combination into the solution, heating for 1-6 hours at 130-180 ℃, and extracting the generated glucose-polyalcohol solution. The method has simple process and low cost, is suitable for industrially decomposing cellulose biomass, but still has certain pollution to the environment because the method needs physical and chemical combination pretreatment on the cellulose raw material before use.
3238 Zxft 3238 in the patent with publication No. CN109468872A, a method for extracting and separating loofah sponge cellulose by using choline eutectic solvent is disclosed. The loofah sponge powder extracted by benzene alcohol is obtained by treating benzene alcohol mixed solution, choline chloride and oxalic acid are further adopted to prepare choline eutectic solvent treated loofah sponge powder, the eutectic solvent is subjected to ultrasonic treatment and centrifugation to obtain precipitate, and the loofah sponge cellulose is obtained by washing and drying. The loofah sponge cellulose prepared by the method has low energy consumption, little pollution and high product yield, but the method uses the benzene alcohol mixed solution in the pretreatment and has the problem of solvent residue.
Disclosed in patents CN102002468B such as Ding Yao are Pseudomonas fluorescens DA4 strain and its obtaining method and application. The strain has the capability of producing pectinase and hemicellulase and has flax degumming activity, and the flax degumming period can be shortened, the flax fiber yield can be increased, the strength of the flax fiber can be increased, and the flax fiber quality can be improved by using the strain for flax microbial degumming. The method can be used for degumming flax protocorm, scouring roving and biological pretreatment of flax fabric, but the degumming time still needs 1-4 days, and the efficiency needs to be further improved.
The prior patent technologies have the problems of long biological degumming time, complex eutectic solvent treatment process and the like. Thus, there remains a need for further optimization and improvement of the process for bioscouring flax rovings in industry.
Disclosure of Invention
The invention aims to provide a method for degumming flax roving by combining a eutectic solvent and microorganisms, wherein the flax roving is pretreated by adopting a eutectic solvent aqueous solution, the fiber in the flax roving is dispersed by the eutectic solvent aqueous solution, part of colloid in the flax roving is removed, and then the flax roving is degummed by inoculating the microorganisms, so that the technical problems of long time consumption, complex treatment process and poor degumming effect of biological degumming are solved.
According to the purpose of the invention, the eutectic solvent and microorganism combined degumming method for the flax roving comprises the following steps:
(1) Adding the flax roving into an aqueous solution of a eutectic solvent, heating and then taking out, wherein the aqueous solution of the eutectic solvent enables fibers in the flax roving to be dispersed and destroys hydrogen bonds among hemicellulose and pectin molecules in the flax roving, thereby promoting the removal of colloid in the flax roving;
(2) And (2) washing the flax roving taken out in the step (1) to remove the water solution of the eutectic solvent remained on the surface, and inoculating degumming microorganisms to carry out microbial degumming.
Preferably, the eutectic solvent is a mixture of choline chloride and a hydrogen bond donor.
Preferably, the hydrogen bond donor is urea or oxalic acid.
Preferably, the aqueous solution of the eutectic solvent is obtained by mutually dissolving the eutectic solvent and water, and the mass fraction of the water in the aqueous solution of the eutectic solvent is 10-40%;
preferably, the mass ratio of the flax roving in the step (1) to the aqueous solution of the eutectic solvent is 1 (40-60).
Preferably, the heating is water bath heating, the temperature is 80-100 ℃, and the time is 1-2 h.
Preferably, the degumming microorganism is a microorganism with a preservation number of CCTCC NO: m2020439 Bacillus subtilis HR5, classified and named as: bacillus subtilis HR5, latin literature name: bacillus subtilis HR5, wherein the unit name of the strain to be preserved is as follows: china center for type culture Collection, addresses: wuhan university, the preservation date is: 21/8/2020, the accession number is: CCTCC NO: m2020439.
Preferably, the volume of the degummed microbial liquid accounts for 4-6% of the volume of the culture liquid after inoculation.
Preferably, the temperature for microbial degumming in the step (2) is 35-38 ℃ and the time is 14h-20 h.
Preferably, degumming microorganisms are inoculated to the washed flax roving in the step (2), and the mass ratio of the flax roving to the water in the culture solution is 1 (50-80).
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
(1) According to the eutectic solvent-biological combined degumming method for the flax roving, the flax roving is pretreated by the eutectic solvent, the fiber can be dispersed by the pretreatment of the eutectic solvent, the hydrogen bonds between hemicellulose and pectin molecules can be destroyed by the eutectic solvent, so that the degradation of the hemicellulose and pectin molecules is promoted, the flax roving is subjected to microbial degumming after the pretreatment, the biological degumming time is obviously shortened, and the biological degumming efficiency is improved.
(2) After the degumming method is adopted, the breaking strength of the processed and produced fiber can reach more than 21.01 cN/dtex.
(3) Preferably, the microorganisms used in the invention are those with a preservation number of CCTCC NO: the Bacillus subtilis HR5 of M2020439 has rich degrading enzyme systems and very low cellulase, and avoids the damage to fibers in the degumming process.
(4) Preferably, the water solution phase of the used eutectic solvent is compared with the eutectic solvent, and when the flax roving fiber is treated at high temperature, the fiber can be effectively prevented from being damaged while part of colloid is removed.
Drawings
Fig. 1 is a scanning electron micrograph of flax roving fiber without any treatment.
Fig. 2 is a scanning electron microscope image of flax roving fiber after microbial degumming treatment.
FIG. 3 is a scanning electron microscope image of flax roving fiber after pretreatment of eutectic solvent aqueous solution consisting of choline chloride and urea.
FIG. 4 is a scanning electron microscope image of flax roving fiber after pretreatment by a eutectic solvent aqueous solution composed of choline chloride and oxalic acid.
Fig. 5 is a scanning electron microscope image of flax roving fiber degummed by combining pretreatment of eutectic solvent aqueous solution consisting of choline chloride and urea with microorganisms.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention. In addition, the technical features involved in the respective embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The flax roving of the present invention is a prior art concept and is derived from the following sources: the flax plants are processed into scutched flax through the procedures of harvesting, retting and the like, and the scutched flax is processed into flax roving through the procedures of carding, slivering, drawing and the like.
The invention relates to a combined degumming method of a eutectic solvent and microorganisms of flax roving, which comprises the following steps:
(1) Drying a certain amount of flax roving to constant weight for later use; the drying temperature is preferably 105 ℃;
(2) Preparing a eutectic solvent aqueous solution with the water content of 10-40%, and mixing the dried flax roving obtained in the step (1) and the eutectic solvent aqueous solution according to a bath ratio of 1:40 to 1:60, mixing, treating in water bath at 80-100 ℃ for 1-2h, taking out the flax roving, and washing to remove residual eutectic solvent water solution on the surface of the flax;
(3) And (3) inoculating the flax roving pretreated in the step (2) into degumming microorganisms for degumming.
More specifically, the method for degumming flax roving by combining eutectic solvent and microorganism comprises the following steps:
s1, eutectic solvent pretreatment: (1) choline chloride: urea or choline chloride: oxalic acid is added in a molar ratio of 1: (1-2) mixing, heating and melting the mixture according to the proportion to synthesize a eutectic solvent; most preferably, the eutectic solvent consists of choline chloride and urea, and the molar ratio of the choline chloride to the urea is 1: 2; mixing the eutectic solvent with water to prepare a eutectic solvent water solution with the water content of 10-40%; (2) And (3) mixing the dried flax roving with the eutectic solvent aqueous solution according to the mass ratio of 1:40 to 1: 60. mixing, carrying out water bath treatment at the temperature of 60-100 ℃ for 1-2h, taking out the flax roving after the treatment is finished, and washing to remove the residual eutectic solvent water solution on the surface of the flax.
S2, seed culture of the degumming strain: the strain preserved at minus 80 ℃ in a freezing way is inoculated into a 500mL triangular flask filled with 100 to 200mL of seed culture medium by the inoculation amount of 2 to 5 percent and cultured for 6 to 8 hours at the temperature of 35 to 37 ℃ and the rotating speed of 150 to 180 rpm. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of degumming strains: inoculating the seed liquid obtained by the step S2 culture into a 100L amplification tank filled with 30-50L amplification culture medium according to the inoculation amount of 1-5%, rotating at 50-80rpm at the temperature of 35-37 ℃, and keeping the rotation speed of 2-6 m 3 H, culturing for 6-8 h under ventilation. Wherein the formula of the amplification culture medium comprises 5-15 g/L of yeast powder, 10-20 g/L of peptone and K 2 HPO 4 0～0.5g/L，MgSO 4 0～1.5g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:50 to 1:80, adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be between 35 and 38 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 4-6%; in a quantity of 1-3 m per ton 3 Ventilating at a ventilation rate/h, and degumming the degummed bacterial liquid for 14-20h.
FIG. 1 is a scanning electron microscope image of flax roving fiber without any treatment, and we can see that most of the fiber surface is covered with colloid and the fibers are adhered by the colloid; FIG. 2 is a scanning electron microscope image of the fiber of flax roving after the microbial degumming treatment, from FIG. 2, it can be seen that a small part of the surface gum of the fiber is removed, and a small amount of the fiber with smooth surface can be observed; FIG. 3 is a scanning electron microscope image of flax roving fiber after pretreatment of eutectic solvent aqueous solution composed of choline chloride and urea, and it can be seen from FIG. 3 that most of the colloid on the fiber surface has been degraded, and only a small amount of colloid remains; FIG. 4 is a scanning electron microscope image of flax roving fiber pretreated by a eutectic solvent aqueous solution composed of choline chloride and oxalic acid, wherein part of fiber colloid can be seen to be removed, but large blocks of colloid exist on the surface of a small part of fiber; fig. 5 is a scanning electron microscope image of flax roving fiber which is formed by pre-treating eutectic solvent aqueous solution consisting of choline chloride and urea and degumming by microorganisms, and the situation that the surface colloid of the fiber is degraded and the fibers are basically separated can be seen.
The following are specific examples:
example 1
S1, eutectic solvent pretreatment: (1) choline chloride: urea is added into the mixture in a molar ratio of 1:2, mixing, heating and melting to synthesize a eutectic solvent; mixing the eutectic solvent with water to obtain a eutectic solvent water solution with the water content of 10%; (2) And (3) mixing the dried flax roving with the eutectic solvent aqueous solution according to the mass ratio of 1:60, mixing, carrying out water bath treatment at the temperature of 90 ℃ for 1h, taking out the flax roving after the treatment is finished, and washing to remove the residual eutectic solvent aqueous solution on the surface of the flax.
S2, seed culture of the degumming strain: the strain frozen at-80 ℃ was inoculated into a 500mL Erlenmeyer flask containing 100mL of seed medium at a temperature of 37 ℃ and a rotation speed of 150rpm for 6 hours at an inoculum size of 2%. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of the degumming strain: inoculating the seed solution obtained by culturing in step S2 into a 100L amplification tank containing 30L amplification culture medium at 3% inoculum size, at 37 deg.C, at 50rpm, and with ventilation capacity of 3m 3 And h, culturing for 6h under the condition of/h. WhereinThe formula of the amplification culture medium comprises 5g/L of yeast powder, 10g/L of peptone and K 2 HPO 4 0.2g/L，MgSO 4 0.5g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:60, adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be maintained at 37 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 5 percent; in an amount of 1m per ton 3 Ventilating at a ventilation rate/h, and degumming the degummed bacterial liquid for 16h.
After the cementation is finished, the subsequent procedures of bleaching, drying and the like are carried out. The breaking strength of the fiber is 22.01 +/-0.41 cN/dtex, and the whiteness is 71.
Example 2
S1, eutectic solvent pretreatment: (1) choline chloride: urea is added in a molar ratio of 1:2, mixing, heating and melting to synthesize a eutectic solvent; mixing the eutectic solvent with water to obtain a eutectic solvent water solution with the water content of 20%; (2) And (3) mixing the dried flax roving with the eutectic solvent aqueous solution according to the mass ratio of 1:60, mixing, treating in water bath at the temperature of 80 ℃ for 1.5h, taking out the flax roving after the treatment is finished, and washing to remove the residual eutectic solvent water solution on the surface of the flax.
S2, seed culture of the degumming strain: the strain frozen at-80 ℃ was inoculated in a 500mL Erlenmeyer flask containing 200mL of seed medium at a temperature of 35 ℃ and at a rotation speed of 180rpm for 8 hours in an inoculum size of 3%. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of degumming strains: inoculating the seed solution obtained by culturing in step S2 into a 100L amplification tank containing 50L amplification medium at 3% inoculum size, and introducing air flow of 2m at 35 deg.C and 60rpm 3 And culturing for 7 hours under the condition of/h. Wherein the formulation of the amplification culture medium comprises 8g/L of yeast powder, 15g/L of peptone and K 2 HPO 4 0.2g/L，MgSO 4 0.7g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:70 adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be maintained at 35 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 5 percent; in an amount of 2m per ton 3 Ventilating at a ventilation rate/h, and degumming the degummed bacterial liquid for 18h.
And after the degumming, performing subsequent procedures of bleaching, drying and the like. The breaking strength of the fiber is 23.61 +/-0.29 cN/dtex, and the whiteness is 73.
Example 3
S1, eutectic solvent pretreatment: (1) choline chloride: urea is added in a molar ratio of 1:2, mixing, heating and melting to synthesize a eutectic solvent; mixing the eutectic solvent with water to obtain a eutectic solvent water solution with the water content of 30%; (2) And (3) mixing the dried flax roving with the eutectic solvent aqueous solution according to the bath mass ratio of 1: mixing 50 parts of the raw materials, treating the mixture in a water bath at the temperature of 100 ℃ for 1.5h, taking out the flax roving after the treatment is finished, and washing to remove the residual eutectic solvent water solution on the surface of the flax.
S2, seed culture of the degumming strain: the strain frozen at-80 ℃ was inoculated in a 500mL Erlenmeyer flask containing 200mL of seed medium at an inoculum size of 5% and cultured at a temperature of 36 ℃ and a rotation speed of 170rpm for 6 hours. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of degumming strains: inoculating the seed solution obtained by culturing in step S2 into a 100L amplification tank containing 50L amplification medium at a temperature of 36 deg.C, a rotation speed of 70rpm, and an air flow of 4m 3 And culturing for 6h under the condition of/h. Wherein the formulation of the amplification culture medium comprises yeast powder 10g/L, peptone 12g/L, and K 2 HPO 4 0.3g/L，MgSO 4 1.0g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:80 adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be 36 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 6 percent; in an amount of 1m per ton 3 Ventilating at a ventilation rate/h, and degumming the degummed bacterial liquid for 20h.
After the cementation is finished, the subsequent procedures of bleaching, drying and the like are carried out. The breaking strength of the fiber is 21.07 +/-0.53 cN/dtex, and the whiteness is 78.
Example 4
S1, eutectic solvent pretreatment: (1) choline chloride: urea is added into the mixture in a molar ratio of 1:2, mixing, heating and melting to synthesize a eutectic solvent; mixing the eutectic solvent with water to obtain a eutectic solvent water solution with the water content of 40%; (2) And (3) mixing the dried flax roving with the eutectic solvent aqueous solution according to the mass ratio of 1:60, mixing, carrying out water bath treatment at the temperature of 100 ℃ for 1.5 hours, taking out the flax roving after the treatment is finished, and washing to remove the residual eutectic solvent water solution on the surface of the flax.
S2, seed culture of the degumming strain: the strain frozen at-80 ℃ was inoculated in a 500mL Erlenmeyer flask containing 100mL of seed medium at an inoculum size of 4% and cultured at 37 ℃ for 8 hours at a rotation speed of 180 rpm. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of degumming strains: inoculating the seed solution obtained by culturing in step S2 into a 100L amplification tank containing 30L amplification medium at 3% inoculum size, rotating at 35 deg.C and 80rpm, and ventilating at 5m 3 And culturing for 7 hours under the condition of/h. Wherein the formulation of the amplification culture medium comprises 8g/L of yeast powder, 20g/L of peptone and K 2 HPO 4 0.5g/L，MgSO 4 0.6g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:60, adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be 37 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 5 percent; in a quantity of 3m per ton 3 Ventilating at a ventilation rate/h, and degumming the degummed bacterial liquid for 16h.
After the cementation is finished, the subsequent procedures of bleaching, drying and the like are carried out. The breaking strength of the fiber is 23.58 +/-0.61 cN/dtex, and the whiteness is 72.
Example 5
S1, eutectic solvent pretreatment: (1) choline chloride: oxalic acid is added into the mixture in a molar ratio of 1:2, mixing, heating and melting to synthesize a eutectic solvent; mixing the eutectic solvent with water to obtain a eutectic solvent water solution with the water content of 10%; (2) And (3) mixing the dried flax roving with the eutectic solvent aqueous solution according to the mass ratio of 1:60, mixing, carrying out water bath treatment at the temperature of 90 ℃ for 1.5 hours, taking out the flax roving after the treatment is finished, and washing to remove the residual eutectic solvent water solution on the surface of the flax.
S2, seed culture of the degumming strain: the strain frozen at-80 ℃ was inoculated in a 500mL Erlenmeyer flask containing 200mL of seed medium at a temperature of 35 ℃ and at a rotation speed of 180rpm for 8 hours in an inoculum size of 3%. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of degumming strains: inoculating the seed solution obtained by culturing in step S2 into a 100L amplification tank containing 50L amplification medium at 3% inoculum size, and introducing air flow of 2m at 35 deg.C and 60rpm 3 And culturing for 7 hours under the condition of/h. Wherein the formula of the amplification culture medium comprises 8g/L of yeast powder, 15g/L of peptone and K 2 HPO 4 0.2g/L，MgSO 4 0.7g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:70 adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be maintained at 35 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 5 percent; in an amount of 2m per ton 3 Ventilating at a ventilation rate/h, and degumming the degummed bacterial liquid for 18h.
And after the degumming, performing subsequent procedures of bleaching, drying and the like. The breaking strength of the fiber is 19.11 +/-0.57 cN/dtex, and the whiteness is 65. Compared with the eutectic solvent composed of choline chloride and urea, the fiber produced by the embodiment has lower breaking strength and whiteness, and the fiber quality is slightly poor.
Example 6
S1, eutectic solvent pretreatment: (1) choline chloride: oxalic acid is added in a molar ratio of 1:1, mixing, heating and melting to synthesize a eutectic solvent; mixing the eutectic solvent and water to prepare a eutectic solvent water solution with the water content of 20%; (2) And (3) mixing the dried flax roving with the eutectic solvent aqueous solution according to the mass ratio of 1:60, mixing, treating in water bath at the temperature of 80 ℃ for 1.5h, taking out the flax roving after the treatment is finished, and washing to remove the residual eutectic solvent water solution on the surface of the flax.
S2, seed culture of the degumming strain: the strain frozen at-80 ℃ was inoculated in a 500mL Erlenmeyer flask containing 200mL of seed medium at a temperature of 37 ℃ and at a rotation speed of 180rpm for 8 hours at an inoculum size of 3%. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of degumming strains: inoculating the seed liquid obtained by culturing in the step S2 with 50L of amplification medium according to the inoculation amount of 3%In a 100L amplification tank, the temperature is 37 deg.C, the rotation speed is 60rpm, and the ventilation rate is 2m 3 And culturing for 7 hours under the condition of/h. Wherein the formulation of the amplification culture medium comprises 8g/L of yeast powder, 15g/L of peptone and K 2 HPO 4 0.2g/L，MgSO 4 0.7g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:60, adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be maintained at 37 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 5 percent; in an amount of 2m per ton 3 Ventilating at a ventilation rate/h, and degumming the degummed bacterial liquid for 18h.
And after the degumming, performing subsequent procedures of bleaching, drying and the like. The breaking strength of the fiber is 20.24 +/-0.94 cN/dtex, and the whiteness is 68. Compared with the eutectic solvent composed of choline chloride and urea, the fiber produced by the embodiment has lower breaking strength and whiteness, and the fiber quality is slightly poor.
Comparative example 1
Essentially the same procedure as for the preparation of example 1, except that the eutectic solvent pretreatment step in step S1 was absent.
S1, mixing the dried flax roving and an aqueous solution according to a mass ratio of 1:60, mixing, and treating in water bath at 90 ℃ for 1h for later use.
S2, seed culture of the degumming strain: the strain frozen at-80 ℃ was inoculated into a 500mL Erlenmeyer flask containing 100mL of seed medium at a temperature of 37 ℃ and a rotation speed of 150rpm for 6 hours at an inoculum size of 2%. Wherein the formulation of the seed culture medium is 10g/L of peptone and 5g/L, naCl g/L of yeast powder.
S3, amplification culture of degumming strains: inoculating the seed solution obtained by culturing in step S2 into a 100L amplification tank containing 30L amplification medium at 3% inoculum size, with temperature of 37 deg.C, rotation speed of 50rpm, and ventilation volume of 3m 3 And culturing for 6h under the condition of/h. Wherein the formulation of the amplification culture medium comprises 5g/L of yeast powder, 10g/L of peptone and K 2 HPO 4 0.2g/L，MgSO 4 0.5g/L。
S4, biological degumming treatment: mixing the flax roving and water according to a bath ratio of 1:60, adding the mixture into a degumming tank, and controlling the temperature in the degumming tank to be maintained at 37 ℃; inoculating degumming bacterial liquid according to the inoculation amount of 5 percent; to each endTon 1m 3 Ventilating at a ventilation rate/h, and degumming for 24h by using the degumming bacterial liquid.
And after the degumming, performing subsequent procedures of bleaching, drying and the like. The breaking strength of the fiber is 18.29 +/-0.36 cN/dtex, and the whiteness is 65. Compared with the method of adopting the eutectic solvent and the microorganism for combined degumming, the fiber produced by the comparative example has lower breaking strength and whiteness, and poorer fiber quality.
The embodiment shows that the method of the invention adopts the eutectic solvent treatment to the flax roving and then adopts the microbial degumming treatment to effectively shorten the degumming time of the flax roving, and the flax yarn produced by the method exceeds the national high-class product standard.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A combined degumming method of a eutectic solvent and microorganisms of flax roving is characterized by comprising the following steps:
(1) Adding the flax roving into an aqueous solution of a eutectic solvent, heating and then taking out, wherein the aqueous solution of the eutectic solvent enables fibers in the flax roving to be dispersed and destroys hydrogen bonds among hemicellulose and pectin molecules in the flax roving, thereby promoting the removal of colloid in the flax roving; the eutectic solvent is a mixture of choline chloride and a hydrogen bond donor; the hydrogen bond donor is urea or oxalic acid;
(2) Washing the flax roving taken out in the step (1) to remove the water solution of the eutectic solvent remained on the surface, and inoculating degumming microorganisms to carry out microbial degumming, wherein the degumming microorganisms are flax rovings with the preservation number of CCTCC NO: of M2020439Bacillus subtilis HR5, the time for microbial degumming is 14h-20 h.
2. The method for degumming flax roving with a eutectic solvent and microorganisms in combination according to claim 1, wherein the aqueous solution of the eutectic solvent is obtained by mutually dissolving the eutectic solvent and water, and the mass fraction of water in the aqueous solution of the eutectic solvent is 10-40%.
3. The method for degumming flax roving with a eutectic solvent and microorganisms in combination according to claim 2, wherein the mass ratio of the flax roving to the aqueous solution of the eutectic solvent is 1 (40-60).
4. The process for degumming flax roving with a eutectic solvent in combination with a microorganism according to claim 1, characterized in that said heating is a water bath heating at a temperature comprised between 80 ℃ and 100 ℃ and for a time comprised between 1h and 2h.
5. The method for degumming flax roving with a eutectic solvent and a microorganism in combination according to claim 1, wherein the volume of the degumming microorganism solution is 4-6% of the volume of the inoculated culture solution.
6. The process for degumming flax rovings with a eutectic solvent in combination with microorganisms according to claim 1, wherein the temperature for microbial degumming in step (2) is between 35 ℃ and 38 ℃.
7. The method for degumming flax roving with eutectic solvent and microorganisms in combination according to claim 1, wherein degumming microorganisms are inoculated to flax roving after washing in step (2), and the mass ratio of flax roving to water in the culture solution is 1 (50-80).
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