CN113789586B - Corn fiber, preparation method and fabric thereof - Google Patents
Corn fiber, preparation method and fabric thereof Download PDFInfo
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- CN113789586B CN113789586B CN202111112877.6A CN202111112877A CN113789586B CN 113789586 B CN113789586 B CN 113789586B CN 202111112877 A CN202111112877 A CN 202111112877A CN 113789586 B CN113789586 B CN 113789586B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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Abstract
The application relates to the technical field of new textile materials, and particularly discloses a corn fiber, a preparation method and a fabric thereof; the corn fiber is prepared from the following raw materials in parts by weight: 45-75 parts of polylactic acid, 20-35 parts of modified bamboo powder and 3-8 parts of filler; the preparation method comprises the following steps: weighing polylactic acid, modified bamboo powder and filler, mixing, and stirring to obtain a mixture; the mixture is melted and extruded, and then the mixture is dried in vacuum to prepare polylactic acid particles; melt spinning polylactic acid particles to prepare corn fibers; the fabric is made of corn fiber; has the advantage of shortening the natural degradation time of the corn fiber in the soil.
Description
Technical Field
The application relates to the technical field of new textile materials, in particular to a corn fiber, a preparation method and a fabric thereof.
Background
The corn fiber is prepared by taking agricultural products containing starch such as corn, wheat and beet as raw materials, fermenting the raw materials to generate lactic acid, and then performing polycondensation and melt spinning on the lactic acid, and is also called polylactic acid fiber; the corn fiber is a synthetic fiber which can be planted as a raw material and is easy to plant, and wastes can be naturally degraded in nature.
The corn fiber can be decomposed into carbon dioxide and water under the action of microorganisms in soil, and is an ecological fiber capable of sustainable development; because corn fiber is a macromolecular polymer, the polymer needs to be continuously decomposed into small molecular substances in the degradation process, and then the degradation is gradually carried out.
Therefore, the corn fiber is buried in the soil, and the natural degradation time is long.
Disclosure of Invention
In order to shorten the natural degradation time of corn fibers in soil, the application provides the corn fibers, a preparation method and a fabric thereof.
In a first aspect, the present application provides a corn fiber, which adopts the following technical scheme:
the corn fiber is prepared from the following raw materials in parts by weight: 45-75 parts of polylactic acid, 20-35 parts of modified bamboo powder and 3-8 parts of filler.
By adopting the technical scheme, the corn fiber is prepared by matching the polylactic acid and the modified bamboo powder, when the corn fiber is buried in soil for degradation, the better water absorption effect of the modified bamboo powder is matched with the better water diffusion effect of the polylactic acid, so that the water molecules are accelerated to reach all positions of the molecular chain of the corn fiber, the water molecules are promoted to attack ester bonds in the polylactic acid molecules, the main chain of the macromolecule is broken, the broken molecular chain is further contacted with water, the hydrolytic degradation of the corn fiber is promoted, and the natural degradation time of the corn fiber in the soil is shortened.
The polylactic acid, the modified bamboo powder and the filler are matched, the polylactic acid and the modified bamboo powder are used as frameworks, the filler is used as an auxiliary material, and in the degradation process of the corn fiber, the filler can loosen the soil structure and promote the growth and the propagation of saprophytic bacteria in the soil, so that the degradation of the saprophytic bacteria to the corn fiber is promoted; and the degradation speed of the modified bamboo powder in the corn fiber is higher, and when the modified bamboo powder is gradually degraded, polylactic acid molecules in the corn fiber are gradually exposed, so that the polylactic acid molecules are in large-area contact with saprophytic bacteria in soil, the degradation of the corn fiber is promoted, and the natural degradation time of the corn fiber in the soil is shortened.
Preferably, the modified bamboo powder is prepared by the following method;
the dried bamboo powder is pretreated by adopting a mixed solution of sodium hydroxide and hydrogen peroxide, and then is subjected to esterification modification treatment by adopting citric acid.
By adopting the technical scheme, after the bamboo powder is pretreated by the mixed solution of sodium hydroxide and hydrogen peroxide, the content of carboxyl groups on the surface of the bamboo powder is improved, and the subsequent citric acid modification treatment is facilitated; the citric acid contains 1 hydroxyl and 3 carboxyl, and the carboxyl group on the surface of the pretreated bamboo powder and the hydroxyl in the citric acid are subjected to esterification reaction to load the citric acid on the surface of the bamboo powder, so that the modified bamboo powder is prepared.
The citric acid loaded on the surface of the modified bamboo powder is used for promoting the growth and the propagation of saprophytic bacteria, fungi in the saprophytic bacteria play a main role in degrading the corn fibers, and the citric acid can promote the growth and the propagation of the fungi, so that the degradation of the corn fibers is promoted, and the natural degradation time of the corn fibers in the soil is shortened.
Preferably, the filler consists of a solution of the supported bentonite and the ethylcellulose in a weight ratio of 1: 0.1-0.35.
By adopting the technical scheme, the loaded bentonite is matched with the ethyl cellulose solution, and the loaded bentonite is coated by utilizing the better viscosity of the ethyl cellulose solution, so that the loaded material in the bentonite is blocked on one hand, and the compatibility of the filler with polylactic acid and modified fiber is improved on the other hand.
When the corn fiber is degraded, the modified bamboo powder is firstly degraded, the filler does not need to be degraded, the bentonite pore structure is utilized to promote the migration of water molecules in soil in capillary channels, and the hydrolysis degradation speed of polylactic acid molecules is improved, so that the natural degradation speed of the corn fiber is improved; meanwhile, the bentonite is used as a filler, so that saprophytic bacteria in soil can be promoted to be loaded on the surface of the bentonite, and after the modified bamboo powder is degraded, the saprophytic bacteria absorb organic matters generated by degradation of the modified bamboo powder, so that growth and propagation of saprophytic bacteria are promoted, degradation of polylactic acid molecules is further promoted, and the natural degradation speed of the corn fiber is increased.
Preferably, the supported bentonite is prepared by the following method:
weighing tartaric acid, placing in water, stirring and dissolving to obtain a stirring solution; then placing the bentonite into the stirring liquid, oscillating, ultrasonically dispersing, standing, filtering and taking out the bentonite, and draining the surface water to obtain the load bentonite.
By adopting the technical scheme, the bentonite is used for loading tartaric acid, in the degradation process of the corn fiber, the saprophytic bacteria firstly degrade ethyl cellulose on the surface of the filler, then the tartaric acid in the bentonite is gradually contacted with the saprophytic bacteria in the soil, particularly penicillium in fungi, and the growth and propagation speed of the penicillium can be accelerated by virtue of the acid groups of the tartaric acid, so that the natural degradation speed of the corn fiber is accelerated.
Preferably, the ethyl cellulose solution is prepared by the following method: weighing ethyl cellulose, placing the ethyl cellulose in ethanol, stirring and dissolving to obtain an ethyl cellulose solution.
By adopting the technical scheme, the ethyl cellulose is dissolved to prepare the ethyl cellulose solution, so that the ethyl cellulose solution not only has a better bonding effect and can be adhered to the surface of the loaded bentonite, but also has better film forming property, and the loaded material in the loaded bentonite is conveniently sealed and locked in the pores inside the bentonite.
Preferably, the filler is prepared by the following method: and spraying the ethyl cellulose solution on the surface of the loaded bentonite, drying, and grinding to obtain the filler.
By adopting the technical scheme, the surface of the loaded bentonite is coated with the ethyl cellulose membrane, the ethyl cellulose membrane is firstly degraded by microorganisms in the degradation process of the corn fiber, and then tartaric acid in pores of the loaded bentonite is utilized to promote growth and reproduction of saprophytic bacteria, promote degradation of the corn fiber and shorten the natural degradation time of the corn fiber in soil.
Preferably, during the spraying process, the load bentonite is stirred at the rotating speed of 250-500r/min, and the spraying speed of the ethyl cellulose solution is 2-6 g/s.
By adopting the technical scheme, the stirring speed of the load bentonite and the spraying speed of the ethyl cellulose are limited, so that the ethyl cellulose solution is uniformly coated on the surface of the load bentonite, and the coating uniformity of the surface of the load bentonite is further improved.
In a second aspect, the present application provides a method for preparing corn fiber, which adopts the following technical scheme:
a preparation method of corn fiber comprises the following steps:
s1, weighing polylactic acid, modified bamboo powder and filler, mixing, and stirring to obtain a mixture;
s2, melting and extruding the mixture, and then drying in vacuum to obtain polylactic acid particles;
and S3, carrying out melt spinning on the polylactic acid particles to obtain the corn fiber.
By adopting the technical scheme, the polylactic acid, the modified bamboo powder and the filler are mixed, and the raw materials are uniformly distributed through stirring operation; in the subsequent granulation process, the polylactic acid, the modified bamboo and the filler in the polylactic acid granules are distributed more uniformly, and finally, the finished product is obtained by drawing.
The raw materials are uniformly dispersed, so that the corn fiber can be in contact with saprophytic bacteria in soil in a large area along with the degradation of the modified bamboo powder in the degradation process, the degradation speed of the corn fiber is improved, and the natural degradation time of the corn fiber in the soil is shortened.
Preferably, the melt spinning temperature is 225-255 ℃, the winding speed is 1600-1850m/min, the drawing temperature is 65-80 ℃, and the drawing multiple is 2.8-3.2 times.
By adopting the technical scheme, the corn fiber silk forming effect is good, and the corn fiber silk forming agent has good breaking strength.
A fabric is prepared from corn fiber or corn fiber prepared by corn fiber preparation method.
By adopting the technical scheme, the prepared corn fiber fabric has better degradability, and the degradation time of the corn fiber fabric can be shortened in the soil or compost environment.
In summary, the present application has the following beneficial effects:
1. the polylactic acid, the modified bamboo powder and the filler are matched, so that the corn fiber hydrolytic degradation speed is improved, and meanwhile, the corn fiber microbial degradation speed is improved, so that the natural degradation time of the corn fiber in soil is shortened.
2. The citric acid loaded on the surface of the modified bamboo powder promotes the growth and the propagation of saprophytic bacteria, fungi in the saprophytic bacteria play a main role in degrading the corn fibers, and the citric acid can promote the growth and the propagation of the fungi, so that the degradation of the corn fibers is promoted, and the natural degradation time of the corn fibers in the soil is shortened.
3. The polylactic acid, the modified bamboo powder, the loaded bentonite and the ethyl cellulose solution are matched, when the corn fiber is degraded, the pore structure of the bentonite promotes water molecules in soil to migrate in capillary channels, the hydrolysis degradation speed of polylactic acid molecules is improved, and therefore the natural degradation speed of the corn fiber is improved.
4. Polylactic acid, modified bamboo powder, load bentonite and ethyl cellulose solution are matched, the ethyl cellulose on the surface of the filler is degraded by saprophytic bacteria, then tartaric acid in the bentonite is gradually contacted with saprophytic bacteria in soil, and the growth and propagation speed of saprophytic bacteria can be accelerated by virtue of the acid groups of the tartaric acid, so that the natural degradation speed of the corn fiber is accelerated.
5. The corn fiber is adopted to prepare the fabric, so that the finished product corn fiber fabric has better degradability, the natural degradation time in soil can be shortened, and the degradation time in a compost environment can be shortened.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of modified bamboo powder
The bamboo powder in the following raw materials is purchased from silicone mining ltd in gao county; other raw materials and equipment are all sold in the market.
Preparation example 1: the modified bamboo powder is prepared by the following method:
material treatment: grinding the commercially available bamboo powder to 100-150nm, and drying at 50 ℃ for 3h to obtain bamboo powder;
pretreatment: weighing 5g of bamboo powder, adding the bamboo powder into 100ml of pretreatment solution, wherein the concentration of the pretreatment solution is 5 percent, and the pretreatment solution is NaOH and H with equal concentration 2 O 2 The mixed solution of (1); then placing the mixture in a room temperature environment and magnetically stirring the mixture for 180min to prepare a mixed solution; filtering the mixed solution, taking the pretreated bamboo powder, washing the bamboo powder with distilled water until the pH value of the filtrate for washing the bamboo powder is about 7, finishing washing, placing the washed bamboo powder in a 50 ℃ oven for blast drying for 24 hours, and storing the dried bamboo powder for later use to prepare a pretreated substance;
modification treatment: weighing 2g of the pretreatment substance and 0.4g of sodium hypophosphite, adding the mixture into 100ml of citric acid solution, wherein the concentration of the citric acid is 20mmol/L, and stirring for 35min at room temperature; pouring the stirred mixed solution into a nonmagnetic steel plate, putting the mixture into a 50 ℃ oven for forced air drying for 24 hours, then heating the mixture to 115 ℃, carrying out thermal reaction for 95 minutes, then cooling the mixture at room temperature, washing the bamboo powder for several times by using distilled water after cooling until the pH value of the filtrate for washing the bamboo powder is about 7, and finishing the washing; and finally, placing the cleaned bamboo powder in a 50 ℃ drying oven for forced air drying for 24h, and grinding the bamboo powder until the particle size is 100-150nm to obtain the modified bamboo powder.
Preparation example of Supported Bentonite
A table type constant temperature oscillator in the following raw materials was purchased from Shanghai Rio Automation technology Co., Ltd; the bentonite is calcium bentonite which is produced in Xingyuan mineral powder processing factories in Lingshu county, the particle size is 325 meshes, and other raw materials and equipment are all sold in the market.
Preparation example 2: the load bentonite is prepared by the following method:
weighing 2kg of tartaric acid, placing the tartaric acid into 98kg of water, stirring and dissolving to obtain a stirring solution; weighing 80kg of bentonite, placing into 100kg of stirring liquid, placing on a table type constant temperature oscillator, oscillating for 20min at the temperature of 45 ℃, performing ultrasonic dispersion for 20min at the temperature of 20kHz, standing for 20min, filtering, taking out the bentonite, and draining the moisture on the surface of the bentonite to obtain the loaded bentonite.
Preparation example of Ethyl cellulose solution
Ethanol in the following raw materials is purchased from Jinan culvert Bai chemical industry Co., Ltd, and the volume fraction is 95%; ethyl cellulose was purchased from Shenzhen Lefu Biotech, Inc.
Preparation example 3: the ethyl cellulose solution is prepared by the following method:
3kg of ethyl cellulose is weighed and placed in 97kg of ethanol to be stirred and dissolved, and then the ethyl cellulose solution is prepared.
Examples of preparation of fillers
Preparation example 4: the filler is prepared by the following method:
and weighing 0.25kg of the ethyl cellulose solution prepared in the preparation example 3, spraying the ethyl cellulose solution on the surface of 1kg of the loaded bentonite prepared in the preparation example 2, stirring the loaded bentonite at the rotating speed of 350r/min in the spraying process, drying the ethyl cellulose solution at room temperature after the spraying is finished, and then grinding the dried solution until the particle size is 150-200nm to obtain the filler.
Preparation example 5: the difference between the preparation example and the preparation example 4 is that:
0.1kg of the ethylcellulose solution prepared in preparation example 3 was weighed out and sprayed onto the surface of 1kg of the supported bentonite prepared in preparation example 2.
Preparation example 6: the difference between the preparation example and the preparation example 4 is that:
0.35kg of the ethylcellulose solution prepared in preparation example 3 was weighed out and sprayed onto the surface of 1kg of the supported bentonite prepared in preparation example 2.
Preparation example 7: the difference between the preparation example and the preparation example 4 is that:
in the spraying process, the load bentonite is stirred at the rotating speed of 250r/min, the spraying speed of the ethyl cellulose solution is 2g/s, and after the spraying is finished, the load bentonite is dried at room temperature and then ground to the particle size of 150-200nm to prepare the filler.
Preparation example 8: the difference between the preparation example and the preparation example 4 is that:
in the spraying process, the load bentonite is stirred at the rotating speed of 500r/min, the spraying speed of the ethyl cellulose solution is 6g/s, and after the spraying is finished, the load bentonite is dried at room temperature and then ground to the particle size of 150-200nm to prepare the filler.
Examples
Polylactic acid among the following raw materials was purchased from PLA raw material, No. 4032D, manufactured by NatureWorks, usa.
Example 1: a corn fiber:
62kg of polylactic acid, 28kg of modified bamboo powder prepared in preparation example 1 and 5kg of filler prepared in preparation example 4;
the preparation method comprises the following steps:
s1, weighing polylactic acid, modified bamboo powder and filler, placing the materials in a mixer, and mixing and stirring the materials for 15min at the rotating speed of 1500r/min to obtain a mixture;
s2, placing the mixture in a double-screw extruder, performing melt extrusion, and performing vacuum drying to obtain polylactic acid particles;
and S3, putting the polylactic acid particles on a melt spinning machine for spinning, and carrying out melt spinning at the spinning temperature of 240 ℃, the winding speed of 1750m/min, the traction temperature of 70 ℃ and the traction multiple of 3.0 times to obtain the corn fiber.
Example 2: the present embodiment is different from embodiment 1 in that:
45kg of polylactic acid, 20kg of modified bamboo powder prepared in preparation example 1, and 3kg of filler prepared in preparation example 4.
Example 3: the present embodiment is different from embodiment 1 in that:
75kg of polylactic acid, 35kg of modified bamboo powder prepared in preparation example 1, and 8kg of filler prepared in preparation example 4.
Example 4: the present embodiment is different from embodiment 1 in that:
s3, putting the polylactic acid particles on a melt spinning machine for spinning, and carrying out melt spinning at the spinning temperature of 225 ℃, the winding speed of 1600m/min, the traction temperature of 65 ℃ and the traction multiple of 2.8 times to obtain the corn fiber.
Example 5: the present embodiment is different from embodiment 1 in that:
s3, putting the polylactic acid particles on a melt spinning machine for spinning, and carrying out melt spinning at the spinning temperature of 255 ℃, the winding speed of 1850m/min, the traction temperature of 80 ℃ and the traction multiple of 3.2 times to obtain the corn fiber.
Example 6: the present embodiment is different from embodiment 1 in that:
the filler was the filler prepared in preparation example 5.
Example 7: the present embodiment is different from embodiment 1 in that:
the filler prepared in preparation example 6 was used as the filler.
Example 8: the present embodiment is different from embodiment 1 in that:
the filler prepared in preparation example 7 was used as the filler.
Example 9: the present embodiment is different from embodiment 1 in that:
the filler prepared in preparation example 8 was used as the filler.
Example 10: the present embodiment is different from embodiment 1 in that:
the modified bamboo powder is prepared by the following method: grinding the commercially available bamboo powder to 100-150nm, and drying at 50 ℃ for 3h to obtain the modified bamboo powder.
Example 11: the present embodiment is different from embodiment 1 in that:
the bentonite with the same mass is used for replacing the load bentonite in the filler raw material.
Example 12: the present embodiment is different from embodiment 1 in that:
the filler is load bentonite.
Example 13: the present embodiment is different from embodiment 1 in that:
the ethyl cellulose solution is replaced by sodium carboxymethyl cellulose aqueous solution with the same mass in the filler raw materials, and the sodium carboxymethyl cellulose aqueous solution is prepared by the following method: 3kg of sodium carboxymethylcellulose is weighed and placed in 97kg of water to be stirred and dissolved, and the sodium carboxymethylcellulose aqueous solution is prepared.
Example 14: the present embodiment is different from embodiment 1 in that:
in the preparation process of the filler, the ethyl cellulose solution is added into the load bentonite at one time, stirred for 63s at the rotating speed of 350r/min, then dried at room temperature and ground to the particle size of 150-200nm to prepare the filler.
Application example: a fabric is prepared by the following steps:
the corn fibers obtained in examples 1 to 14 were respectively blended and woven by a textile machine.
Comparative example
Comparative example 1: this comparative example differs from example 1 in that:
the filler is replaced by polylactic acid with the same mass in the raw materials.
Comparative example 2: this comparative example differs from example 1 in that:
the modified bamboo powder with the same quality is used for replacing the filler in the raw materials.
Comparative example 3: this comparative example differs from example 1 in that:
the raw materials are modified bamboo powder replaced by polylactic acid with the same mass.
Comparative example 4: this comparative example differs from example 1 in that:
the modified bamboo powder and the filler are replaced by polylactic acid with the same mass in the raw materials.
Comparative example 5: the comparative example differs from example 1 in that:
corn fiber was purchased from corn fiber silk manufactured by sumatrine group limited.
Performance test
The preparation methods of examples 1 to 14 and comparative examples 1 to 5 are respectively adopted to prepare the corn fiber, and the length of the corn fiber is 250 mm; screening natural soil with particle diameter less than 2mm, wherein the natural soil has pH of 6.75, gray scale of 67.32%, humidity of 60.73%, contains saprophytic bacteria, such as fungi, bacteria, and actinomycetes, and has bacteria number of 1.2 × 10 7 CFU/g, number of fungi 9.1X 10 4 CFU/g, actinomycete count 1.3X 10 5 CFU/g, wherein the content of penicillium in the fungus is 32CFU/g, saprophytic bacteria are uniformly dispersed in the screened natural soil, and then the natural soil is divided into 19 parts respectively, wherein the 19 parts of the natural soil respectively correspond to the corn fibers prepared in the examples 1-14 and the comparative examples 1-5.
In examples 1 to 14 and comparative examples 1 to 5, 500g of polypropylene cellulose is weighed, agglomerated into a dough, and then balanced for 24 hours under the condition of standard atmospheric pressure to serve as a sample; the samples prepared in examples 1 to 14 and comparative examples 1 to 5 were placed in 19 parts of 8kg of soil, and the samples were completely covered with the soil to prepare samples to be tested.
1. Degradation rate test
When the sample is buried for 1 month, 6 months and 12 months, removing the sample, removing the soil with viscosity on the surface of the sample by using a brush, wiping the surface of the sample by using absolute ethyl alcohol, further removing impurities, drying the sample for 24 hours in a vacuum drying oven at the temperature of 50 ℃, measuring the mass of the degraded sample by using an electronic balance (the electronic balance is accurate to 0.0001g), and calculating the degradation rate;
degradation rate (m) 1 -m 2 )/m 1 ×100％；
Wherein: m is 1 For the pre-degradation sample mass, m 2 The quality of the degraded sample.
2. Fungal content test
After 1 month and 6 months respectively, the test sample is subjected to GB/T14643.4-2009 soil fungus determination and a plate counting method to detect the content of the fungi in the soil, wherein the test sample is prepared by the following method: screening soil, weighing 25g of soil sample, placing the soil sample in 225ml of physiological saline, stirring and mixing to prepare a diluent, then weighing 5ml of the diluent, placing the diluent in 45ml of sterile physiological saline, continuously mixing and stirring until the diluent, weighing 5g of soil, placing the soil in sterile physiological saline for dilution, diluting until the number of bacterial colonies in a culture dish is less than 300, pouring the diluent into a flat culture dish, culturing for 7 days at 25 ℃, calculating the fungal content in 1g of soil, wherein the dilution multiples of the samples to be tested prepared in examples 1-14 and comparative examples 1-5 are the same.
TABLE 1 test chart of natural degradation property
By combining the example 1 and the examples 2-5 and combining the table 1, the corn fiber prepared by the method has high natural degradation rate in soil, the degradation rate is as high as 95.5% when the corn fiber is naturally degraded in the soil for 12 months, and the fungal content is increased at 1 month and 6 months respectively; the polylactic acid, the modified bamboo powder and the filler are matched, and along with the degradation of the modified bamboo powder, energy substances are provided for fungus thalli, so that the growth and the propagation of the thalli are promoted; the natural degradation time of the corn fiber in the soil is shortened by utilizing the combination of microbial degradation and hydrolytic degradation, thereby shortening the natural degradation time of the corn fiber.
Combining example 1 and examples 6-9 with Table 1, it can be seen that examples 6-7 have different ratios of filler raw materials and examples 8-9 have different methods of making the filler than example 1, indicating that the ratios of the raw materials and methods of making the filler have an effect on the rate of natural degradation of the finished corn fiber in soil.
As can be seen by combining example 1 and examples 10-14 with table 1, the degradation rate of the corn fiber prepared in example 10 was less than that of the corn fiber prepared in example 1 in the corresponding month regardless of 1 month, 6 months, or 12 months, and the fungus number was less than that of example 1 in the corresponding month regardless of 1 month or 6 months, compared to example 1, without the citric acid modification treatment of the bamboo powder in the raw material of example 10; the method is characterized in that the bamboo powder is modified by citric acid, so that the citric acid is loaded on the surface of the bamboo powder, and is gradually released along with the degradation of the modified bamboo powder by microorganisms, the citric acid can promote the growth and the propagation of fungi in soil, and the fungi in the soil have a good degradation effect on the corn fiber, so that the natural degradation time of the corn fiber in the soil is shortened.
Example 11 replacement of the loaded bentonite with an equivalent mass of bentonite in the filler feedstock, compared to example 1, the degradation rate of the corn fiber produced in example 11 was less than the degradation rate of the corn fiber produced in example 1 in the corresponding month, whether degraded for 1 month, 6 months, or 12 months, and the fungal population was less than the fungal population of example 1 in the corresponding month, whether degraded for 1 month or 6 months; the tartaric acid loaded in the bentonite plays a role in promoting the growth and the propagation of fungi, and the good degradation effect of the fungi in the soil on the corn fiber is utilized, so that the natural degradation time of the corn fiber in the soil is shortened.
Example 12 the filler was bentonite loaded, and compared to example 1, the degradation rate of the corn fiber produced in example 12 was less than the degradation rate of the corn fiber produced in example 1 in the corresponding month, whether degraded for 1 month, 6 months, or 12 months, and the number of fungi was less than the number of fungi in example 1 in the corresponding month, whether degraded for 1 month or 6 months; the loaded bentonite which is not coated by the ethyl cellulose is shown in the specification, the tartaric acid in pores of the loaded bentonite is easy to separate from the pores, and thus the natural degradation speed of the corn fiber in the soil is easily influenced.
Example 13 in which an ethyl cellulose solution was replaced with an equal mass of an aqueous solution of sodium carboxymethyl cellulose in the starting material, compared to example 1, the degradation rate of the corn fiber prepared in example 13 was less than that of the corn fiber prepared in example 1 in the corresponding month regardless of 1 month, 6 months, or 12 months, and the fungal population was less than that of example 1 in the corresponding month regardless of 1 month or 6 months; the water-soluble sodium carboxymethylcellulose water solution has an influence on tartaric acid in the pores of the bentonite, so that the natural degradation speed of the corn fiber in the soil is easily influenced.
Example 14 filler during the preparation, ethyl cellulose solution was added to the loaded bentonite clay at once, and compared to example 1, the degradation rate of corn fiber prepared in example 14 was less than that of corn fiber prepared in example 1 in the corresponding month, whether degraded for 1 month, 6 months, or 12 months, and the fungus number was less than that of example 1 in the corresponding month, whether degraded for 1 month or 6 months; the ethyl cellulose solution is uniformly coated on the surface of the loaded bentonite, so that the coating uniformity of the surface of the loaded bentonite is further improved, and the natural degradation rate of the corn fiber in the soil is improved.
Combining example 1 and comparative examples 1-5 and table 1, it can be seen that, replacing the filler with polylactic acid of the same quality in the raw material of comparative example 1, replacing the filler with modified bamboo powder of the same quality in the raw material of comparative example 2, replacing the modified bamboo powder with polylactic acid of the same quality in the raw material of comparative example 3, replacing the modified bamboo powder and the filler with polylactic acid of the same quality in the raw material of comparative example 4, compared to example 1, the degradation rate of the corn fiber prepared in comparative examples 1, 2, 3, 4 is less than that of the corn fiber prepared in example 1 in the corresponding month no matter the corn fiber is degraded for 1 month, 6 months, or 12 months, and the fungus number is less than that of example 1 in the corresponding month no matter the corn fiber is degraded for 1 month or 6 months; the polylactic acid, the modified bamboo powder, the loaded bentonite and the ethyl cellulose solution are matched, the saprophytic bacteria firstly degrade the ethyl cellulose on the surface of the filler, then the tartaric acid in the bentonite is gradually contacted with the saprophytic bacteria in the soil, and the growth and propagation speed of the saprophytic bacteria can be accelerated by virtue of the acid groups of the tartaric acid, so that the natural degradation speed of the corn fiber in the soil is accelerated.
Compared with the corn fiber prepared in the example 1, the corn fiber prepared in the comparative example 5 is degraded for 1 month, 6 months or 12 months, the degradation rate of the corn fiber prepared in the comparative example 5 is smaller than that of the corn fiber prepared in the example 1 corresponding to the month, and the fungus quantity is smaller than that of the example 1 corresponding to the month in 1 month or 6 months; the corn fiber prepared by the method has high degradation rate and good natural degradation speed in soil.
3. Compost degradation test
The corn fibres were prepared using the preparation methods of examples 1 to 14 and comparative examples 1 to 5, respectively, with reference to the determination of the final aerobic biological decomposition capacity of the material under controlled composting conditions of GB/T19277.1-2011, using the method of determining the carbon dioxide released, part one: the general method comprises the steps of respectively detecting the biological decomposition rate of the compost after 165 days of degradation and recording data; in examples 1-14 and comparative examples 1-5, only the corn fiber material was different during the testing process, and the other parameters were the same.
4. Breaking Strength test
The preparation methods of examples 1 to 3 were respectively used to prepare corn fibers, referring to the first part of the tensile properties of GB/T3923.1-2013 textile fabrics: and (4) measuring the breaking strength and the breaking elongation, detecting the radial breaking strength of the corn fiber, and recording data.
5. Bacteriostasis rate test
The preparation methods of examples 1-3 and comparative examples 1-5 are respectively adopted to prepare the corn fiber, and reference is made to the third part of the evaluation of the antibacterial performance of the textile in GB/T20944.3-2008: an oscillation method; respectively detecting the bacteriostasis rates of the prepared corn fibers to staphylococcus aureus, escherichia coli and candida albicans, and recording data, wherein the staphylococcus aureus is marked as bacterium A, the escherichia coli is marked as bacterium B, and the candida albicans is marked as bacterium C; wherein the samples are: 0.75 g. + -. 0.05g of corn fibres, cut into pieces 5mm in length.
TABLE 2 other Performance test tables
By combining the example 1 and the examples 2-5 and combining the table 2, it can be seen that different raw material ratios and different preparation methods in the corn fiber preparation process have influences on the degradation rate of the finished corn fiber compost, the breaking strength of the finished corn fiber and the bacteriostasis rate; the corn fiber prepared by matching polylactic acid, modified bamboo powder and filler has better biodegradation rate in 165 days, so that the finished corn fiber has the advantage of short degradation time.
Combining example 1 with examples 6-9 and table 2, it can be seen that the filler ratios of examples 6-7 were different, examples 8-9 were different in the filler preparation process, and the corn fibers prepared in examples 6-9 had similar biodegradability rates as example 1 compared to example 1, indicating that different filler ratios and filler speeds have an effect on the biodegradability rate of the finished corn fiber.
Combining example 1 with examples 10-14 and table 2, it can be seen that the modified bamboo powder in the raw material of example 10 is not modified with citric acid, compared to example 1, the corn fiber prepared in example 10 has a lower biodegradability at 165 days than example 1; the citric acid loaded on the surface of the modified bamboo powder promotes the growth and the propagation of saprophytic bacteria, the fungi in the saprophytic bacteria play a main role in the degradation of the corn fiber, and the citric acid can promote the growth and the propagation of the fungi, so that the degradation of the corn fiber is promoted, and the degradation time of the corn fiber compost is shortened.
Example 11 the bentonite loaded was replaced with an equivalent mass of bentonite in the feedstock, and compared to example 1, the corn fiber produced in example 11 had a shorter biodegradation rate in 165 days than in example 1; the tartaric acid in the bentonite can accelerate the growth and reproduction speed of the saprophytic bacteria, thereby accelerating the compost degradation speed of the corn fiber.
Example 12 the corn fiber prepared in example 12 had a lower biodegradability than example 1 in 165 days compared to example 1 without the addition of an ethylcellulose solution to the filler; the better film forming effect of the ethyl cellulose is proved to obstruct the tartaric acid in the loaded bentonite, when the corn fiber is degraded, the tartaric acid is released from the gaps of the bentonite along with the degradation of the ethyl cellulose, and the composting degradation time of the corn fiber is shortened by utilizing the characteristic that the tartaric acid promotes the growth and the reproduction of the saprophytic bacteria thallus.
Example 13 replacing the ethylcellulose solution with an equal mass of aqueous sodium carboxymethylcellulose solution in the filler feedstock, the corn fiber prepared in example 13 had a lower biodegradability rate over 165 days than in example 1; the method is characterized in that the tartaric acid aqueous solution is conveniently blocked in the pores of the bentonite by utilizing the water-insoluble function of the ethyl cellulose, and if the caking property and the film forming effect are simply considered and the water-soluble cellulose is selected, the tartaric acid in the pores of the bentonite is easily dissolved, so that the degradation of the corn fiber is influenced.
Example 14 filler during the preparation, ethyl cellulose solution was added to the loaded bentonite clay in one portion, and compared to example 1, the corn fiber prepared in example 14 had a less than example 1 biodegradation rate in 165 days; the one-time addition is proved, so that the ethyl cellulose solution is not easy to uniformly coat the surface of the loaded bentonite, the tartaric acid loading condition in the pores of the loaded bentonite is easily influenced, and the degradation speed of the corn fiber is influenced.
Combining example 1 and comparative examples 1-5 and table 2, it can be seen that, replacing the filler with polylactic acid of the same mass in the raw material of comparative example 1, replacing the filler with modified bamboo powder of the same mass in the raw material of comparative example 2, replacing the modified bamboo powder with polylactic acid of the same mass in the raw material of comparative example 3, and replacing the modified bamboo powder and the filler with polylactic acid of the same mass in the raw material of comparative example 4, compared with example 1, the corn fiber prepared in comparative examples 1, 2, 3 and 4 has a shorter biodegradation rate in 165 days than example 1, and has a lower bacteriostatic rate on staphylococcus aureus, escherichia coli and candida albicans than example 1; the matching of the polylactic acid, the modified bamboo powder and the filler is illustrated, in the degradation process, the modified bamboo powder is degraded firstly, so that polylactic acid molecules in the corn fiber and the filler are in contact with soil, the contact area of saprophytic bacteria and the polylactic acid is increased, meanwhile, the filler is utilized to promote the growth and the propagation of saprophytic bacteria, promote the degradation of the corn fiber and shorten the degradation time of the corn fiber.
The corn fiber of comparative example 5 is a commercial corn fiber, and compared to example 1, the corn fiber prepared in comparative example 1 has a less biodegradation rate at 165 days than example 1; the degradation rate of the commercially available corn fiber is lower than that of the corn fiber prepared by the method, and the degradation time of the corn fiber prepared by the method is shorter.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (6)
1. The corn fiber is characterized by being prepared from the following raw materials in parts by weight: 45-75 parts of polylactic acid, 20-35 parts of modified bamboo powder and 3-8 parts of filler; the modified bamboo powder is prepared by the following method;
pretreating the dried bamboo powder by using a mixed solution of sodium hydroxide and hydrogen peroxide, and then carrying out esterification modification treatment on the bamboo powder by using citric acid;
the filler is prepared from a load bentonite and an ethyl cellulose solution with the weight ratio of 1: 0.1-0.35;
the load bentonite is prepared by the following method:
weighing tartaric acid, placing in water, stirring and dissolving to obtain a stirring solution; then placing bentonite into the stirring liquid, oscillating, ultrasonically dispersing, standing, filtering to take out the bentonite, and draining the surface water to obtain the load bentonite;
the filler is prepared by the following method: and spraying the ethyl cellulose solution on the surface of the loaded bentonite, drying, and grinding to obtain the filler.
2. The corn fiber as claimed in claim 1, wherein the ethyl cellulose solution is prepared by the following method: weighing ethyl cellulose, placing the ethyl cellulose in ethanol, stirring and dissolving to obtain an ethyl cellulose solution.
3. The corn fiber as claimed in claim 1, wherein the bentonite is stirred at a speed of 500r/min and the ethyl cellulose solution is sprayed at a speed of 2-6g/s during the spraying process.
4. A method of producing corn fiber as claimed in any one of claims 1 to 3, comprising the steps of:
s1, weighing polylactic acid, modified bamboo powder and filler, mixing, and stirring to obtain a mixture;
s2, melting and extruding the mixture, and then drying in vacuum to obtain polylactic acid particles;
and S3, carrying out melt spinning on the polylactic acid particles to obtain the corn fiber.
5. The method as claimed in claim 4, wherein the melt spinning temperature is 225-255 ℃, the winding speed is 1600-1850m/min, the drawing temperature is 65-80 ℃, and the drawing ratio is 2.8-3.2.
6. A fabric made from a composition comprising the corn fiber of any one of claims 1 to 3 or made by the method of making the corn fiber of any one of claims 4 to 5.
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