CN113786819A - Waste cotton fabric modified microfiber and preparation method and application thereof - Google Patents
Waste cotton fabric modified microfiber and preparation method and application thereof Download PDFInfo
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 88
- 239000002699 waste material Substances 0.000 title claims abstract description 87
- 239000004744 fabric Substances 0.000 title claims abstract description 78
- 229920001410 Microfiber Polymers 0.000 title claims abstract description 70
- 239000003658 microfiber Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 22
- 239000000835 fiber Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000011343 solid material Substances 0.000 claims abstract description 13
- 238000000265 homogenisation Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000000967 suction filtration Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 230000004048 modification Effects 0.000 claims description 13
- 238000012986 modification Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000003463 adsorbent Substances 0.000 claims description 2
- 238000004043 dyeing Methods 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 16
- 238000001179 sorption measurement Methods 0.000 abstract description 15
- 239000000975 dye Substances 0.000 abstract description 9
- 125000003277 amino group Chemical group 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 229910001948 sodium oxide Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 239000004753 textile Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 229920000433 Lyocell Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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- 239000006227 byproduct Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明属于吸附材料技术领域，具体涉及一种废旧棉织物改性微纤及其制备方法和应用，包括以下步骤：1)制备得到废旧棉织物纤维粉；2)将废旧棉织物纤维粉与氢氧化钠溶液混合后进行碱处理，抽滤洗涤后得到碱处理的废旧棉织物纤维；3)将碱处理后的废旧棉织物纤维与去离子水混合后进行高速匀浆，得到废旧棉织物微纤悬浮液；4)将废旧棉织物微纤悬浮液先用聚乙烯亚胺处理和戊二醛处理，进行固液分离，再将所得固体物料经去离子水洗涤后冷冻干燥，得到改性废旧棉织物微纤。该方法以废旧棉织物为原料，利用聚乙烯亚胺和戊二醛对微纤进行改性，使其表面裸露出大量的胺基，对染料具有较强的吸附能力。
The invention belongs to the technical field of adsorption materials, and in particular relates to a waste cotton fabric modified microfiber and a preparation method and application thereof, comprising the following steps: 1) preparing waste cotton fabric fiber powder; 2) mixing waste cotton fabric fiber powder with hydrogen Alkali treatment is carried out after the sodium oxide solution is mixed, and the waste cotton fabric fibers of the alkali treatment are obtained after suction filtration and washing; 3) the waste cotton fabric fibers after the alkali treatment are mixed with deionized water and then subjected to high-speed homogenization to obtain waste cotton fabric microfibers 4) The waste cotton fabric microfiber suspension is first treated with polyethyleneimine and glutaraldehyde to carry out solid-liquid separation, and then the obtained solid material is washed with deionized water and then freeze-dried to obtain modified waste cotton Fabric Microfiber. The method uses waste cotton fabrics as raw materials, and uses polyethyleneimine and glutaraldehyde to modify the microfibers, so that a large number of amine groups are exposed on the surface, and the microfibers have strong adsorption capacity for dyes.
Description
Technical Field
The invention belongs to the technical field of adsorption materials, and particularly relates to a waste cotton fabric modified microfiber and a preparation method and application thereof.
Background
With the continuous improvement of living standard and the development of textile industry, people pay more attention to chasing up the trend, so that the service cycle of the textile is shortened, and the quantity of the waste textile is continuously increased. About 2000 million tons of waste textiles are produced in the production and consumption links every year in China, but the comprehensive utilization rate is only about 15%. Most of the waste textiles are incinerated and buried, which not only wastes resources, but also causes a heavy burden on the environment.
At present, the most researches on recycling waste cotton textiles are to produce regenerated cellulose fibers. The traditional method is to dissolve the mixture into dilute alkali solution to prepare spinning solution after the procedures of alkalization, ageing, yellowing and the like by a chemical process, and the spinning solution is prepared by wet spinning, but the method can generate byproducts with high toxicity. The traditional method is replaced by a solvent method for producing Lyocell fibers at present, the chemical raw materials used in the method are nontoxic, but ionic liquid is high in cost and viscosity, and certain difficulty is caused to the production process.
Therefore, the research and development of a novel efficient, low-cost, environment-friendly and reusable waste textile recycling process has very important practical significance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a waste cotton fabric modified microfiber and a preparation method and application thereof. The raw materials of the method provided by the invention are derived from waste cotton fabrics, the resources are rich, and the waste utilization is realized. The method has the advantages of simple process, environmental protection and low production cost.
The technical scheme provided by the invention is as follows:
a preparation method of waste cotton fabric modified microfiber comprises the following steps:
1) crushing the waste pure cotton fabric dried to constant weight into chips, and crushing the chips into powder by using a crusher to obtain waste cotton fabric fiber powder;
2) mixing the waste cotton fabric fiber powder obtained in the step 1) with a sodium hydroxide solution, performing alkali treatment, and performing suction filtration and washing to obtain alkali-treated waste cotton fabric fibers;
3) mixing the alkali-treated waste cotton fabric fibers obtained in the step 2) with deionized water, and then performing high-speed homogenization to obtain waste cotton fabric microfiber suspension;
4) treating the waste cotton fabric microfiber suspension obtained in the step 3) with polyethyleneimine, cooling to room temperature, then treating with glutaraldehyde, performing solid-liquid separation on the obtained system to obtain a solid material, washing the solid material with deionized water, and then performing freeze drying to obtain the waste cotton fabric modified microfiber.
In the above technical scheme:
stripping the waste cotton fabric fiber powder into waste cotton fabric fibers with smaller sizes through the alkali treatment in the step 2). Furthermore, the waste cotton fabric fibers are homogenized at a high speed through high-speed homogenization to obtain a waste cotton fabric microfiber suspension, wherein the microfibers have a loose net structure and the specific surface area is remarkably improved, so that more amino groups can be exposed on the surface of the modified waste cotton fabric fibers, and the modified waste cotton fabric microfiber suspension has a better dye adsorption effect.
In the modification process of the step 4), interchain crosslinking is formed between polyethyleneimine and cotton fiber molecules through hydrogen bonds. After being added, glutaraldehyde reacts with polyethyleneimine and cotton fibers to generate chemical bonds respectively, and reacts with-OH groups of the cotton fibers to remove water molecules, and meanwhile, glutaraldehyde and polyethyleneimine molecules are crosslinked together through generating C ═ N double bonds. The surface of the cotton fiber is modified by polyethyleneimine through the bridging action of glutaraldehyde molecules, and the cotton fiber is rich in chargedGroup (-NH)2). The principle is as follows:
specifically, in the step 1), the particle size of the waste cotton fabric fiber powder is 0.05-0.2 mm.
Specifically, in the step 2):
the concentration of the sodium hydroxide solution is 5-8 wt.%, and the dosage ratio of the solid material to the sodium hydroxide solution in the system during alkali treatment is 1g: 20-30 mL;
the temperature of the alkali treatment is 80-100 ℃, the time of the alkali treatment is 2-4 h, the stirring speed during the alkali treatment is 150-350 rpm, and the filtrate is washed after suction filtration until the pH value of the filtrate is 7-8.
Specifically, in the step 3), the number of times of medium-high speed homogenization treatment is 8-10.
Specifically, the method comprises the following steps:
the solid content of the system is 2-3 wt% during high-speed homogenization treatment;
the rotating speed of the high-speed homogenizing treatment is 15000-20000 rpm, and the time of single high-speed homogenizing treatment is 5-8 min.
Specifically, in the step 4):
the concentration of the polyethyleneimine solution is 1-1.5 wt.%, the dosage ratio of the solid material to the polyethyleneimine solution in the polyethyleneimine modification system is 1g (3-5) mL, the treatment time is 4-6 h, the treatment temperature is 45-55 ℃, and the stirring speed is 150-350 rpm;
the dosage ratio of the solid material to the glutaraldehyde in the glutaraldehyde treatment system is 1g (0.3-0.5) mL, the treatment time is 1.5-2.5 h, and the stirring speed is 150-350 rpm;
washing for 3-5 times by using deionized water after solid-liquid separation, wherein the using amount ratio of the deionized water to the solid material is (80-100) mL:1 g;
the temperature of the freeze drying is-50 ℃ to-60 ℃, and the freezing time is 36-48 h.
The invention also provides the waste cotton fabric modified microfiber prepared by the preparation method.
The modified microfiber based on waste cotton fabric provided by the invention has a large specific surface area and a loose reticular structure, and a large amount of amino groups are arranged on the fiber surface, so that the modified microfiber has strong adsorption capacity on dyes.
The invention also provides the modified microfiber based on the waste cotton fabric as an adsorbent for treating printing and dyeing wastewater.
The invention has the advantages that:
1) the high-speed homogenate is used for replacing the traditional acid hydrolysis, so that the problem of environmental pollution caused by the traditional chemical treatment is greatly relieved;
2) the high-speed homogenate can enable the fibers to be stripped into microfibrillated cellulose with a loose net-shaped structure, so that the specific surface area of the microfibrillated cellulose is greatly increased;
3) polyethyleneimine and glutaraldehyde are used for modifying waste cotton fabric microfiber, and the surface of the microfiber has a large number of amino groups, so that the microfiber has strong adsorption capacity on dyes.
4) The invention has simple production process, high efficiency and low production cost.
Drawings
FIG. 1 shows a waste cotton fabric microfiber suspension liquid after high-speed homogenization.
FIG. 2 shows a freeze-dried sample of waste cotton fabric modified microfiber.
FIG. 3 is SEM test chart of waste cotton fabric modified microfiber.
FIG. 4 FTIR spectra of waste cotton fabric microfibers before and after modification (CE is the microfibers before modification; PEI @ CE is the modified microfibers).
FIG. 5 shows thermogravimetric analysis results of waste cotton fabric micro-fibers before and after modification (CE is micro-fiber before modification; PEI @ CE is modified micro-fiber).
FIG. 6 shows pictures before and after the waste cotton fabric modified microfiber adsorbs the methyl blue solution.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
The waste cotton fabric modified microfiber can be obtained according to the following method:
10g of waste white pure cotton T-shirt is taken and dried in an oven at 60 ℃ to constant weight. Cutting into pieces with scissors, and pulverizing into powder with particle size of 0.05-0.2mm with pulverizer. And (3) mixing fiber powder according to the solid-liquid ratio of 1: 20 was added to a 7% aqueous solution of NaOH. Stirring at 80 deg.C for 2 hr, vacuum filtering, and washing the filter residue with deionized water until the pH of the filtrate is neutral. Taking the cotton fiber treated by the alkali, preparing a 2 wt% cellulose suspension by water, homogenizing at a high speed (15000rpm) for 5min, and circularly homogenizing for 10 times to obtain a waste cotton fabric microfiber suspension (see figure 1). To this suspension was added dropwise 30mL of a 1 wt% polyethyleneimine solution, and the mixture was stirred (rotation speed: 350rpm) at 55 ℃ for 4 hours. After naturally cooling to room temperature, 5mL of glutaraldehyde was added and stirred (rotation speed 350rpm) for 1.5 hours. After the reaction was complete, it was filtered and the filter residue was washed 3 times with water. And (3) freeze-drying the washed sample (drying at the temperature of-50 ℃ for 48 hours) to obtain the waste cotton fabric modified microfiber product (see figure 2).
The SEM test result of the waste cotton fabric modified microfiber is shown in figure 3. As can be seen from fig. 3, after the waste cotton fabric is subjected to alkali treatment, high-speed homogenization and crosslinking treatment, the microfibers are peeled off, and a loose mesh structure is formed, and the surface of the waste cotton fabric is coated with a large amount of polyethyleneimine. FIG. 4 is an FTIR absorption spectrum of the waste cotton fabric microfiber before and after modification prepared in example 1, and it can be seen from FIG. 4 that the positions of peaks appeared in the microfiber before and after modification are substantially the same, but the microfiber after modification is 1650cm-1The obvious characteristic absorption peak of C ═ N proves that PEI is successfully crosslinked with cellulose. Fig. 5 shows thermogravimetric analysis results of the waste cotton fabric micro-fibers before and after modification, and it can be seen from fig. 5 that the maximum decomposition temperature of the modified waste cotton fabric micro-fibers is increased to 481 ℃ compared with that before modification, and the thermal stability of the modified waste cotton fabric micro-fibers is increased probably due to intermolecular cross-linking caused by glutaraldehyde.
Example 2
The waste cotton fabric modified microfiber can be obtained according to the following method:
10g of waste white pure cotton T-shirt is taken and dried in an oven at 60 ℃ to constant weight. Cutting into pieces with scissors, and pulverizing into powder with particle size of 0.05-0.2mm with pulverizer. And (3) mixing fiber powder according to the solid-liquid ratio of 1: 30, adding 5 percent NaOH aqueous solution, stirring (150rpm) at 100 ℃ for 4 hours, filtering, and fully washing filter residues with deionized water until the filtrate is neutral. Taking the cotton fiber treated by the alkali, preparing a 3 wt% cellulose suspension by water, homogenizing at a high speed (20000rpm) for 8min, and circularly homogenizing for 8 times to obtain the waste cotton fabric microfiber suspension. To this suspension was added dropwise 50mL of a 1.5 wt% Polyethyleneimine (PEI) solution and the mixture was stirred (rotation speed 350rpm) at 45 ℃ for 6 hours. After cooling to room temperature, 3mL of glutaraldehyde were added and stirred (350 rpm) for 2.5 h. Filter and wash the residue 5 times with water. And (4) freeze-drying the washed sample at (-60 ℃ for 36 hours) to obtain the waste cotton fabric modified microfiber product. The characterization results of the waste cotton fabric modified microfiber prepared in example 2 are similar to the sample prepared in example 1, and are all loose net structures.
Example 3
Adsorption of the waste cotton fabric modified microfiber on dye:
50mg of the waste cotton fabric modified microfiber prepared in example 1 was added to 100mL of a methyl blue solution with a concentration of 50mg/L, and the mixture was stirred and adsorbed at room temperature and 100rpm for 30min (see FIG. 5), and the dye removal rate was calculated to be 98.4%. Adding 50mg of waste cotton fabric modified microfiber into 100mL of methyl blue solution with the concentration of 150mg/L, stirring and adsorbing for 120min at room temperature and 100rpm, calculating the adsorption capacity to be 279.26mg/g, and soaking the microfiber after dye adsorption in 40mL of methanol solution containing 1N KSCN for analysis. After filtration, the filter residue is soaked in 60mL deionized water solution for 30 minutes, the filter residue is filtered to obtain the resolved microfiber, and the microfiber is added into 100mL methyl blue solution with the concentration of 150mg/L again to be adsorbed at room temperature for 120 min. The adsorption and analysis process was repeated 5 times, and the adsorption rate of the dye is shown in Table 1. The results show that the adsorption rate of the dye after 5 times of repetition is still as high as 84.6%.
TABLE 1 repeated adsorption rate of waste cotton fabric modified microfiber to methyl blue solution
The adsorption performance of the waste cotton fabric modified microfiber prepared in example 2 is tested according to the method, and the result shows that the adsorption capacity of the waste cotton fabric modified microfiber prepared in example 2 to a methyl blue solution of 150mg/L is 278.35 mg/g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A preparation method of waste cotton fabric modified microfiber is characterized by comprising the following steps:
1) crushing the waste pure cotton fabric dried to constant weight into chips, and crushing the chips into powder by using a crusher to obtain waste cotton fabric fiber powder;
2) mixing the waste cotton fabric fiber powder obtained in the step 1) with a sodium hydroxide solution, performing alkali treatment, and performing suction filtration and washing to obtain alkali-treated waste cotton fabric fibers;
3) mixing the alkali-treated waste cotton fabric fibers obtained in the step 2) with deionized water, and then performing high-speed homogenization to obtain waste cotton fabric microfiber suspension;
4) treating the waste cotton fabric microfiber suspension obtained in the step 3) with polyethyleneimine, cooling to room temperature, then treating with glutaraldehyde, performing solid-liquid separation on the obtained system to obtain a solid material, washing the solid material with deionized water, and then performing freeze drying to obtain the waste cotton fabric modified microfiber.
2. The preparation method of the waste cotton fabric modified microfiber according to claim 1, which is characterized in that: in the step 1), the particle size of the waste cotton fabric fiber powder is 0.05-0.2 mm.
3. The preparation method of the waste cotton fabric modified microfiber according to claim 1, wherein in the step 2):
the concentration of the sodium hydroxide solution is 5-8 wt.%, and the dosage ratio of the solid material to the sodium hydroxide solution in the system during alkali treatment is 1g (20-30) mL;
the temperature of the alkali treatment is 80-100 ℃, the time of the alkali treatment is 2-4 h, the stirring speed during the alkali treatment is 150-350 rpm, and the filtrate is washed to have the pH value of 7-8 after suction filtration.
4. The preparation method of the waste cotton fabric modified microfiber according to claim 1, which is characterized in that: and 3), performing medium-high speed homogenization treatment for 8-10 times.
5. The preparation method of the waste cotton fabric modified microfiber according to claim 4, wherein the preparation method comprises the following steps:
the solid content of the system is 2-3 wt% during high-speed homogenization treatment;
the rotating speed of the high-speed homogenizing treatment is 15000-20000 rpm, and the time of single high-speed homogenizing treatment is 5-8 min.
6. The preparation method of the waste cotton fabric modified microfiber according to claim 1, wherein in the step 4):
the concentration of the polyethyleneimine solution is 1-1.5 wt.%, the dosage ratio of the solid material to the polyethyleneimine solution in the polyethyleneimine modification system is 1g (3-5) mL, the treatment time is 4-6 h, the treatment temperature is 45-55 ℃, and the stirring speed is 150-350 rpm;
the dosage ratio of the solid material to the glutaraldehyde in the glutaraldehyde treatment system is 1g (0.3-0.5) mL, the treatment time is 1.5-2.5 h, and the stirring speed is 150-350 rpm;
washing for 3-5 times by using deionized water after solid-liquid separation, wherein the using amount ratio of the deionized water to the solid material is (80-100) mL:1 g;
the temperature of the freeze drying is-50 ℃ to-60 ℃, and the freezing time is 36-48 h.
7. A waste cotton fabric modified microfiber prepared by the preparation method according to any one of claims 1 to 6.
8. The application of the waste cotton fabric modified microfiber according to claim 7, wherein the waste cotton fabric modified microfiber comprises the following components in percentage by weight: used as an adsorbent for treating printing and dyeing wastewater.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114890564A (en) * | 2022-05-09 | 2022-08-12 | 广东前进牛仔布有限公司 | Recovery method of denim fabric desizing wastewater |
| CN114990935A (en) * | 2022-06-01 | 2022-09-02 | 齐鲁工业大学 | Method for preparing antibacterial waterproof packaging paper by using regenerated waste cotton fibers |
| CN115233471A (en) * | 2022-08-17 | 2022-10-25 | 武汉纺织大学 | Method for preparing colored dye by using waste cotton fabric |
| CN115350723A (en) * | 2022-08-17 | 2022-11-18 | 武汉纺织大学 | Waste cotton fabric superfine powder-TiO 2 Preparation method and application of composite photocatalytic material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105013447A (en) * | 2015-07-01 | 2015-11-04 | 南通大学 | Preparation method of modified cellulose heavy metal adsorbent |
| CN110746655A (en) * | 2019-10-28 | 2020-02-04 | 上海工程技术大学 | Cellulose nanowhisker-based pH-sensitive nanospheres and their preparation and application |
| CN110833820A (en) * | 2019-10-23 | 2020-02-25 | 浙江理工大学 | Preparation method of cellulose nanofiber-based reusable environment restoration material capable of adsorbing heavy metal ions and dyes |
| CN111576069A (en) * | 2020-04-26 | 2020-08-25 | 武汉纺织大学 | Ramie bone microfibrillated cellulose and preparation method and application thereof |
| CN113004571A (en) * | 2021-03-08 | 2021-06-22 | 池州学院 | Preparation method of waste fabric fiber aerogel |
-
2021
- 2021-09-27 CN CN202111134539.2A patent/CN113786819A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105013447A (en) * | 2015-07-01 | 2015-11-04 | 南通大学 | Preparation method of modified cellulose heavy metal adsorbent |
| CN110833820A (en) * | 2019-10-23 | 2020-02-25 | 浙江理工大学 | Preparation method of cellulose nanofiber-based reusable environment restoration material capable of adsorbing heavy metal ions and dyes |
| CN110746655A (en) * | 2019-10-28 | 2020-02-04 | 上海工程技术大学 | Cellulose nanowhisker-based pH-sensitive nanospheres and their preparation and application |
| CN111576069A (en) * | 2020-04-26 | 2020-08-25 | 武汉纺织大学 | Ramie bone microfibrillated cellulose and preparation method and application thereof |
| CN113004571A (en) * | 2021-03-08 | 2021-06-22 | 池州学院 | Preparation method of waste fabric fiber aerogel |
Non-Patent Citations (1)
| Title |
|---|
| YANHONG DING等: "Robust, sustainable, hierarchical multi-porous cellulose beads via pre-crosslinking strategy for efficient dye adsorption", 《CELLULOSE》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114890564A (en) * | 2022-05-09 | 2022-08-12 | 广东前进牛仔布有限公司 | Recovery method of denim fabric desizing wastewater |
| CN114990935A (en) * | 2022-06-01 | 2022-09-02 | 齐鲁工业大学 | Method for preparing antibacterial waterproof packaging paper by using regenerated waste cotton fibers |
| CN114990935B (en) * | 2022-06-01 | 2023-01-24 | 齐鲁工业大学 | Method for preparing antibacterial waterproof packaging paper by using regenerated waste cotton fibers |
| CN115233471A (en) * | 2022-08-17 | 2022-10-25 | 武汉纺织大学 | Method for preparing colored dye by using waste cotton fabric |
| CN115350723A (en) * | 2022-08-17 | 2022-11-18 | 武汉纺织大学 | Waste cotton fabric superfine powder-TiO 2 Preparation method and application of composite photocatalytic material |
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