CN110540187A - preparation method of clay/carbon aerogel material - Google Patents
preparation method of clay/carbon aerogel material Download PDFInfo
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- CN110540187A CN110540187A CN201910929596.6A CN201910929596A CN110540187A CN 110540187 A CN110540187 A CN 110540187A CN 201910929596 A CN201910929596 A CN 201910929596A CN 110540187 A CN110540187 A CN 110540187A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/28—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
- B01J20/28047—Gels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
The invention belongs to the field of resource utilization, relates to preparation of clay/carbon aerogel with an adsorption effect, and particularly relates to a method for preparing clay/carbon aerogel with an adsorption effect by using waste textiles. The preparation method comprises the following steps: firstly, washing and shearing waste textiles of natural fibers such as cotton, hemp, silk, wool and the like, and adding the fragments into water for mechanical homogenization treatment; then adding clay particles and a cross-linking agent, uniformly stirring, and freezing by using liquid nitrogen to form a frozen gel; obtaining aerogel after freeze drying; and finally, carrying out preoxidation and carbonization treatment on the aerogel to obtain the aerogel with an adsorption effect. On one hand, the clay/carbon aerogel prepared by the method can realize high-value utilization of waste textiles to a certain extent; on the other hand, the cross-linked carbon aerogel has certain mechanical strength, is not easy to break in the using process, is used as a new adsorption material, and has wide application prospect in the aspect of adsorbing harmful organic matters and heavy metals in wastewater so as to purify water.
Description
Technical Field
the invention mainly relates to the technical field of materials, in particular to a preparation method of a clay/carbon aerogel material, which is a high-value utilization fiber of waste textiles and can be used in the field of adsorption.
Background
In addition to the rapid development of the times, the world also faces serious problems such as resource shortage, environmental pollution and the like, wherein the quantity of waste textiles made of natural fibers such as cotton, hemp, silk, wool and the like generated every year attracts attention, and the total quantity of textiles such as clothes, home textiles and the like eliminated in daily life is continuously increased besides processing waste and defective goods in industrial production. At present, most of the treatment methods of the waste water are still in the stages of incineration, burial and the like, so that the waste of resources and the environmental pollution are greatly caused. Although textile enterprises in China achieve certain achievements in the recycling industry of waste textiles, the waste textiles have great defects in the aspect of high-efficiency recycling, so that the method has important significance in exploring high-value utilization of the waste textiles.
the printing and dyeing wastewater contains complex organic matters with azo bonds and polyaromatic rings and heavy metal ions, and after being discharged, the printing and dyeing wastewater has toxic action on plants, microorganisms and fishes in water, and even some toxic and difficultly-degradable organic dyes can cause harm to human health. There are many methods for treating printing and dyeing wastewater, and oxidation-reduction method, photocatalytic degradation method, ion exchange method, physical adsorption method, etc. are commonly used. The structure of dye molecules is generally stable and is difficult to degrade or oxidize, and some dyes can generate carcinogenic and toxic substances after degradation, so that the treatment of some printing and dyeing wastewater by common chemical or biochemical methods is difficult, while the treatment of dyes by adsorption methods has great advantages and is widely concerned by people. The commercial adsorbent active carbon commonly used in the industry at present has a highly developed internal pore structure, a higher specific surface area, excellent adsorption and decoloration performance and can adsorb various organic matters and metal ions in water. However, the activated carbon has the disadvantages of easy dispersion, loss, environmental pollution, complex filtering operation and the like. The carbon aerogel combines the unique structure of the aerogel and the excellent and stable physical characteristics of the carbon material, and has super strong adsorption performance. Although carbon aerogels have adsorptive properties and are not easily dispersed, most carbon aerogels have a poor skeletal stability in water.
In view of this, the invention is particularly proposed.
Disclosure of Invention
aiming at the defects in the existing method, the first purpose of the invention is to provide a porous aerogel material prepared by high-valued utilization of waste textiles such as cotton, hemp, silk and wool.
A second object of the present invention is to provide a clay/carbon aerogel material having an adsorption property and excellent skeleton stability in water.
In order to achieve the above object, the present invention provides a method for preparing clay/carbon aerogel, comprising the steps of:
(1) adding a detergent into waste textiles of natural fibers such as cotton, hemp, silk, wool and the like for cleaning; washing with water for the second time;
(2) placing the waste textile obtained in the step (1) in an oven, wherein the temperature of the oven is 60 ℃, drying and then cutting into pieces;
(3) adding the textile fragments obtained in the step (2) into water, and homogenizing the textile fragments to obtain a mixture containing fibers and water;
(4) Adding clay particles and a cross-linking agent into the mixture obtained in the step (3), adding phosphoric acid to adjust the pH value to 3-4 so as to provide an acid environment for cross-linking, stirring at high speed for 30-80min on a mechanical stirrer at the rotating speed of 1200rpm, and uniformly stirring to obtain a homogeneous suspension;
(5) freezing the suspension obtained in the step (4) in liquid nitrogen at-196 ℃ to obtain frozen gel;
(6) drying the frozen gel obtained in the step (5) in a freeze dryer at the temperature of minus 80 ℃ to minus 50 ℃ for 48-96 hours, and removing the solvent in the gel to form aerogel;
(7) placing the aerogel obtained in the step (6) in a tubular furnace, firstly heating to 150-; then raising the temperature to 600-1000 ℃ in the nitrogen atmosphere, preserving the heat for 4-6h for carbonization, and then slowly cooling to room temperature to obtain the clay/carbon aerogel.
The area of the fragments in the step (2) is 0.2-4cm 2.
the step (3) of adding the textile fragments into water means that one or more of cotton, hemp, silk and wool waste old textile fragments are added into water.
The mechanical treatment in the step (3) comprises any one of ultrasonic treatment and high-pressure homogenization treatment, wherein the ultrasonic treatment is an ultrasonic cell crusher, and the ultrasonic power is 800-; the ultrasonic treatment time is 60-150 min; the high-pressure homogenizing treatment is a high-pressure homogenizer with the pressure of 500-800 bar.
the mass fraction of the fibers in the mixture containing the fibers and the water in the step (3) is 1040%.
The length range of the fiber in the step (3) is 0.5-3 mm.
And (4) the clay particles in the step (4) are one of montmorillonite, sepiolite, kaolinite, talcum powder and saponite.
the mass fraction of the clay particles in the step (4) is 1-15%.
The cross-linking agent in the step (4) is one or more of glutaraldehyde, divinyl sulfone, diisocyanate, methylol melamine resin, melamine-formaldehyde resin, boric acid and borate.
The mass fraction of the cross-linking agent in the step (4) is 1-10%.
has the advantages that:
(1) the method recycles the fibers in the waste cotton, hemp, silk and wool textiles to prepare the aerogel, effectively reduces the environmental pollution caused by burning the waste textiles, and realizes the high-value utilization of the waste textiles.
(2) the inorganic clay particles added in the invention have wide sources and low price, and have good performances of adsorption, ion exchange and the like. Phosphorus is one of the nutrients for algal plant growth. After the phosphorus-containing wastewater seriously pollutes water sources, the phosphorus content of rivers and lakes can be increased, algae grow crazy and generate a 'red tide' phenomenon, so that the eutrophication of water, the water quality deterioration and turbidity and the aquatic organisms are difficult to survive. The inorganic clay particles can not only improve the stability of the carbon aerogel skeleton, but also adsorb phosphorus-containing substances in water.
(3) Glutaraldehyde, divinyl sulfone, diisocyanate, hydroxymethyl melamine resin, melamine-formaldehyde resin, boric acid and borate in the cross-linking agent used in the invention are used as cross-linking agents containing carbon, sulfur, nitrogen and boron elements for cross-linking fiber aerogel, the carbon aerogel with a cross-linking network can be obtained after carbonization, the mechanical property of the aerogel can be improved, the cross-linking agent containing sulfur, nitrogen or boron elements can play a role in doping, and the adsorption property of the aerogel can be improved.
Drawings
FIG. 1 SEM image of clay/carbon aerogel prepared by waste textiles according to the present invention
The specific implementation mode is as follows:
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
A preparation method of clay/carbon aerogel is characterized by comprising the following steps:
(1) adding 10g of cotton waste textiles into a detergent for cleaning; then washing for the second time by using an aqueous solution;
(2) Drying the waste textiles obtained in the step (1) in an oven, and cutting the waste textiles into fragments with the area of about 1cm 2;
(3) adding the textile fragments obtained in the step (2) into 100ml of water, placing the textile fragments into a high-pressure homogenizer, and homogenizing under the conditions that the rotating speed is 8000rpm and the pressure is 800bar to obtain a mixture containing fibers and water;
(4) Adding 10g of montmorillonite and 5g of hydroxymethyl melamine resin into the mixture obtained in the step (3), and stirring for 1h at high speed of 1200rpm on a mechanical stirrer to obtain homogeneous suspension;
(5) Freezing the suspension obtained in the step (4) in liquid nitrogen at-196 ℃ to obtain frozen gel;
(6) drying the frozen gel obtained in the step (5) in a freeze dryer, wherein the freeze drying temperature is-50 ℃, the freeze drying time is 72 hours, and removing the solvent in the gel to form aerogel;
(7) Placing the aerogel obtained in the step (6) in a tubular furnace, firstly heating to 300 ℃ in an air atmosphere at a heating rate of 2 ℃/min for pre-oxidation treatment, and preserving heat for 3 hours; and then raising the temperature to 1000 ℃ in the nitrogen atmosphere, preserving the heat for 4h for carbonization, and then slowly cooling to room temperature to obtain the clay/carbon aerogel.
Example 2
A preparation method of clay/carbon aerogel is characterized by comprising the following steps:
(1) adding 15g of waste linen textiles into a detergent for cleaning; then washing for the second time by using an aqueous solution;
(2) drying the waste textiles obtained in the step (1) in an oven, and cutting the waste textiles into fragments with the area of about 2cm 2;
(3) Adding the textile fragments obtained in the step (2) into 100ml of water, and placing the textile fragments into an ultrasonic cell crusher with the ultrasonic power of 800W; homogenizing under the condition of ultrasonic time of 100min to obtain a mixture containing fibers and water;
(4) Adding 5g of montmorillonite and 2g of melamine-formaldehyde resin into the mixture obtained in the step (3), and stirring for 1.5h at a high speed of 1200rpm on a mechanical stirrer to obtain homogeneous suspension;
(5) freezing the suspension obtained in the step (4) in liquid nitrogen at-196 ℃ to obtain frozen gel;
(6) drying the frozen gel obtained in the step (5) in a freeze dryer, wherein the freeze drying temperature is-60 ℃, the freeze drying time is 60 hours, and removing the solvent in the gel to form aerogel;
(7) Placing the aerogel obtained in the step (6) in a tubular furnace, firstly heating to 300 ℃ in an air atmosphere at a heating rate of 3 ℃/min for pre-oxidation treatment, and preserving heat for 3 hours; and then raising the temperature to 1000 ℃ in the nitrogen atmosphere, preserving the heat for 5h for carbonization, and then slowly cooling to room temperature to obtain the clay/carbon aerogel.
example 3
A preparation method of clay/carbon aerogel is characterized by comprising the following steps:
(1) adding 15g of waste wool textiles into a detergent for cleaning; then washing for the second time by using an aqueous solution;
(2) drying the waste textiles obtained in the step (1) in an oven, and cutting the waste textiles into fragments with the area of about 1cm 2;
(3) Adding the textile fragments obtained in the step (2) into 100ml of water, placing the textile fragments into a high-pressure homogenizer, and homogenizing under the conditions that the rotating speed is 8000rpm and the pressure is 800bar to obtain a mixture containing fibers and water;
(4) adding 8g of montmorillonite and 2g of boric acid into the mixture obtained in the step (3), and stirring for 2 hours at high speed of 1200rpm on a mechanical stirrer to obtain homogeneous suspension;
(5) Freezing the suspension obtained in the step (4) in liquid nitrogen at-196 ℃ to obtain frozen gel;
(6) Drying the frozen gel obtained in the step (5) in a freeze dryer, wherein the freeze drying temperature is-80 ℃, the freeze drying time is 84 hours, and removing the solvent in the gel to form aerogel;
(7) placing the aerogel obtained in the step (6) in a tubular furnace, firstly heating to 300 ℃ in an air atmosphere at a heating rate of 5 ℃/min for pre-oxidation treatment, and keeping the temperature for 4 hours; and then raising the temperature to 1000 ℃ in the nitrogen atmosphere, preserving the heat for 5h for carbonization, and then slowly cooling to room temperature to obtain the clay/carbon aerogel.
Example 4
a preparation method of clay/carbon aerogel is characterized by comprising the following steps:
(1) Adding 20g of silk waste textiles into a detergent for cleaning; then washing for the second time by using an aqueous solution;
(2) Drying the waste textiles obtained in the step (1) in an oven, and cutting the waste textiles into fragments with the area of about 1cm 2;
(3) adding the textile fragments obtained in the step (2) into 100ml of water, and placing the textile fragments into a high-pressure homogenizer for homogenization treatment under the pressure of 800bar to obtain a mixture containing fibers and water;
(4) adding 15g of montmorillonite and 6g of glutaraldehyde into the mixture obtained in the step (3), and stirring for 1h at high speed of 1200rpm on a mechanical stirrer to obtain homogeneous suspension;
(5) Freezing the suspension obtained in the step (4) in liquid nitrogen at-196 ℃ to obtain frozen gel;
(6) Drying the frozen gel obtained in the step (5) in a freeze dryer, wherein the freeze drying temperature is-79 ℃, the freeze drying time is 96 hours, and removing the solvent in the gel to form aerogel;
(7) Placing the aerogel obtained in the step (6) in a tubular furnace, firstly heating to 300 ℃ in an air atmosphere at a heating rate of 4 ℃/min for pre-oxidation treatment, and keeping the temperature for 4 h; and then heating to 900 ℃ in the nitrogen atmosphere, preserving the heat for 5 hours for carbonization, and then slowly cooling to room temperature to obtain the clay/carbon aerogel.
finally, it should be noted that the present invention is not limited to the above-mentioned embodiments, the description of the above-mentioned embodiments is only the principle of the present invention, and various changes and modifications of the present invention may be made without departing from the spirit and scope of the present invention, and some technical features may be replaced with equivalents and the described technical solutions may be modified and included in the protection scope of the present invention.
Claims (10)
1. the preparation method of the adsorption aerogel is characterized by comprising the following steps:
(1) Adding a detergent into waste textiles of natural fibers such as cotton, hemp, silk, wool and the like for cleaning; washing with water for the second time;
(2) placing the waste textile obtained in the step (1) in an oven, wherein the temperature of the oven is 60 ℃, drying and then cutting into pieces;
(3) adding the textile fragments obtained in the step (2) into water, and homogenizing the textile fragments to obtain a mixture containing fibers and water;
(4) Adding clay particles and a cross-linking agent into the mixture obtained in the step (3), adding phosphoric acid to adjust the pH value to 3-4 so as to provide an acid environment for cross-linking, stirring at high speed for 30-60min on a mechanical stirrer at the rotating speed of 1200rpm, and uniformly stirring to obtain a homogeneous suspension;
(5) Freezing the suspension obtained in the step (4) in liquid nitrogen at-196 ℃ to obtain frozen gel;
(6) drying the frozen gel obtained in the step (5) in a freeze dryer at the temperature of minus 80 ℃ to minus 50 ℃ for 48-96 hours, and removing the solvent in the gel to form aerogel;
(7) placing the aerogel obtained in the step (6) in a tubular furnace, firstly heating to 150-; then raising the temperature to 600-1000 ℃ in the nitrogen atmosphere, preserving the heat for 4-6h for carbonization, and then slowly cooling to room temperature to obtain the clay/carbon aerogel.
2. the process for preparing a clay/carbon aerogel according to claim 1, wherein: the area of the fragments in the step (2) is 0.2-2cm 2.
3. The process for preparing a clay/carbon aerogel according to claim 1, wherein: the step (3) of adding the textile fragments into water means that one or more of cotton, hemp, silk and wool waste old textile fragments are added into water.
4. The process for preparing a clay/carbon aerogel according to claim 1, wherein: the mechanical treatment in the step (3) comprises any one of ultrasonic treatment and high-pressure homogenization treatment, wherein the ultrasonic treatment is an ultrasonic cell crusher, and the ultrasonic power is 800-; the ultrasonic treatment time is 60-150 min; the high-pressure homogenizing treatment is a high-pressure homogenizer with the pressure of 500-800 bar.
5. the process for preparing a clay/carbon aerogel according to claim 1, wherein: the mass fraction of the fibers in the mixture containing the fibers and the water in the step (3) is 10-40%.
6. the process for preparing a clay/carbon aerogel according to claim 1, wherein: the length range of the fiber in the step (3) is 0.5-3 mm.
7. the process for preparing a clay/carbon aerogel according to claim 1, wherein: and (4) the clay particles in the step (4) are one of montmorillonite, sepiolite, kaolinite, talcum powder and saponite.
8. The process for preparing a clay/carbon aerogel according to claim 1, wherein: the mass fraction of the clay particles in the step (4) is 1-15%.
9. The process for preparing a clay/carbon aerogel according to claim 1, wherein: the cross-linking agent in the step (4) is one or more of glutaraldehyde, divinyl sulfone, diisocyanate, methylol melamine resin, melamine-formaldehyde resin, boric acid and borate.
10. The process for preparing a clay/carbon aerogel according to claim 1, wherein: the mass fraction of the cross-linking agent in the step (4) is 1-10%.
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Cited By (2)
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| CN112426979A (en) * | 2020-11-13 | 2021-03-02 | 四川大学 | Waste textile metal nanoparticle composite carbon fiber aerogel and preparation method thereof |
| CN113150365A (en) * | 2021-05-27 | 2021-07-23 | 淮阴工学院 | Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method |
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| CN113150365A (en) * | 2021-05-27 | 2021-07-23 | 淮阴工学院 | Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method |
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Application publication date: 20191206 |