CN109806850B - Viscose non-woven fabric material with adsorption performance and preparation method thereof - Google Patents
Viscose non-woven fabric material with adsorption performance and preparation method thereof Download PDFInfo
- Publication number
- CN109806850B CN109806850B CN201910226537.2A CN201910226537A CN109806850B CN 109806850 B CN109806850 B CN 109806850B CN 201910226537 A CN201910226537 A CN 201910226537A CN 109806850 B CN109806850 B CN 109806850B
- Authority
- CN
- China
- Prior art keywords
- woven fabric
- beta
- viscose
- cyclodextrin
- adsorption
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a viscose non-woven fabric material with adsorption performance, which is characterized in that the preparation method comprises the following steps: beta-cyclodextrin (beta-CD) is used as a raw material, hexachlorocyclotriphosphazene (PNC) is used as a cross-linking agent, nucleophilic substitution reaction is carried out, so that the beta-cyclodextrin is chemically immobilized on the viscose non-woven fabric, and then the viscose non-woven fabric material with adsorption performance is prepared by washing, filtering, soaking in acid solution and drying. The viscose non-woven fabric material prepared by the invention has a multi-level pore structure of micropores, mesopores, macropores and the like, and can efficiently adsorb organic pollutants, heavy metal ions and industrial waste gas in wastewater.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a viscose non-woven fabric material with adsorption performance and a preparation method thereof.
Background
The beta-cyclodextrin has a ' cone-shaped cavity structure with ' inner hydrophobicity and outer hydrophilicity ', the cavity can interact with hydrophobic organic molecules to form a reversible host-guest inclusion compound, gas molecules can be absorbed into the cavity of the beta-cyclodextrin, and the beta-cyclodextrin is simple in preparation method, low in price and widely used as an adsorption material. However, the beta-cyclodextrin has good water solubility in an aqueous solution, so that the application of the beta-cyclodextrin in the field of adsorption is limited.
The viscose fiber is a common textile raw material, has excellent water absorption and is environment-friendly. The viscose non-woven fabric is used as a substrate material to chemically immobilize the beta-cyclodextrin porous material, so that the environment-friendly efficient adsorbing material can be prepared. The adsorption material has a multi-level pore structure of micropores, mesopores, macropores and the like, can improve the range of adsorbed molecules, and has the advantages of convenience in use, reusability and the like in a fabric form.
Due to the reactivity of phosphorus-chlorine bonds, chlorine can be easily substituted by hexachlorocyclotriphosphazene (PNC), and a series of phosphazene compounds can be prepared. In addition, due to the stability of the six-membered ring, the six-membered ring has the characteristics of acid resistance, alkali resistance and high temperature resistance. Therefore, hexachlorocyclotriphosphazene is taken as a cross-linking agent, and nucleophilic substitution reaction is easy to occur with hydroxyl (-OH) of beta-cyclodextrin and hydroxyl (-OH) of the viscose non-woven fabric, so that the viscose non-woven fabric material with high-efficiency adsorption performance is prepared and is used for adsorbing organic pollutants, heavy metal ions, industrial waste gas and the like in waste water.
Most of the existing viscose non-woven fabric adsorption materials are nanocellulose-based materials prepared by blending nanocellulose with activated carbon, chitosan, ferroferric oxide and the like, but the nanocellulose is expensive, the blending preparation process with the activated carbon, the ferroferric oxide and the like is complex, and the defects of low adsorption capacity to organic pollutants and the like exist.
Disclosure of Invention
The invention aims to solve the technical problem of providing a viscose non-woven fabric material with adsorption performance and a preparation method thereof, so as to realize high-efficiency adsorption of organic pollutants, heavy metal ions, industrial waste gas and the like in waste water.
In order to solve the technical problem, the invention provides a viscose non-woven fabric material with adsorption performance, which is characterized in that the preparation method comprises the following steps: beta-cyclodextrin (beta-CD) and viscose non-woven fabric are used as raw materials, hexachlorocyclotriphosphazene (PNC) is used as a cross-linking agent, nucleophilic substitution reaction is carried out to enable the beta-cyclodextrin to be chemically immobilized on the viscose non-woven fabric, and then washing, filtering, acid solution soaking and drying are carried out to obtain the viscose non-woven fabric material with the adsorption performance.
Preferably, the nucleophilic substitution reaction is a pairwise nucleophilic substitution reaction between hydroxyl (-OH) of the beta-cyclodextrin and hydroxyl (-OH) of the viscose non-woven fabric and halogen (-Cl) of hexachlorocyclotriphosphazene.
Preferably, the viscose non-woven fabric material with the adsorption performance has three pore structures of micro pores, meso pores and macro pores, and can quickly and efficiently adsorb organic pollutants, heavy metal ions and industrial waste gas in waste water.
The invention also provides a preparation method of the viscose non-woven fabric material with the adsorption performance, which is characterized by comprising the following steps:
step 1: under the protection of nitrogen, Tetrahydrofuran (THF) and N, N Dimethylformamide (DMF) are placed in a reaction kettle, then beta-cyclodextrin (beta-CD), viscose non-woven fabric, hexachlorocyclotriphosphazene (PNC) and a catalyst are added into the reaction kettle for nucleophilic substitution reaction, and the viscose non-woven fabric immobilized with the beta-cyclodextrin is obtained after filtration;
step 2: repeatedly washing and filtering the non-woven fabric with deionized water, then soaking in an acid solution, washing and filtering to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum to obtain the viscose non-woven fabric material with the adsorption performance.
Preferably, the feeding mass ratio of the tetrahydrofuran to the N, N-dimethylformamide in the step 1 is 5: 1-10: 1.
Preferably, the feeding molar ratio of the beta-cyclodextrin to the tetrahydrofuran in the step 1 is 1: 6-1: 10; the feeding molar ratio of the beta-cyclodextrin to the N, N-dimethylformamide is 2: 1-1: 3.
Preferably, the feeding molar ratio of the beta-cyclodextrin to the hexachlorocyclotriphosphazene in the step 1 is 2: 1-1: 5; the feeding molar ratio of the catalyst to the beta-cyclodextrin is 9: 1-12: 1; the feeding mass ratio of the beta-cyclodextrin to the viscose non-woven fabric is 7: 1-10: 1.
Preferably, the reaction temperature of the nucleophilic substitution reaction in the step 1 is 50-90 ℃, and the reaction time is 12-48 h.
Preferably, the catalyst in the step 1 is any one of anhydrous sodium carbonate, antimony trioxide, manganese dioxide and ferric trichloride.
Preferably, the acid solution in the step 2 is any one of a hydrochloric acid solution, a nitric acid solution and a sulfuric acid solution, the concentration is 0.01-0.1 mol/L, and the soaking time is 1-6 h.
Preferably, the drying temperature of the vacuum drying in the step 3 is 50-80 ℃, and the drying time is 12-48 h.
Compared with the prior art, the invention has the beneficial effects that:
the invention utilizes a one-step method to chemically immobilize the beta-cyclodextrin on the viscose non-woven fabric through nucleophilic substitution reaction to prepare the viscose non-woven fabric material with adsorption property, and the preparation method is simple, the raw material source is wide, and the price is low. The prepared viscose non-woven fabric material with the adsorption performance is environment-friendly, has a multi-level pore structure of micropores, mesopores, macropores and the like, can quickly and efficiently adsorb organic pollutants, heavy metal ions and industrial waste gas in wastewater, and has a good application prospect.
Drawings
FIG. 1 is a schematic view of a process for preparing a viscose nonwoven material with absorbent properties;
fig. 2 is an infrared spectrum of the viscose nonwoven material with adsorption properties prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The molecular structure and composition of the finally synthesized viscose non-woven fabric material pass through an X-ray photoelectron spectrometer (C, O, N, P) and a nuclear magnetic resonance instrument (13C NMR、31P NMR), fourier transform infrared spectrometer (FTIR), and the like; characterizing the specific surface area, the pore size and the distribution range of the non-woven material by a BET specific surface area and porosity analyzer; characterization of the tables by Scanning Electron Microscopy (SEM)A surface morphology structure, and the like.
Weighing 20mg of viscose non-woven fabric material, respectively putting the viscose non-woven fabric material into 20ml of methylene blue solutions with different concentrations (100mol/L,200mol/L,400mol/L,800mol/L and 1000mol/L), then putting the viscose non-woven fabric material into a constant temperature oscillator, carrying out absorption oscillation for 12 hours at room temperature to ensure that the viscose non-woven fabric solution reaches absorption balance, filtering the viscose non-woven fabric solution by using a filter membrane after oscillation is finished, testing the absorbance of methylene blue in filtrate by using an ultraviolet-visible spectrophotometer, and calculating the absorption rate of the material to the methylene blue according to a formula.
100mL of Cd with the mass concentration of 100 mg/L-1000 mg/L2+Adding 0.1g of viscose non-woven fabric material into the solution, stirring and adsorbing for 24 hours in a water bath shaking table under the conditions of room temperature and pH 6, and measuring Cd before and after adsorption by using an atomic absorption spectrophotometer2+And (5) calculating the absorbance according to a formula.
CO treatment by temperature programmed chemisorption instrument TPD/TPR2The adsorption performance test of (1) is that 200mg of viscose non-woven fabric material, N, is weighed firstly2Heating to 200 deg.C at 10 deg.C/min, drying, purging for 1 hr, cooling to 50 deg.C, introducing CO2/N2(20ml/min), adsorption experiment was performed for 120min, and N was introduced2Heating to 250 deg.C (10 deg.C/min) to remove adsorbed CO2And CO is obtained after the experiment is finished2Data on the amount of adsorption.
Example 1
A method for preparing viscose non-woven fabric material with adsorption performance (as shown in figure 1) comprises the following steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.71g), hexachlorocyclotriphosphazene (PNC) (1.74g) and anhydrous sodium carbonate (12.42g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L hydrochloric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
FIG. 2 shows an infrared spectrum (3400 cm) of the prepared viscose non-woven fabric material-1～3200cm-1Is an absorption peak generated by the stretching vibration of hydroxyl (-OH); 2960cm-1Is an absorption peak generated by methylene stretching vibration; 1305cm-1Is an absorption peak generated by P ═ O stretching vibration; 698cm-1Is the absorption peak due to P-Cl vibration). The P ═ O and P-Cl vibration peaks are generated, which indicates that the beta-CD is successfully immobilized on the viscose non-woven fabric.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the immobilization rate of beta-cyclodextrin (beta-CD) obtained by a weighing method is 16.7 percent, the adsorption rate of methylene blue reaches 96.7 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 94.6 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.12mmol g-1。
Example 2
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottomed flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.71g), hexachlorocyclotriphosphazene (PNC) (1.74g) and antimony trioxide (15.18g) into the round-bottomed flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L sulfuric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the beta-cyclodextrin (beta-CD) immobilization rate is 21.4 percent, the methylene blue adsorption rate is 95.2 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 93.7 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.02mmol g-1。
Example 3
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.71g), hexachlorocyclotriphosphazene (PNC) (1.74g) and manganese dioxide (16.58g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L hydrochloric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the immobilization rate of beta-cyclodextrin (beta-CD) obtained by a weighing method is 16.6 percent, the adsorption rate of methylene blue reaches 94.8 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 93.2 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.01mmol g-1。
Example 4
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.71g), hexachlorocyclotriphosphazene (PNC) (1.74g) and ferric trichloride (13.8g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L nitric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the beta-cyclodextrin (beta-CD) immobilization rate is 17.3 percent, the methylene blue adsorption rate is 94.3 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 93.9 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.10mmol g-1。
Example 5
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.71g), hexachlorocyclotriphosphazene (PNC) (3.48g) and anhydrous sodium carbonate (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L hydrochloric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the beta-cyclodextrin (beta-CD) immobilization rate is 21.7 percent, the methylene blue adsorption rate is 97.3 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 96.7 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.17mmol g-1。
Example 6
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.5g), hexachlorocyclotriphosphazene (PNC) (3.48g) and ferric trichloride (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L sulfuric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized material has adsorption performanceThe adhesive non-woven fabric material is obtained by a weighing method, the beta-cyclodextrin (beta-CD) immobilization rate is 25.4 percent, the methylene blue adsorption rate is 95.1 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 94.3 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.31mmol g-1。
Example 7
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.33g), hexachlorocyclotriphosphazene (PNC) (3.48g) and anhydrous sodium carbonate (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L hydrochloric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the immobilization rate of beta-cyclodextrin (beta-CD) obtained by a weighing method is 28.8 percent, the adsorption rate of methylene blue reaches 96.7 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 95.2 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.23mmol g-1。
Example 8
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.2g), hexachlorocyclotriphosphazene (PNC) (6.96g) and anhydrous sodium carbonate (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L nitric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the immobilization rate of beta-cyclodextrin (beta-CD) obtained by a weighing method is 24.7 percent, the adsorption rate of methylene blue reaches 96.1 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 95.8 percent, and the catalyst has high CO adsorption rate2The adsorption capacity of (b) is up to 4.17mmol g-1。
Example 9
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.33g), hexachlorocyclotriphosphazene (PNC) (13.92g) and anhydrous sodium carbonate (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L sulfuric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the immobilization rate of beta-cyclodextrin (beta-CD) obtained by a weighing method is 31.7 percent, the adsorption rate of methylene blue reaches 95.6 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 95.3 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.27mmol g-1。
Example 10
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.33g), hexachlorocyclotriphosphazene (PNC) (13.92g) and manganese dioxide (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L hydrochloric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the immobilization rate of beta-cyclodextrin (beta-CD) obtained by a weighing method is 38.7 percent, the adsorption rate of methylene blue reaches 96.9 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 94.6 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.16mmol g-1。
Example 11
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.33g), hexachlorocyclotriphosphazene (PNC) (13.92g) and anhydrous sodium carbonate (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L hydrochloric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the immobilization rate of beta-cyclodextrin (beta-CD) obtained by a weighing method is 45.7 percent, the adsorption rate of methylene blue reaches 98.1 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 96.5 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.37mmol g-1。
Example 12
A preparation method of a viscose non-woven fabric material with adsorption performance comprises the following specific preparation steps:
step 1: under the protection of nitrogen, putting 180mL of Tetrahydrofuran (THF) and 20mL of N, N-Dimethylformamide (DMF) into a round-bottom flask, then adding beta-cyclodextrin (beta-CD) (12g), viscose non-woven fabric (1.33g), hexachlorocyclotriphosphazene (PNC) (13.92g) and ferric trichloride (15.18g) into the round-bottom flask, carrying out nucleophilic substitution reaction at 80 ℃ for 36h, and carrying out suction filtration by a circulating water type vacuum pump to obtain the viscose non-woven fabric immobilized with the beta-cyclodextrin;
step 2: washing the non-woven fabric with deionized water for 4-5 times, performing suction filtration with a circulating water vacuum pump, soaking in 100mL of 0.01mol/L nitric acid solution for 1h, washing with deionized water for 2-3 times, and performing suction filtration with the circulating water vacuum pump to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum at the drying temperature of 60 ℃ for 12 hours to obtain the viscose non-woven fabric material with the adsorption performance.
The synthesized viscose non-woven fabric material with the adsorption performance has the advantages that the beta-cyclodextrin (beta-CD) immobilization rate is 36.9 percent, the methylene blue adsorption rate is 96.6 percent, and heavy metal ions (Cd)2+) The adsorption rate of the catalyst reaches 94.7 percent, and the catalyst has CO adsorption rate2The adsorption capacity of (b) is up to 4.22mmol g-1。
Claims (9)
1. A viscose non-woven fabric material with adsorption performance is characterized in that the preparation method comprises the following steps: taking beta-cyclodextrin and viscose non-woven fabric as raw materials, taking hexachlorocyclotriphosphazene as a cross-linking agent, carrying out nucleophilic substitution reaction to enable the beta-cyclodextrin to be chemically immobilized on the viscose non-woven fabric, and then washing, filtering, soaking in an acid solution and drying to obtain the viscose non-woven fabric material with adsorption performance; the viscose non-woven fabric material with the adsorption performance has three pore structures of micro pores, meso pores and macro pores.
2. The viscose nonwoven material with adsorption performance of claim 1, wherein the nucleophilic substitution reaction is a pair-wise nucleophilic substitution reaction of hydroxyl groups of β -cyclodextrin and hydroxyl groups of viscose nonwoven with halogen of hexachlorocyclotriphosphazene.
3. A method for preparing the viscose non-woven fabric material with adsorption property according to claim 1, which comprises the following steps:
step 1: under the protection of nitrogen, placing tetrahydrofuran and N, N-dimethylformamide into a reaction kettle, then adding beta-cyclodextrin, viscose non-woven fabric, hexachlorocyclotriphosphazene and a catalyst into the reaction kettle, carrying out nucleophilic substitution reaction, and filtering to obtain beta-cyclodextrin immobilized viscose non-woven fabric;
step 2: repeatedly washing and filtering the non-woven fabric with deionized water, then soaking in an acid solution, washing and filtering to obtain the non-woven fabric;
and step 3: and (3) drying the non-woven fabric obtained in the step (2) in vacuum to obtain the viscose non-woven fabric material with the adsorption performance.
4. The method for preparing the viscose nonwoven material with adsorption property according to claim 3, wherein the feeding mass ratio of the tetrahydrofuran to the N, N-dimethylformamide in the step 1 is 5: 1-10: 1; the feeding molar ratio of the beta-cyclodextrin to the tetrahydrofuran is 1: 6-1: 10; the feeding molar ratio of the beta-cyclodextrin to the N, N-dimethylformamide is 2: 1-1: 3.
5. The method for preparing viscose nonwoven material with adsorption performance according to claim 3, wherein the feeding molar ratio of the beta-cyclodextrin to the hexachlorocyclotriphosphazene in the step 1 is 2: 1-1: 5; the feeding molar ratio of the catalyst to the beta-cyclodextrin is 9: 1-12: 1; the feeding mass ratio of the beta-cyclodextrin to the viscose non-woven fabric is 7: 1-10: 1.
6. The method for preparing the viscose nonwoven material with adsorption property according to claim 3, wherein the nucleophilic substitution reaction temperature in the step 1 is 50-90 ℃ and the reaction time is 12-48 h.
7. The method for preparing viscose nonwoven material with adsorption property according to claim 3, wherein the catalyst in step 1 is any one of anhydrous sodium carbonate, antimony trioxide, manganese dioxide and ferric trichloride.
8. The method for preparing a viscose nonwoven material with adsorption property according to claim 3, wherein the acid solution in the step 2 is any one of hydrochloric acid solution, nitric acid solution and sulfuric acid solution, the concentration is 0.01 mol/L-0.1 mol/L, and the soaking time is 1-6 h.
9. The method for preparing the viscose nonwoven fabric material with the adsorption property according to claim 3, wherein the drying temperature of the vacuum drying in the step 3 is 50 ℃ to 80 ℃, and the drying time is 12h to 48 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910226537.2A CN109806850B (en) | 2019-03-25 | 2019-03-25 | Viscose non-woven fabric material with adsorption performance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910226537.2A CN109806850B (en) | 2019-03-25 | 2019-03-25 | Viscose non-woven fabric material with adsorption performance and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109806850A CN109806850A (en) | 2019-05-28 |
| CN109806850B true CN109806850B (en) | 2021-12-10 |
Family
ID=66610172
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910226537.2A Active CN109806850B (en) | 2019-03-25 | 2019-03-25 | Viscose non-woven fabric material with adsorption performance and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109806850B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220362A (en) * | 2015-11-06 | 2016-01-06 | 吉林大学 | A kind of beta-schardinger dextrin-based nano-fiber film and preparation method thereof and the application in Dye Adsorption, separation |
| FR3039840A1 (en) * | 2015-08-05 | 2017-02-10 | Ajelis Sas | MATERIAL BASED ON HYDROPHILIC NATURAL FIBERS AND USE THEREOF FOR THE EXTRACTION OF METALS PRESENT IN AQUEOUS ENVIRONMENT |
| CN106398109A (en) * | 2016-10-07 | 2017-02-15 | 河南工业大学 | Preparation method of cyclotriphosphazene cured phenolic resin |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003243885B8 (en) * | 2002-05-09 | 2009-08-06 | Hemoteq Ag | Medical products comprising a haemocompatible coating, production and use thereof |
| US8152902B2 (en) * | 2009-09-30 | 2012-04-10 | Cellresin Technologies, Llc | Packaging material such as film, fiber, woven and nonwoven fabric with adsorbancy |
| CN102002118B (en) * | 2010-10-15 | 2012-07-25 | 华东理工大学 | Method for preparing dimer(fatty acid)yl polyester by grafting on cyclodextrin |
| CN103554428B (en) * | 2013-11-18 | 2015-05-13 | 中国林业科学研究院林产化学工业研究所 | Core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite and application thereof in rigid polyurethane foaming plastic |
| US10364163B2 (en) * | 2014-06-06 | 2019-07-30 | University Of Houston System | Porous nanocomposite polymer hydrogels for water treatment |
| CN104109221B (en) * | 2014-07-08 | 2016-08-17 | 中国农业科学院农业环境与可持续发展研究所 | A kind of synthetic method of cellulose graft cyclodextrin hydroscopic high-molecular resin |
| CN104530437A (en) * | 2014-12-02 | 2015-04-22 | 天津工业大学 | Preparation method of cyclodextrin grafted chitosan polymer with water pollutant separating property |
| CN104785215B (en) * | 2015-04-03 | 2017-11-24 | 山东大学 | A kind of magnetic cyclodextrin carbon nano-fiber composite material and preparation method thereof |
| CN107099049A (en) * | 2017-05-16 | 2017-08-29 | 东华大学 | A kind of beta-cyclodextrin cross-linked chitosan multi-porous sorbing material of citric acid-modified and its preparation and application |
-
2019
- 2019-03-25 CN CN201910226537.2A patent/CN109806850B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3039840A1 (en) * | 2015-08-05 | 2017-02-10 | Ajelis Sas | MATERIAL BASED ON HYDROPHILIC NATURAL FIBERS AND USE THEREOF FOR THE EXTRACTION OF METALS PRESENT IN AQUEOUS ENVIRONMENT |
| CN105220362A (en) * | 2015-11-06 | 2016-01-06 | 吉林大学 | A kind of beta-schardinger dextrin-based nano-fiber film and preparation method thereof and the application in Dye Adsorption, separation |
| CN106398109A (en) * | 2016-10-07 | 2017-02-15 | 河南工业大学 | Preparation method of cyclotriphosphazene cured phenolic resin |
Non-Patent Citations (1)
| Title |
|---|
| "负载β-环糊精纤维素纤维在污水处理中的应用研究";万军民等;《环境污染与防治》;20040225;第26卷(第1期);第58页左栏第1.2.1节，第59页右栏第2段 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109806850A (en) | 2019-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109806851B (en) | Cyclodextrin porous material and preparation method thereof | |
| US20220040669A1 (en) | Supported poly(allyl)amine and derivatives for co2 capture from flue gas or ultra-dilute gas streams such as ambient air or admixtures thereof | |
| CN103406096A (en) | Nitrogen-doped porous carbon material, preparation method and use thereof | |
| CN109021245A (en) | A kind of preparation and application of multi-stage porous Cu Base Metal organic framework material | |
| CN110040732B (en) | Alkali metal modified porous carbon material and preparation method and application thereof | |
| CN103933929A (en) | Mesoporous silica adsorbent for adsorbing hydrophobic organic matters as well as preparation method and application of mesoporous silica adsorbent | |
| CN112657472A (en) | Ionic covalent triazine skeleton polymer material and preparation method and application thereof | |
| CN109806850B (en) | Viscose non-woven fabric material with adsorption performance and preparation method thereof | |
| CN114632550B (en) | MOF derivatization carrier and preparation method and application thereof | |
| KR101968386B1 (en) | Gas adsorbent and method of manufacturing of the same | |
| KR101418868B1 (en) | Manufacturing method of microporous adsorbents for carbon dioxide capture | |
| CN112574370A (en) | Three-dimensional hydroxyl-containing covalent organic framework material and preparation method thereof | |
| CN109293937A (en) | A method of tradition ZIF-90 material is prepared using bimetal salt room temperature | |
| CN113754796B (en) | Naphthalene-modified crosslinked beta-cyclodextrin gel, preparation method and application | |
| CN115521426B (en) | Imine-linked microporous covalent organic framework material, preparation method and application thereof | |
| CN111004103A (en) | Compound, covalent organic framework material, and preparation method and application thereof | |
| CN112851939B (en) | Porous polymer rich in hydroxyl and secondary amino and preparation method thereof | |
| CN114950388A (en) | Preparation method of amine hollow fiber adsorbent loaded by polymer/silicon dioxide | |
| CN114773598A (en) | Ionic type hypercrosslinked porous polymer and preparation method thereof | |
| CN113198425A (en) | Covalent organic framework material and preparation method and application thereof | |
| CN115739043B (en) | Triazine structure functionalized cationic organic polymer and preparation method and application thereof | |
| CN114425301A (en) | Nitrogen-phosphorus co-doped carbon material for adsorbing heavy metal ions and preparation method thereof | |
| CN113845606B (en) | Modified cyclodextrin dye adsorbent and preparation method thereof | |
| KR101777838B1 (en) | Nanoporous Fluorinated Covalent Organic Polymers for Selective Adsorption of Organic Molecules and Method of Preparing Same | |
| CN115010942B (en) | Preparation method and application of ratiometric fluorescent probe Tb-UiO-66 with high selectivity on styrene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |