CN112358642B - Method for preparing cellulose/polyester fiber composite aerogel by adopting waste textiles - Google Patents
Method for preparing cellulose/polyester fiber composite aerogel by adopting waste textiles Download PDFInfo
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- CN112358642B CN112358642B CN202011083789.3A CN202011083789A CN112358642B CN 112358642 B CN112358642 B CN 112358642B CN 202011083789 A CN202011083789 A CN 202011083789A CN 112358642 B CN112358642 B CN 112358642B
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- 239000002699 waste material Substances 0.000 title claims abstract description 66
- 239000004753 textile Substances 0.000 title claims abstract description 61
- 229920000728 polyester Polymers 0.000 title claims abstract description 56
- 239000004964 aerogel Substances 0.000 title claims abstract description 52
- 239000000835 fiber Substances 0.000 title claims abstract description 50
- 229920002678 cellulose Polymers 0.000 title claims abstract description 45
- 239000001913 cellulose Substances 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229920000742 Cotton Polymers 0.000 claims abstract description 31
- 239000000243 solution Substances 0.000 claims abstract description 31
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 18
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004090 dissolution Methods 0.000 claims abstract description 15
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 14
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000499 gel Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000011240 wet gel Substances 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 230000003203 everyday effect Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims 2
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 238000007710 freezing Methods 0.000 abstract description 3
- 230000008014 freezing Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- RECVMTHOQWMYFX-UHFFFAOYSA-N oxygen(1+) dihydride Chemical compound [OH2+] RECVMTHOQWMYFX-UHFFFAOYSA-N 0.000 description 1
- 239000010893 paper waste Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
Abstract
The invention relates to a method for preparing cellulose/polyester fiber composite aerogel by using waste textiles, which comprises the steps of immersing the waste cotton-containing textiles into an anhydrous ethylenediamine solution for pretreatment, and then immersing the pretreated waste cotton-containing textiles into an N-methylmorpholine-N-oxide aqueous solution for dissolution; secondly, mixing the waste textile containing polyester fibers with phenol, and heating for dissolving; uniformly mixing an N-methylmorpholine-N-oxide aqueous solution containing cotton cellulose and a phenol solution containing polyester fibers according to a certain proportion, immersing the mixed solution into deionized water for gelling, and replacing the deionized water in the gel with tert-butyl alcohol to prepare wet gel; and finally, freezing and drying to obtain the aerogel. The waste cotton and polyester fiber textile has the characteristics of large yield, low price, difficult degradation and the like, and the cellulose/polyester fiber composite aerogel prepared from the waste cotton and polyester fiber textile improves a new way for the efficient utilization of the waste cotton and polyester fiber textile.
Description
Technical Field
The invention belongs to the technical field of preparation of composite aerogel, and particularly relates to a method for preparing cellulose/polyester fiber composite aerogel by using waste textiles.
Background
The aerogel takes air as a dispersion medium, and a skeleton is composed of polymers or nano particles, and is a nano-scale three-dimensional network structure material. In 1931, kistler prepared SiO using sodium silicate as a starting material by a sol-gel process 2 Aerogel, the findings of this study are standard to the emergence of aerogels. At present, various aerogel materials are developed vigorously, and inorganic aerogels such as silica, titania, and alumina are developed into organic aerogels and various composite aerogels.
Millions of tons of waste cotton and waste polyester fiber scraps exist in textile factories and clothing factories every year, in addition, along with the improvement of living standard of people, the waste cotton and waste polyester fiber textiles are increased day by day, and the reasonable and effective utilization of the waste textiles becomes a difficult problem to be solved at present. The aerogel material can be prepared by recycling the waste aerogel material by combining the modern technology, and the effective recycling of waste resources is realized.
Currently, cellulose as a main raw material has been widely prepared as an aerogel material, such as: the Chinese invention patent application number 201310095059.9 reports a preparation method of nano-cellulose aerogel; chinese invention patent application No. 201410227151.0 reports a method for preparing magnetic cellulose aerogel from waste paper. In order to improve the performance of cellulose aerogel, cellulose and other material composite aerogel is receiving wide attention and is becoming a hot point of research. The cellulose and other material composite aerogel changes the characteristics of cellulose, stronger interaction exists among molecules, and the prepared composite aerogel has great application prospects in the fields of gas adsorption, water ion adsorption and the like. The literature research shows that the aerogel material compounded by the cellulose and the polyester fiber is not reported yet.
Currently, aerogel is gradually coming into people's lives as an ultra-light material. The waste cotton and polyester fiber textile has the characteristics of large yield, low price, difficult degradation and the like, and the preparation of the waste cotton and polyester fiber textile into the aerogel material has important significance. With the progress of research, the preparation process of various material aerogels is increasingly simple, and the unique optical and thermal properties and mechanical properties of the aerogels can make the aerogels unique in the field of material science and widely applied.
Disclosure of Invention
Aiming at the problem that the cotton cellulose fiber and the polyester fiber are difficult to compound, the invention proposes a solution, namely, two fibers are respectively dissolved in different organic solvents, and then the organic solvents are mixed, thereby achieving the purpose of the invention. The invention aims to overcome the defects of the prior art and provides a method for preparing cellulose/polyester fiber composite aerogel by adopting waste textiles. The technical scheme of the invention provides reference for the efficient utilization of waste cotton and waste polyester fiber textiles.
A method for preparing cellulose/polyester fiber composite aerogel by adopting waste textiles comprises the following steps:
(1) Ethylene diamine pretreatment: immersing the waste cotton-containing textile into anhydrous ethylenediamine solution for 24-48 hours.
Preferably, the solid-to-liquid ratio of the waste cotton-containing textile (g) to the anhydrous ethylenediamine (mL) is as follows: 5 to 10 percent.
(2) Preparation of cellulose solution: immersing the waste cotton-containing textile treated in the step (1) into 70-90% of N-methylmorpholine-N-oxide (NMMO) aqueous solution for 24-48 hours, and stirring the textile every 1-3 hours during immersion to better dissolve cellulose in the NMMO aqueous solution; after the dissolution time was over, the solution was filtered and the filtrate collected.
Preferably, the solid-to-liquid ratio of the waste cotton-containing textiles (g) treated in the step (1) to the aqueous NMMO solution (mL) is as follows: 15 to 20 percent.
(3) Dissolution of polyester fiber: mixing the waste textile containing polyester fiber with phenol, heating to dissolve at 70-90 ℃ for 4-8 hours, and stirring every 30 minutes to fully dissolve the waste textile containing polyester fiber; after the dissolution time is over, the solution is filtered at 60-70 ℃ and the filtrate is collected.
Preferably, the mass ratio of the waste polyester fiber-containing textile (g) to the phenol (g) is as follows: 10 to 20 percent.
(4) Mixing: mixing the cellulose-containing NMMO aqueous solution prepared in the step (2) with the polyester-containing phenol solution prepared in the step (3); soaking the mixed solution into deionized water for gelling for 3-4 days, and replacing the deionized water every day to wash the gel; the deionized water in the gel was replaced with tert-butanol.
Preferably, the volume ratio of the cellulose-containing NMMO aqueous solution prepared in the step (2) to the polyester-containing phenol solution prepared in the step (3) is 1: 1-3.
(5) Preparing aerogel: and (4) freeze-drying the wet gel prepared in the step (4) at-60-65 ℃ to prepare the aerogel.
The invention has the following remarkable characteristics:
(1) The method selects the ethylenediamine to pretreat the waste cotton-containing textiles, so that the crystalline regions of the cellulose swell, and the microcrystalline regions have the function of decrystallization; therefore, the cellulose crystal form part is changed from cellulose-I to cellulose-III, and the dissolution of the cellulose by the NMMO aqueous solution is facilitated.
(2) The waste cotton and the waste polyester fiber textile have the characteristics of high yield, low price, difficult degradation and the like, and the cellulose/polyester fiber composite aerogel prepared from the waste cotton and the waste polyester fiber textile is a new way for improving the efficient utilization of the waste cotton and the waste polyester fiber textile.
(3) The invention adopts NMMO and phenol as solvents respectively, skillfully mixes the waste cotton and the waste polyester fibers together, and the mixing method provides reference for preparing the composite material.
Drawings
FIG. 1 Electron micrograph of aerogel a prepared in example 1.
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
In this embodiment, a method for preparing a cellulose/polyester fiber composite aerogel by using waste textiles includes the following steps:
(1) Ethylene diamine pretreatment: 75g of waste cotton-containing textile is immersed in 1000mL of anhydrous ethylenediamine solution for 36 hours.
(2) Preparation of cellulose solution: soaking 50g of the waste cotton-containing textile treated in the step (1) into 286mL of 80% NMMO aqueous solution for 36 hours, and stirring the textile every 2 hours during soaking to better dissolve cellulose in the NMMO aqueous solution; after the dissolution time was over, the solution was filtered and the filtrate was collected.
(3) Dissolution of polyester fiber: mixing 50g of waste textile containing polyester fibers with 333g of phenol, heating to dissolve at 80 ℃ for 6 hours, and stirring every 30 minutes to fully dissolve the waste textile containing polyester fibers; after the dissolution time was complete, the solution was filtered at 65 ℃ and the filtrate collected.
(4) Mixing: mixing 100mL of the cellulose-containing NMMO aqueous solution prepared in step (2) with 200mL of the polyester-containing phenol solution prepared in step (3); soaking the mixed solution in deionized water for gelling for 3.5 days, and replacing the deionized water every day to wash the gel; the deionized water in the gel was replaced with tert-butanol.
(5) Preparing aerogel: and (5) freezing and drying the wet gel prepared in the step (4) at-60 ℃ to prepare aerogel a, wherein an electron microscope image of the aerogel a is shown in figure 1.
Example 2
In this embodiment, a method for preparing a cellulose/polyester fiber composite aerogel by using waste textiles includes the following steps:
(1) Ethylene diamine pretreatment: 50g of waste cotton-containing textile is immersed in 1000mL of anhydrous ethylenediamine solution for 24 hours.
(2) Preparation of cellulose solution: 50g of waste cotton-containing textile treated in the step (1) is immersed in 333mL of 70% NMMO aqueous solution for 24 hours, and the textile is stirred every 1 hour during immersion, so that cellulose is better dissolved in the NMMO aqueous solution; after the dissolution time was over, the solution was filtered and the filtrate was collected.
(3) Dissolution of polyester fiber: mixing 50g of waste textile containing polyester fibers with 500g of phenol, heating to dissolve at 70 ℃ for 4 hours, and stirring every 30 minutes to fully dissolve the waste textile containing polyester fibers; after the dissolution time was complete, the solution was filtered at 70 ℃ and the filtrate collected.
(4) Mixing: mixing 100mL of the cellulose-containing NMMO aqueous solution prepared in step (2) with 100mL of the polyester-containing phenol solution prepared in step (3); soaking the mixed solution in deionized water for gelling for 3.5 days, and replacing the deionized water every day to wash the gel; the deionized water in the gel was replaced with tert-butanol.
(5) Preparing aerogel: and (4) freeze-drying the wet gel prepared in the step (4) at-65 ℃ to prepare aerogel b.
Example 3
In this embodiment, a method for preparing a cellulose/polyester fiber composite aerogel by using waste textiles includes the following steps:
(1) Ethylene diamine pretreatment: 100g of waste cotton-containing textile is immersed in 1000mL of anhydrous ethylenediamine solution for 48 hours.
(2) Preparation of cellulose solution: soaking 50g of the waste cotton-containing textile treated in the step (1) into 250mL of 90% NMMO aqueous solution for 48 hours, and stirring the textile every 3 hours during soaking to better dissolve cellulose in the NMMO aqueous solution; after the dissolution time was over, the solution was filtered and the filtrate was collected.
(3) Dissolution of polyester fiber: mixing 50g of waste textile containing polyester fibers with 250g of phenol, heating to dissolve, wherein the heating temperature is 90 ℃, the heating time is 8 hours, and stirring every 30 minutes to fully dissolve the waste textile containing polyester fibers; after the dissolution time was complete, the solution was filtered at 60 ℃ and the filtrate collected.
(4) Mixing: mixing 100mL of the cellulose-containing NMMO aqueous solution prepared in step (2) with 300mL of the polyester-containing phenol solution prepared in step (3); soaking the mixed solution in deionized water for gelling for 3.5 days, and replacing the deionized water every day to wash the gel; the deionized water in the gel was replaced with tert-butanol.
(5) Preparing aerogel: and (5) freezing and drying the wet gel prepared in the step (4) at the temperature of-65 ℃ to prepare the aerogel c.
Claims (5)
1. A method for preparing cellulose/polyester fiber composite aerogel by adopting waste textiles is characterized by comprising the following steps:
(1) Ethylene diamine pretreatment: immersing the waste cotton-containing textile into anhydrous ethylenediamine solution for 24-48 hours;
(2) Preparation of cellulose solution: immersing the waste cotton-containing textile treated in the step (1) into 70-90% of NMMO aqueous solution for 24-48 hours, and stirring the textile every 1-3 hours during immersion to better dissolve cellulose in the NMMO aqueous solution; after the dissolving time is over, filtering the solution, and collecting filtrate;
(3) Dissolution of polyester fiber: mixing the waste textile containing polyester fiber with phenol, heating to dissolve at 70-90 ℃ for 4-8 hours, and stirring every 30 minutes to fully dissolve the waste textile containing polyester fiber; after the dissolving time is over, filtering the solution, and collecting filtrate;
(4) Mixing: mixing the cellulose-containing NMMO aqueous solution prepared in the step (2) with the polyester-containing phenol solution prepared in the step (3); soaking the mixed solution into deionized water for gelling, wherein the soaking time is 3-4 days, and replacing the deionized water every day to wash the gel; replacing the deionized water in the gel by using tert-butyl alcohol;
(5) Preparing aerogel: and (4) freeze-drying the wet gel prepared in the step (4) at-60-65 ℃ to prepare the aerogel.
2. The method for preparing the cellulose/polyester fiber composite aerogel by adopting the waste textiles according to the claim 1 is characterized in that: the solid-liquid ratio of the waste cotton-containing textiles/g to the anhydrous ethylenediamine/mL in the step (1) is as follows: 5 to 10 percent.
3. The method for preparing the cellulose/polyester fiber composite aerogel by adopting the waste textiles according to the claim 1 is characterized in that: the solid-to-liquid ratio of the waste cotton-containing textiles treated in the step (1) in the step (2) to the NMMO aqueous solution/mL is as follows: 15 to 20 percent.
4. The method for preparing the cellulose/polyester fiber composite aerogel by adopting the waste textiles according to claim 1, which is characterized by comprising the following steps of: the mass ratio of the waste polyester fiber-containing textile/g to the phenol/g in the step (3) is as follows: 10 to 20 percent.
5. The method for preparing the cellulose/polyester fiber composite aerogel by adopting the waste textiles according to the claim 1 is characterized in that: the volume ratio of the NMMO aqueous solution containing cellulose prepared in the step (2) to the phenol solution containing polyester prepared in the step (3) in the step (4) is 1: 1-3.
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Effective date of registration: 20240123 Address after: 230000 floor 1, building 2, phase I, e-commerce Park, Jinggang Road, Shushan Economic Development Zone, Hefei City, Anhui Province Patentee after: Dragon totem Technology (Hefei) Co.,Ltd. Country or region after: China Address before: 430073 No. 1 Textile Road, Hongshan District, Hubei, Wuhan Patentee before: Wuhan Textile University Country or region before: China |