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 PDF

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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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waste
polyester fiber
cellulose
textile
solution
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CN112358642A (en
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崔永明
赵逸飞
石从众
陈悟
董雄伟
朱立成
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Dragon Totem Technology Hefei Co ltd
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Wuhan Textile University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00Foams characterised by their properties
    • C08J2205/02Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026Aerogel, i.e. a supercritically dried gel
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/02Cellulose; 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

Method for preparing cellulose/polyester fiber composite aerogel by adopting waste textiles
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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Citations (8)

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CN102391534A (en) * 2011-08-02 2012-03-28 李大纲 Method for preparing film for high barrier property packaging by using bacterial cellulose
CN102666669A (en) * 2009-09-14 2012-09-12 诺丁汉大学 Cellulose nanoparticle aerogels, hydrogels and organogels
CN105622980A (en) * 2015-11-27 2016-06-01 南京林业大学 Method for preparing wood fiber gel material from LiCl/DMSO dissolved lignocelluloses
CN107699966A (en) * 2017-09-18 2018-02-16 浙江纺织服装职业技术学院 A kind of method of cellulose electrostatic spinning
WO2019047176A1 (en) * 2017-09-08 2019-03-14 香港纺织及成衣研发中心 Method for recycling waste polyester-cotton blend fabrics
CN109912835A (en) * 2019-03-06 2019-06-21 中国科学院过程工程研究所 A kind of method of polyester cotton preparation cellulose aerogels
WO2019190400A1 (en) * 2018-03-28 2019-10-03 National University Of Singapore A polyethylene terephthalate (pet) aerogel
CN111205506A (en) * 2020-03-20 2020-05-29 四川大学 Preparation method of waste textile flame-retardant aerogel

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106065085A (en) * 2016-06-30 2016-11-02 余燕平 A kind of recovery of solubilized textile, regenerate, recycling technology
US10611891B2 (en) * 2018-02-01 2020-04-07 The Hong Kong Research Institute Of Textiles And Apparel Limited Textile waste processing

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102666669A (en) * 2009-09-14 2012-09-12 诺丁汉大学 Cellulose nanoparticle aerogels, hydrogels and organogels
CN102391534A (en) * 2011-08-02 2012-03-28 李大纲 Method for preparing film for high barrier property packaging by using bacterial cellulose
CN105622980A (en) * 2015-11-27 2016-06-01 南京林业大学 Method for preparing wood fiber gel material from LiCl/DMSO dissolved lignocelluloses
WO2019047176A1 (en) * 2017-09-08 2019-03-14 香港纺织及成衣研发中心 Method for recycling waste polyester-cotton blend fabrics
CN107699966A (en) * 2017-09-18 2018-02-16 浙江纺织服装职业技术学院 A kind of method of cellulose electrostatic spinning
WO2019190400A1 (en) * 2018-03-28 2019-10-03 National University Of Singapore A polyethylene terephthalate (pet) aerogel
CN109912835A (en) * 2019-03-06 2019-06-21 中国科学院过程工程研究所 A kind of method of polyester cotton preparation cellulose aerogels
CN111205506A (en) * 2020-03-20 2020-05-29 四川大学 Preparation method of waste textile flame-retardant aerogel

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