CN112657437B - Biomass-based composite aerogel and preparation method thereof - Google Patents
Biomass-based composite aerogel and preparation method thereof Download PDFInfo
- Publication number
- CN112657437B CN112657437B CN202011393756.9A CN202011393756A CN112657437B CN 112657437 B CN112657437 B CN 112657437B CN 202011393756 A CN202011393756 A CN 202011393756A CN 112657437 B CN112657437 B CN 112657437B
- Authority
- CN
- China
- Prior art keywords
- biomass
- based composite
- composite aerogel
- preparation
- drying
- 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
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a preparation method of biomass-based composite aerogel, which comprises the following steps: s1: mixing biomass fiber waste powder and a functional material in a weight ratio of 1: 0.1-12, then adding water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2-15 mg/mL; s2: homogenizing the stirring liquid obtained in the step (S1) to obtain a homogenized mixed liquid; s3: and (3) freeze-drying the homogeneous mixed solution obtained in the step (S2) to obtain the biomass-based composite aerogel. The invention takes biomass-based waste as a raw material, adopts a full-component self-assembly method, has very simple preparation process, does not introduce chemical reagents with serious pollution, is beneficial to large-scale production, and the obtained composite aerogel has excellent mechanical properties and great application prospects in the fields of gas storage, environmental protection and the like.
Description
Technical Field
The invention relates to the technical field of functional nano composite material preparation, in particular to biomass-based composite aerogel and a preparation method thereof.
Background
With the rapid development of global industry, heavy metal and organic dye pollution is becoming increasingly serious, and any emission thereof poses a threat to the health of human beings and natural ecosystems. These contaminants are highly toxic, non-biodegradable and tend to accumulate in the organism through the food chain, causing a great panic to people. Heavy metal ions and organic dyes are commonly adsorbed using ion exchange, chemical precipitation, catalytic degradation, and the like techniques using various inorganic water treatment materials such as activated alumina, MCM-41, gamma-zirconium phosphate, titanates, and the like. However, due to the existence of the inorganic adsorbent in powder form and low specific surface area, the above inorganic adsorbent often shows low removal capacity, poor capture kinetics, difficult separation, easy water loss, and difficult recycling in sewage treatment, and its practical application is seriously hindered. Therefore, there is a need for new materials that can overcome the above disadvantages.
Cellulose-based composite aerogel materials have been produced. Due to multiple excellent characteristics of environmental protection, rich resources, renewability, easy degradation, good biocompatibility and the like, the material becomes a functional material with good application prospect and great development value. However, the cellulose aerogel is usually prepared by a bottom-up method, and firstly, hemicellulose and lignin components in the bamboo/wood raw material are removed by a series of physical or chemical means to obtain single nano-scale cellulose fibers or nano-crystals; then, the nano-grade cellulose is assembled into bulk nano-cellulose hydrogel or aerogel by different assembling means. This complex process often results in a large consumption of time, energy and chemicals, resulting in higher cost, lower efficiency and more pollution. In addition, due to the insufficient mechanical properties of the cellulose-based composite adsorbent in the prior art, shrinkage/expansion deformation and even breakage may exist in the practical application of water treatment, so that the composite aerogel is difficult to recover. Therefore, there is an urgent need to find a method for preparing a biomass-based composite material that can be mass-produced and has high mechanical strength.
Disclosure of Invention
Therefore, in order to overcome the problems in the prior art, the invention provides the following technical scheme:
the invention provides a preparation method of biomass-based composite aerogel, which comprises the following steps:
s1: mixing biomass fiber waste powder and a functional material according to a weight ratio of 1: 0.1-12, then adding an aqueous solvent into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 0.1-20 mg/mL;
s2: homogenizing the stirring liquid obtained in the step (S1) to obtain a homogenized mixed liquid;
s3: freezing and drying the homogeneous mixed solution obtained in the step S2 to obtain the biomass-based composite aerogel;
further, the biomass fiber waste in the step S1 is plant fiber waste; furthermore, the plant fiber waste is selected from any one or more of waste paper, fallen leaves, straws, bagasse, weeds and waste seaweeds; further, the fallen leaves include, but are not limited to, fallen leaves of bamboo leaves, ginkgo leaves or willow leaves;
further, the functional material of step S1 includes, but is not limited to, magnesium aluminum layered double hydroxide (i.e. Mg-Al-LDH), calcined magnesium aluminum layered double hydroxide (i.e. Mg-Al-CLDH), metal organic framework compound or covalent organic framework porous crystalline material;
still further, the metal organic framework compounds include, but are not limited to, ZIF-67, mg-MOF-74, or HKUST-1;
further, covalent organic framework porous crystalline materials include, but are not limited to, COF-5, CAU-17, or JUC-5;
further, the preparation method of the Mg-Al-LDH comprises the following steps: mixing AlCl 3 ·6H 2 O and MgCl 2 ·6H 2 O is mixed in deionized water to form a molar ratio Mg: a solution in which Al is 3; next, the resulting solution was added to Na 2 CO 3 And NaOH in a mass ratio of 2; then, transferring the obtained suspension into a polytetrafluoroethylene-lined stainless steel autoclave with a proper volume, sealing, and then reacting for 6-10 hours at 150-200 ℃; thirdly, carrying out centrifugal washing on the reaction system for three times by using deionized water to remove redundant impurities, and drying for 10-16 h at 50-70 ℃ to obtain Mg-Al-LDH; preferably, the reaction is carried out for 8 hours at 180 ℃; preferably, drying is carried out for 12 hours at 60 ℃;
further, the preparation method of Mg-Al-CLDH comprises the following steps: calcining commercially available Mg-Al-LDH or Mg-Al-LDH prepared by the method at 350-600 ℃ for 3-6 h to obtain the functional material Mg-Al-CLDH; preferably, the calcination temperature is 450 ℃; preferably, the calcination time is 4h;
further, the weight ratio of the biomass fiber waste powder to the functional material is 1:2 to 10; further preferably, the weight ratio of the biomass fiber waste powder to the functional material is 1:9;
further, the particle size of the biomass fiber waste powder in the step S1 is 30-200 meshes; preferably, the particle size of the biomass fiber waste powder in the step S1 is 100 meshes;
further, the aqueous solvent in step S1 is distilled water, deionized water or an alcohol-containing aqueous solution; furthermore, the alcohol is any one or more of methanol, ethanol, propanol and butanol;
further, the concentration of the biomass fiber waste in the suspension in the step S1 is 2-10 mg/mL;
further, the homogenizing device in the step S2 is any one or more of a pulping machine, a colloid mill and a ball mill;
furthermore, the rotation speed of the homogenizing using equipment in the step S2 is 200-800 r/min; preferably 400r/min;
furthermore, the homogenization time in the step S2 is 3-8 h; preferably 4h;
furthermore, the times in the step S2 are 1 to 6 times; preferably 3 times;
further, the freezing mode in the step S3 is liquid nitrogen freezing or low-temperature freezer freezing;
furthermore, the freezing temperature of the low-temperature refrigerator is-10 to-50 ℃, and the freezing time is 5 to 48 hours; the preferable temperature is-40 ℃, and the freezing time is 24h;
further, the drying method in the step S3 is any one or more of critical point drying, freeze drying and supercritical drying;
further, the drying time of the step S3 is 6-60 h; preferably, the drying time is 48h.
Advantageous effects
The invention provides a large-scale preparation method of biomass-based composite aerogel with excellent mechanical properties, which has the following advantages:
(1) The raw materials adopted by the invention are biomass-based waste materials, such as waste paper (board), fallen leaves, weeds, seaweed and the like, the raw materials are rich in source, the waste is changed into valuable, and the environment-friendly requirement is met;
(2) The preparation method adopted by the invention is a full-component self-assembly method, the preparation process is very simple, no chemical reagent with serious pollution is introduced, the defects of complex process, serious energy consumption/pollution, high cost, low efficiency, use of a large amount of chemical reagents and the like in the assembly process of bottom-up in the traditional method for preparing the cellulose-based composite aerogel are avoided, and the large-scale production is facilitated.
(3) According to the biomass-based composite aerogel prepared by the invention, due to strong rubber grinding force, the biomass-converted polyhydroxy microfibers and the interface of a functional material (such as Mg-Al-LDH, mg-Al-CLDH, a metal organic framework compound or a covalent organic framework porous crystal material) are strongly interacted, and the polyhydroxy microfibers and the functional material are densely stacked with each other to form a core-shell structure taking the biomass microfibers as a core and the functional material as a shell. Through continuous mechanical load distribution between the core and the shell, after freeze drying, the unique structure enables the composite aerogel to have excellent mechanical properties.
(4) In the freeze drying process of the biomass-based composite aerogel prepared by the invention, the nucleation and directional growth of ice crystals enable the composite aerogel to have a continuously interconnected three-dimensional honeycomb structure, and the composite aerogel has low density and high porosity. The weight is light, the specific surface area is large, and the adsorption capacity and the anti-swelling capacity are obviously improved. The method has great application prospect in the aspects of gas storage, heavy metal adsorption, organic dye adsorption, toxic gas purification, air filtration and the like.
(5) According to the invention, different functional materials, such as magnesium-aluminum layered double hydroxide, metal organic framework compounds or covalent organic framework porous crystal materials, are added according to actual requirements, so that the corresponding functional biomass-based composite aerogel can be prepared.
Drawings
FIG. 1 is a low-magnification SEM image of a biomass-based composite aerogel prepared in example 4;
FIG. 2 is a high-magnification SEM image of a biomass-based composite aerogel prepared in example 4;
fig. 3 is a graph comparing the compression resistance tests for different biomass-based composite aerogel samples: (a) the biomass-based composite aerogel prepared in example 4; (b) the biomass-based composite aerogel prepared in comparative example 1; (c) The pure biomass-based cellulose aerogel prepared in comparative example 2;
FIG. 4 shows different material pairs CrO 4 2- Wherein "Cellulose", "Mg-Al-CLDH", "C-7, C-8, C-9, C-10" respectively denote the pure biomass-based Cellulose aerogel prepared in comparative example 2, the Mg-Al-CLDH functional material obtained in example 4 by 1) calcination, and the biomass-based composite aerogel prepared in examples 8, 9, 4, 10 of the present invention vs. CrO 4 2- The adsorption performance of (a) is compared in bar graphs.
Detailed Description
All of the starting materials used in the examples of the present invention are commercially available or can be prepared by themselves (e.g., the functional materials Mg-Al-LDH or Mg-Al-CLDH of examples 1 and 4).
Example 1:
1) The preparation method of the functional material Mg-Al-LDH comprises the following steps:
firstly, the AlCl is added 3 ·6H 2 O and MgCl 2 ·6H 2 O is mixed in deionized water to form a mixture with a molar ratio of Mg: a solution with Al being 3; next, the resulting solution was added to Na 2 CO 3 And NaOH in a mass ratio of 2; subsequently, the obtained suspension was transferred to a polytetrafluoroethylene-lined stainless steel autoclave of an appropriate volume, sealed, and then reacted at 180 ℃ for 8 hours; thirdly, centrifugal washing is carried out on the reaction system for three times by deionized water, redundant impurities are removed, and drying is carried out for 12 hours at the temperature of 60 ℃, so as to obtain Mg-Al-LDH.
2) A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 3g of waste paper powder of 100 meshes with 27g of functional material Mg-Al-LDH, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2Mg/mL; s2: homogenizing the suspension obtained in the step S1 in a colloid mill, wherein the rotating speed of the colloid mill is 400r/min, the running time is 4h, and the colloid mill frequency is 3 times to obtain a homogenized mixture; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then placing the urine cup into a low temperature of-40 ℃ for freezing for 24 hours, and then transferring the urine cup into a freeze dryer for drying for 48 hours to obtain the biomass-based composite aerogel.
Example 2:
1) The preparation method of the functional material is the same as that of example 1;
2) A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 3g of 100-mesh deciduous leaf (bamboo leaf) powder and 6g of functional material Mg-Al-LDH, and then adding 1.5L of distilled water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2Mg/mL; s2: homogenizing the suspension obtained in the step S1 in a ball mill at a glue milling speed of 200r/min for 8h for 5 times to obtain a homogenized mixed solution; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then freezing at the low temperature of-20 ℃ for 48 hours, and transferring to a freeze dryer for drying for 60 hours to obtain the biomass-based composite aerogel.
Example 3:
1) The functional material was prepared as in example 1;
2) A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 15g of 100-mesh deciduous leaf (bamboo leaf) powder and 90g of functional material Mg-Al-LDH, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 10Mg/mL; s2: homogenizing the suspension obtained in the step S1 in a pulping machine, wherein the rotational speed of a rubber mill is 800r/min, the running time is 3h, and the number of times of the rubber mill is 2, so as to obtain a homogenized mixture; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then freezing at the low temperature of-50 ℃ for 8 hours, and transferring to a freeze dryer for drying for 24 hours to obtain the biomass-based composite aerogel.
Example 4:
1) The preparation method of the functional material Mg-Al-CLDH comprises the following steps:
firstly, mg-Al-LDH is obtained through the embodiment 1, and then the obtained Mg-Al-LDH is placed in a muffle furnace and calcined for 4 hours at the high temperature of 450 ℃ to obtain the functional material Mg-Al-CLDH.
2) Preparing the biomass-based composite aerogel: different from the functional material prepared in the step 1), the biomass-based composite aerogel is prepared according to the step 1.
3) And (3) performance testing:
FIG. 1 is a low-magnification SEM image of a Mg-Al-CLDH/biomass-based composite aerogel prepared in example 4 of the present invention. It can be seen from fig. 1 that Mg-Al-CLDH/biomass-based composite aerogel in which Mg-Al-CLDH is entangled with biomass fibers, exhibits a continuous interconnected three-dimensional honeycomb structure with high porosity.
FIG. 2 is a high-magnification SEM picture of the Mg-Al-CLDH/biomass-based composite aerogel prepared in example 4 of the present invention. High resolution scanning electron microscopy revealed a core-core structure of Mg-Al-CLDH and biomass fibers stacked on top of each other with biomass microfibers as the inner core and Mg-Al-CLDH as the outer shell. Through continuous mechanical load distribution between the core and the shell, the unique structure can enable the composite aerogel to have excellent mechanical properties.
FIG. 3 is a graph comparing the compression resistance test of a sample prepared in example 4 of the present invention and a comparative sample, wherein (a) is Mg-Al-CLDH/biomass-based composite aerogel prepared in example 4 by mechanical colloid milling; (b) is comparative example 1: preparing Mg-Al-CLDH/biomass-based composite aerogel without mechanical colloid milling; (c) is comparative example 2: pure biomass aerogel without added Mg-Al-CLDH prepared by mechanical colloid milling. Obviously, the Mg-Al-CLDH/biomass-based composite aerogel prepared by mechanical colloid milling has better compression resistance.
Example 5
1) The preparation of the functional material Mg-Al-LDH is the same as that in example 1.
2) A preparation method of biomass-based composite aerogel comprises the following steps:
s1: mixing 3g, 100 mesh straw powder and functional material with 27g functional materialUniformly mixing materials Mg-Al-LDH, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2Mg/mL; s2: homogenizing the suspension obtained in the step S1 in a colloid mill, wherein the rotating speed of the colloid mill is 400r/min, the running time is 4h, and the colloid mill frequency is 3 times to obtain a homogenized mixture; s3: transferring the homogenized mixed solution obtained in S2 into a 50ml urine cup, freezing with liquid nitrogen for 12h, and transferring to CO 2 And drying in a supercritical dryer for 48 hours to obtain the biomass-based composite aerogel.
Example 6
A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 3g of waste paper powder of 100 meshes with 27g of commercially available functional material metal organic framework ZIF-67, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2mg/mL; s2: homogenizing the suspension obtained in the step S1 in a colloid mill, wherein the rotating speed of the colloid mill is 600r/min, the running time is 4h, and the colloid mill frequency is 3 times to obtain a homogenized mixture; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then placing the urine cup into a low temperature of-40 ℃ for freezing for 24 hours, and then transferring the urine cup into a freeze dryer for drying for 48 hours to obtain the biomass-based composite aerogel.
Example 7
A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 3g of waste paper powder of 100 meshes with 27g of a commercially available functional material covalent organic framework CAU-17, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2mg/mL; s2: homogenizing the suspension obtained in the step S1 in a colloid mill, wherein the rotating speed of the colloid mill is 600r/min, the running time is 4h, and the colloid mill frequency is 3 times to obtain a homogenized mixture; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then freezing at the low temperature of-40 ℃ for 24 hours, and transferring to a freeze dryer for drying for 48 hours to obtain the biomass-based composite aerogel.
Example 8:
1) The preparation method of the functional material Mg-Al-CLDH is the same as that of the embodiment 4;
2) A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 3g of waste paper powder of 100 meshes with 21g of functional material Mg-Al-LDH, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2Mg/mL; s2: homogenizing the suspension obtained in the step S1 in a colloid mill, wherein the rotation speed of the colloid mill is 400r/min, the running time is 4h, and the times of the colloid mill are 3 times to obtain a homogenized mixture; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then freezing at the low temperature of-40 ℃ for 24 hours, and transferring to a freeze dryer for drying for 48 hours to obtain the biomass-based composite aerogel.
Example 9:
1) The preparation method of the functional material Mg-Al-CLDH is the same as that of the embodiment 4;
2) A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 3g of waste paper powder of 100 meshes with 24g of functional material Mg-Al-CLDH, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2Mg/mL; s2: homogenizing the suspension obtained in the step S1 in a colloid mill, wherein the rotating speed of the colloid mill is 400r/min, the running time is 4h, and the colloid mill frequency is 3 times to obtain a homogenized mixture; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then placing the urine cup into a low temperature of-40 ℃ for freezing for 24 hours, and then transferring the urine cup into a freeze dryer for drying for 48 hours to obtain the biomass-based composite aerogel.
Example 10
1) The preparation method of the functional material Mg-Al-CLDH is the same as that of the embodiment 4;
2) A preparation method of biomass-based composite aerogel comprises the following steps:
s1: uniformly mixing 3g of waste paper powder of 100 meshes with 30g of functional material Mg-Al-CLDH, and then adding 1.5L of deionized water into the mixture to form a suspension, so that the concentration of the biomass fiber waste in the suspension is 2Mg/mL; s2: homogenizing the suspension obtained in the step S1 in a colloid mill, wherein the rotating speed of the colloid mill is 400r/min, the running time is 4h, and the colloid mill frequency is 3 times to obtain a homogenized mixture; s3: and (3) transferring the homogenized mixed solution obtained in the step (S2) into a 50ml urine cup, then placing the urine cup into a low temperature of-40 ℃ for freezing for 24 hours, and then transferring the urine cup into a freeze dryer for drying for 48 hours to obtain the biomass-based composite aerogel.
Comparative example 1:
1) The preparation method of the functional material Mg-Al-CLDH is the same as that of the embodiment 4;
a preparation method of biomass-based composite aerogel comprises the following steps: firstly, 200mg of waste paper scraps are added into 100ml of aqueous solution to swell overnight; then, ultrasonic crushing is carried out under an ultrasonic cell crusher of 600W until a uniform pulp solution is formed; subsequently, 1800Mg of functional material Mg-Al-LDH is added into the solution, and is intensively stirred for 8 hours at the rotating speed of 800r/min to obtain a uniform mixed solution; then, freezing the obtained mixed solution at the low temperature of-20 ℃ for 18h; and finally, transferring the frozen block into a low-temperature freeze dryer to be frozen and dried for 48 hours at the temperature of minus 50 ℃ to obtain the freeze-dried block.
Comparative example 2:
a preparation method of biomass-based composite aerogel comprises the following steps: firstly, 200mg of wastepaper is added into 100ml of aqueous solution; then, transferring the mixed solution into a ball mill for high-speed ball milling for 4 hours at the speed of 400r/min to obtain homogeneous waste paper pulp; subsequently, freezing the obtained slurry at the low temperature of-20 ℃ for 18h; and finally, transferring the frozen block into a low-temperature freeze dryer to be frozen and dried for 48 hours at the temperature of minus 50 ℃ to obtain the freeze-dried block.
Examples of the experiments
FIG. 4 depicts different material pairs CrO 4 2- Wherein "Cellulose", "Mg-Al-CLDH", "C-7, C-8, C-9, C-10" respectively represent the Mg-Al-CLDH functional material prepared in comparative example 2 (pure biomass-based Cellulose aerogel without addition of the functional material Mg-Al-CLDH), 1) of example 4, and examples 8, and 10 of the present invention,9. 4, 10, preparing the obtained biomass-based composite aerogel to CrO 4 2- The adsorption performance of (A) is compared with that of (B), and it is obvious that for CrO 4 2- The adsorption performance of the composite aerogel of the embodiment of the invention (examples 8, 9, 4 and 10) > Mg-Al-CLDH functional material > pure biomass-based cellulose aerogel, and the adsorption performance of the composite aerogel is gradually enhanced as the mass ratio of the raw biomass fiber waste to the Mg-Al-CLDH functional material is smaller, and the adsorption performance is the best when the mass ratio of the raw biomass fiber waste to the Mg-Al-CLDH functional material is 1.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. The preparation method of the biomass-based composite aerogel is characterized by comprising the following steps
The method comprises the following steps:
s1: mixing plant fiber waste powder and functional materials in a weight ratio of 1: 0.1-12, then adding an aqueous solvent into the mixture to form a suspension, so that the concentration of the vegetable fiber waste in the suspension is 0.1-20 mg/mL;
the plant fiber waste is selected from one or more of waste paper, fallen leaves, straws, bagasse, weeds and waste seaweed, the particle size of the plant fiber waste powder is 30-200 meshes,
the functional material is magnesium-aluminum layered double hydroxide (namely Mg-Al-LDH), or calcined magnesium-aluminum layered double hydroxide (namely Mg-Al-CLDH), a metal organic framework compound or a covalent organic framework porous crystal material;
the aqueous solvent is distilled water, deionized water or an alcohol-containing aqueous solution,
the preparation method of the Mg-Al-LDH comprises the following steps: mixing AlCl 3 ·6H 2 O and MgCl 2 ·6H 2 O is mixed in deionized water to form a mixture with a molar ratio of Mg: a solution with Al being 3; next, the resulting solution was added to Na 2 CO 3 And NaOH in an alkaline aqueous solution with the mass ratio of 2; then, transferring the obtained suspension into a polytetrafluoroethylene-lined stainless steel autoclave with a proper volume, sealing, and then reacting for 6-10 hours at 150-200 ℃; thirdly, centrifugal washing is carried out on the reaction system for three times by deionized water to remove redundant impurities, drying is carried out for 10-16 h at the temperature of 50-70 ℃ to obtain Mg-Al-LDH,
the preparation method of the Mg-Al-CLDH comprises the following steps: placing commercially available Mg-Al-LDH or Mg-Al-LDH prepared by adopting the preparation method of the Mg-Al-LDH at the temperature of 350-600 ℃ for high-temperature calcination for 3-6 h to obtain the functional material Mg-Al-CLDH;
s2: homogenizing the stirring liquid obtained in the step S1 to obtain a homogenized mixed liquid, wherein the equipment used for homogenizing is any one or more of a pulping machine, a colloid mill and a ball mill, the rotating speed of the equipment used for homogenizing is 200-800 r/min, the homogenizing time is 3-8 h, and the homogenizing times are 1-6 times;
s3: freeze-drying the homogeneous mixed solution obtained in the step S2 to obtain the biomass-based composite
And the aerogel is frozen by a low-temperature freezer, the temperature is-10 to-50 ℃, the freezing time is 5 to 48 hours, the drying method is any one or more of critical point drying, freeze drying and supercritical drying, and the drying time in the step S3 is 6 to 60 hours.
2. The method for preparing the biomass-based composite aerogel according to claim 1, wherein the fallen leaves in step S1 are fallen leaves of bamboo leaves, ginkgo leaves or willow leaves, the metal organic framework compound comprises but is not limited to ZIF-67, mg-MOF-74 or HKUST-1, and the covalent organic framework porous crystal material comprises but is not limited to COF-5, CAU-17 or JUC-5.
3. The preparation method of the biomass-based composite aerogel according to claim 1, wherein the weight ratio of the biomass fiber waste powder to the functional material is 1:2 to 10.
4. The method for preparing the biomass-based composite aerogel according to claim 1, wherein in the aqueous solution containing alcohol in step S1, the alcohol is any one or more of methanol, ethanol, propanol and butanol.
5. The preparation method of the biomass-based composite aerogel according to claim 1, wherein the concentration of the biomass fiber waste in the suspension in the step S1 is 2-10 mg/mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011393756.9A CN112657437B (en) | 2020-12-03 | 2020-12-03 | Biomass-based composite aerogel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011393756.9A CN112657437B (en) | 2020-12-03 | 2020-12-03 | Biomass-based composite aerogel and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112657437A CN112657437A (en) | 2021-04-16 |
| CN112657437B true CN112657437B (en) | 2022-11-25 |
Family
ID=75400908
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011393756.9A Active CN112657437B (en) | 2020-12-03 | 2020-12-03 | Biomass-based composite aerogel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112657437B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248775B (en) * | 2021-05-21 | 2022-07-05 | 苏州因安特新材料科技有限公司 | Bacterial cellulose-silicon dioxide P-COF aerogel and preparation method and application thereof |
| CN113617302B (en) * | 2021-08-24 | 2023-03-14 | 广东工业大学 | Cellulose/magnesium-aluminum layered bimetal oxide aerogel, and preparation method and application thereof |
| CN114247388B (en) * | 2021-11-12 | 2023-09-22 | 巢湖学院 | Preparation method of zinc aluminate and magnesium aluminate aerogel with high specific surface area |
| CN114259989A (en) * | 2022-01-07 | 2022-04-01 | 云南中烟工业有限责任公司 | Biological carbon aerogel loaded hydrotalcite material, and synthesis method and application thereof |
| CN115193417B (en) * | 2022-06-08 | 2023-11-03 | 苏州科技大学 | Lamellar covalent organic framework aerogel and preparation method and application thereof |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566673B (en) * | 2015-12-17 | 2018-11-02 | 中国科学院兰州化学物理研究所 | A kind of preparation method of the elastic aeroge of multifunctional fibre element |
| CN106824080B (en) * | 2017-03-03 | 2019-11-12 | 中国科学院理化技术研究所 | High-adsorption-performance carbon aerogel and preparation method and application thereof |
| CN107376880B (en) * | 2017-07-27 | 2019-11-15 | 浙江理工大学 | Three-dimensional porous ZIF-8/ aeroge of a kind of cellulose base for adsorbing heavy metal ion and preparation method thereof |
| CN108623833B (en) * | 2018-03-21 | 2020-09-15 | 武汉理工大学 | Preparation method of multifunctional composite aerogel material |
| CN108690223A (en) * | 2018-04-26 | 2018-10-23 | 浙江理工大学 | A kind of layered double hydroxide/fibrination hole composite material and preparation method thereof |
| CN109433024B (en) * | 2018-10-30 | 2021-06-18 | 武汉纺织大学 | Membrane material or aerogel material containing metal organic framework nanofiber as well as preparation method and application thereof |
| CN111518309B (en) * | 2020-06-04 | 2021-04-09 | 东北林业大学 | Biomass nanocellulose/polypyrrole composite aerogel and preparation method and application thereof |
-
2020
- 2020-12-03 CN CN202011393756.9A patent/CN112657437B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112657437A (en) | 2021-04-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112657437B (en) | Biomass-based composite aerogel and preparation method thereof | |
| Feng et al. | Extraction and preparation of cellulose nanocrystals from dealginate kelp residue: structures and morphological characterization | |
| Zhang et al. | Preparation of spherical nanocellulose from waste paper by aqueous NaOH/thiourea | |
| US20180291266A1 (en) | A carbon quantum dot synthesizing method and its application of modifying functional water purification material | |
| Song et al. | Synthesis of sustainable lignin-derived mesoporous carbon for supercapacitors using a nano-sized MgO template coupled with Pluronic F127 | |
| CN107840979B (en) | A kind of preparation method of crosslinking nano cellulose/hexagonal boron nitride nanosheet composite membrane | |
| Al Rai et al. | High-performance nanostructured bio-based carbon electrodes for energy storage applications | |
| CN106179200A (en) | A kind of preparation method and applications of magnetic porous carbon based on native cellulose | |
| CN113398771B (en) | Multi-component bacterial cellulose composite filter membrane and preparation method and application thereof | |
| CN114146679B (en) | Millimeter-level nitrogen-doped porous carbon sphere and preparation and application thereof | |
| US20230235136A1 (en) | Method of making cellulose bioplastics | |
| Suryanto et al. | Nano fibrillation of Bacterial Cellulose Using High-Pressure Homogenization and Its Films Characteristics | |
| CN103342826A (en) | Preparation method of chitin nano-fiber/montmorillonite composite membrane material | |
| Wu et al. | Study on the preparation and adsorption property of polyvinyl alcohol/cellulose nanocrystal/graphene composite aerogels (PCGAs) | |
| Carrillo-Varela et al. | Methylene blue adsorption onto hydrogels made from different Eucalyptus dissolving pulps | |
| CN110526228A (en) | The preparation method of one type petal-shaped carbon nanosheet | |
| CN115155520A (en) | Phosphoric acid modified sawdust hydrothermal carbon and application thereof | |
| CN109942880A (en) | A kind of preparation method of nano-cellulose base porous compound material | |
| CN109187462A (en) | A kind of solid phase nano composite membrane of field portable Visual retrieval heavy metal Hg ion and its preparation and application | |
| CN105460916A (en) | Preparation method of hollow carbon nanospheres-assembled mesoporous carbon fiber material | |
| CN1317193C (en) | Method for microwave preparation of titania nanometer tube | |
| CN113292747B (en) | Preparation method and application of biomass lignin nanoshell | |
| CN106633215A (en) | Sulfonated beta-cyclodextrin-LDH complex and synthesis method thereof | |
| CN112194129B (en) | Method for preparing straw-based ordered porous carbon material through hydrothermal-assisted chemical activation and application | |
| CN108190906A (en) | A kind of method that ordered mesoporous material SBA-16 is prepared using attapulgite |
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 |