CN111961222A - Method for preparing gel elastomer based on wood liquefied product and gel elastomer - Google Patents
Method for preparing gel elastomer based on wood liquefied product and gel elastomer Download PDFInfo
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- CN111961222A CN111961222A CN202010679815.2A CN202010679815A CN111961222A CN 111961222 A CN111961222 A CN 111961222A CN 202010679815 A CN202010679815 A CN 202010679815A CN 111961222 A CN111961222 A CN 111961222A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2220/00—Compositions for preparing gels other than hydrogels, aerogels and xerogels
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Abstract
The invention provides a preparation method of a gel elastomer based on wood liquefaction products, in particular to a gel elastomer prepared by using biomass resource liquefaction products such as wood and the like, and also relates to a gel elasticity regulation and control technology in the process of preparing the gel elastomer. The gel elastomer prepared by the biomass material liquefied substance by adopting the technology of the invention has the compression rebound rate of 50-90%. In addition, the invention utilizes the precursor for preparing the wood gel elastomer and utilizes the polymerization reaction of the liquefied substance and the aldehyde to prepare the highly crosslinked gel elastomer, thereby fully utilizing wood resources. Meanwhile, the technology takes biomass resources as the raw material of the gel elastomer, reduces the production cost and has strong competitiveness in the market.
Description
Technical Field
The invention provides a preparation method of a gel elastomer based on a wood liquefied product, and particularly relates to a method for preparing a gel elastomer based on a wood liquefied product and the gel elastomer.
Background
Aerogels are superporous structures obtained by removing a liquid-phase medium from a wet gel while keeping the volume as much as possible without shrinking. Aerogel materials have the characteristics of large specific surface area, high porosity, low density, extremely low thermal conductivity and the like, and show great application potential in many aspects such as separation materials, heat-insulating materials, high-energy physics, high-efficiency catalysts and catalyst carriers, gas and biosensors, low-dielectric-constant materials and electrode materials, and are called as 'magic materials which will change the world'. Later, aerogels were found to have high compressive strength under large strains, which provides a theoretical basis for aerogels as cushioning packaging materials. However, most of the precursors of organic aerogels are from the petroleum industry and prepared through a sol-gel process, and most of the raw materials are harmful to human bodies and the environment and difficult to store on a large scale, so people always explore the raw materials which are rich in sources, low in price and environment-friendly to prepare the organic aerogels and the carbon aerogels. Cellulose is usually extracted from woody plants, which, however, contain, in addition to cellulose, constituents such as hemicellulose, lignin and some minerals. Therefore, the cellulose aerogel has insufficient resource utilization in the preparation process, has the resource waste phenomenon and can not meet the large-scale practical application requirements. Therefore, the preparation of aerogel with good compression resilience performance by using green and cheap raw materials as precursors has received much attention.
Wood is a renewable biomass raw material, and meanwhile, as an important technical means for efficient value-added utilization of wood, a liquefaction technology is continuously deepened and developed. Wood is a natural, renewable resource, and its utilization method is attracting increasing attention. The wood contains a large number of active groups, and the liquefaction of the woody biomass resources is to convert main components such as cellulose, hemicellulose, lignin and the like in the biomass into substances with certain chemical reaction activity and liquid fluidity by utilizing a physical method, a thermochemical method, a biological conversion method and the like. The product can be used for manufacturing adhesives, polyurethane foam plastics, fibers, carbon fibers and other new high molecular substances, particularly high molecular substances with biodegradability, greatly expands the utilization and recovery field of wood resources, and has wider and wider application prospect.
In consideration of the properties of the aerogel and the development of the liquefaction technology, the invention takes biomass resources such as wood and the like as raw materials, takes the liquefied substance of the raw materials as a precursor for preparing the wood gel elastomer, and generates highly crosslinked gel through the sol-gel process by utilizing the polymerization reaction of the liquefied substance and aldehyde, thereby fully utilizing the wood resources. The wood gel elastomer makes full use of raw materials, simultaneously utilizes the excellent compression resilience as a buffering packaging material, is expected to replace the waste of excessive paper (such as corrugated boards) and plastic (such as foamed plastics) and other buffering packaging materials in the transportation of large instruments, precision instruments and the like, and relieves the environmental pollution problems of difficult degradation and the like caused by the buffering packaging material of plastic products.
Disclosure of Invention
The invention aims to provide a gel elastomer prepared by using biomass liquefied materials such as wood, and the main raw materials of the gel elastomer are mainly biomass resources such as wood.
The invention firstly liquefies the biomass materials such as wood to obtain a wood liquefied substance precursor, then adds a synthesis agent, a catalytic cross-linking agent and a concentration regulator to prepare a uniformly mixed solution, and obtains the gel elastomer with adjustable elasticity by a sol-gel method.
The technical scheme of the invention is as follows:
a preparation method of a gel elastomer based on wood liquefaction comprises the following steps:
1) crushing a biomass raw material into powder, adding phenol, and carrying out liquefaction reaction by using phosphoric acid as a catalyst to obtain a liquefied substance;
2) respectively adding a catalytic cross-linking agent and a concentration regulator according to the weight of 3-7% and 46.8-93.6% of the liquefied substance, and stirring at a constant speed (750rpm) at 30-40 ℃ for 40-50 min to obtain a completely dissolved mixed solution;
3) adding a synthetic agent accounting for 48.9-81.5% of the weight of the liquefied substance into the mixed solution, and performing ultrasonic dispersion for 30-40 min to obtain a reaction solution with uniform dispersion.
4) And putting the uniformly dispersed solution into a sealed glass reaction bottle, placing the glass reaction bottle in a water bath kettle preheated to 85-90 ℃ for sol-gel reaction for 4-10 days, taking out the obtained wet gel, washing, and freeze-drying to obtain the gel elastomer.
The weight of the added phenol is 4-7 times of that of the raw materials.
The adding amount of the phosphoric acid is 6 to 8 percent of the weight of the phenol, and the concentration of the phosphoric acid is 85 percent.
The liquefaction reaction is carried out for 2.5-3 hours under the condition of stirring at 150-160 ℃ under normal pressure.
The synthetic agent is formaldehyde.
The catalytic cross-linking agent is hexamethylene tetramine.
The concentration regulator is absolute ethyl alcohol.
The biomass raw materials are wood, bamboo and straw; the biomass raw material is crushed, and the fineness of the raw material powder is 20-80 meshes.
The elasticity control method of the gel elastomer comprises the steps of adding a synthetic agent accounting for 48.9-81.5% of the weight of a liquefied material, a catalytic cross-linking agent accounting for 3-7% of the weight of the liquefied material and a concentration regulator accounting for 46.8-156% of the weight of the liquefied material into a wood liquefied material, and carrying out sol-gel for 4-10 days at the temperature of 85-90 ℃ to obtain the gel elastomer with different elasticity.
The gel elastomer prepared based on the method has the following characteristics:
density: 1403.31-1601.55 (mg/cm)3)；
Modulus of elasticity: 0.27 to 10.14 (MPa);
compression rebound resilience: 50-90 (%).
Has the advantages that:
according to the characteristics of the biomass material, the inventor applies a liquefaction technology and a sol-gel technology, and through a large amount of research and experiments, the gel elastomer prepared by the biomass material liquefaction product by adopting the technology can achieve 50-90% of compression rebound rate, and the performance of the gel elastomer is higher than that of the existing product. In addition, the invention prepares the gel elastomer with different resilience performance by controlling the ratio of each component, the gel condition and other influencing factors. The technology takes biomass resources as raw materials of the gel elastomer, reduces the production cost and has strong competitiveness in the market.
Drawings
FIG. 1: liquefying wood;
FIG. 2: a gel elastomer.
Detailed Description
The wood liquefaction product is prepared by the following method:
1) crushing biomass raw materials such as wood and the like into powder, and drying for later use;
2) adding phenol, and liquefying with phosphoric acid as catalyst to obtain liquefied substance;
through years of research and experiments, researchers of the invention find that the phosphoric acid has the best catalytic performance in the inorganic acid catalyst, so that the phosphoric acid is adopted to liquefy biomass raw materials such as wood, and the method specifically comprises the following steps: the method comprises the steps of crushing a wood biomass raw material into powder, adding phenol which is 4-7 times of the weight of the raw material and a phosphoric acid catalyst which is 6-8% of the weight of the added phenol and has a concentration of 85%, and stirring at the normal pressure and at the temperature of 150-160 ℃ for reaction for 2.5-3 hours to obtain a liquefied substance. The liquefaction process can be carried out in a conventional liquefaction plant.
The biomass raw materials such as the selectable wood can be wood, bamboo, straw, plant fiber and the like. The fineness of the raw material powder is preferably 20-80 meshes (the aperture of a mesh screen is 0.9-0.18 mm), and the biomass raw material can be crushed in a crusher.
The liquefaction treatment can be carried out in a conventional liquefaction apparatus.
Adding a concentration regulator, a catalytic cross-linking agent and a synthesis agent into the obtained wood liquefied substance, wherein the catalytic cross-linking agent and the concentration regulator are respectively added according to the weight of 3-7% and 46.8-93.6% of the liquefied substance, stirring until the catalytic cross-linking agent and the concentration regulator are completely dissolved, adding the synthesis agent according to the weight of 48.9-81.5% of the liquefied substance, and performing ultrasonic dispersion to obtain a uniformly mixed solution.
Further, the invention prepares the gel elastomer by the uniformly mixed solution prepared by the method of sol-gel, and the specific method comprises the following steps: and pouring the mixed solution into a glass reaction bottle, completely sealing, putting into a water bath kettle preheated to 85-90 ℃, carrying out gel reaction for 4-10 days, taking out the obtained wet gel, washing (absolute ethyl alcohol and deionized water), and carrying out freeze drying for 24 hours to obtain the gel elastomer.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Pulverizing fir into 80 mesh powder (mesh screen aperture 0.18mm), adding the wood powder, phenol 4 times of the weight of wood and catalyst phosphoric acid (phosphoric acid concentration 85%) in an amount of 8% of the amount of phenol added into a three-port glass bottle, placing in an oil bath preheated to 160 ℃, installing a condenser, starting a stirring device (rotating speed 1058rpm) for liquefaction, and obtaining a liquefied substance after the liquefaction time is 2.5 hours. (see FIG. 1)
Adding absolute ethanol accounting for 46.8 percent of the weight of the wood liquefied substance and hexamethylene tetramine accounting for 3 percent of the weight of the wood liquefied substance into the wood liquefied substance, and stirring for 40min at a constant speed (750rpm) at 40 ℃ to obtain a completely dissolved mixed solution.
Adding formaldehyde into the completely dissolved mixed solution according to 48.9% of the weight of the liquefied substance, and performing ultrasonic dispersion (35 ℃, 30min) to obtain a uniformly dispersed solution.
Pouring the uniformly dispersed solution into a glass reaction bottle (high temperature resistant), completely sealing, and placing into a water bath kettle preheated to 85 ℃.
And after 7 days, taking out the wet gel, sequentially washing the wet gel with 10 times of anhydrous ethanol and deionized water by volume of the gel elastomer for 5 times respectively, then placing the wet gel in a freeze dryer for freezing for 12 hours at (-51 ℃) and drying for 24 hours to obtain the gel elastomer. (see FIG. 2)
Density of the gel elastomer prepared: 1551.58mg/cm3(ii) a Modulus of elasticity: 0.65 MPa; the rebound resilience: 80 percent.
Example 2
Pulverizing fir into 60 mesh powder, adding the fir powder, phenol 6 times of the weight of fir and catalyst phosphoric acid (phosphoric acid concentration is 85%) 6% of the phenol addition amount into a three-neck glass bottle, placing in an oil bath preheated to 150 ℃, installing a condenser, starting a stirring device (rotating speed 1058rpm) for liquefaction, and obtaining a liquefied substance after the liquefaction time is 3 hours. (see FIG. 1)
Adding 78% of absolute ethyl alcohol and 3% of hexamethylenetetramine into the wood liquefied substance, and stirring at a constant speed (750rpm) at 30 ℃ for 40min to obtain a completely dissolved mixed solution.
Adding formaldehyde into the completely dissolved mixed solution according to 48.9% of the weight of the liquefied substance, and performing ultrasonic dispersion (35 ℃, 30min) to obtain a uniformly dispersed solution.
Pouring the uniformly dispersed solution into a glass reaction bottle (high temperature resistant), completely sealing, and placing into a water bath kettle preheated to 90 ℃.
And after 6 days, taking out the wet gel, sequentially washing the wet gel with 10 times of anhydrous ethanol and deionized water by volume of the gel elastomer for 5 times respectively, then placing the wet gel in a freeze dryer for freezing for 12 hours at (-51 ℃) and drying for 24 hours to obtain the gel elastomer. (see FIG. 2)
Density of the gel elastomer prepared: 1458.78mg/cm3(ii) a Modulus of elasticity: 0.58 MPa; the rebound resilience: 75 percent.
Example 3
Pulverizing Chinese fir into 40 mesh powder, adding the Chinese fir powder and 5 times of phenol and catalyst phosphoric acid (phosphoric acid concentration is 85%) of the weight of the Chinese fir into a three-neck glass bottle, placing the three-neck glass bottle in an oil bath preheated to 160 ℃, installing a condenser, starting a stirring device (rotating speed of 1058rpm) for liquefaction, and obtaining a liquefied substance after the liquefaction time is 2.5 hours. (see FIG. 1)
Adding absolute ethanol accounting for 46.8 percent of the weight of the wood liquefied substance and hexamethylene tetramine accounting for 4 percent of the weight of the wood liquefied substance into the wood liquefied substance, and stirring for 50min at a constant speed (750rpm) at 40 ℃ to obtain a completely dissolved mixed solution.
Adding formaldehyde into the completely dissolved mixed solution according to 48.9% of the weight of the liquefied substance, and performing ultrasonic dispersion (35 ℃, 30min) to obtain a uniformly dispersed solution.
Pouring the uniformly dispersed solution into a glass reaction bottle (high temperature resistant), completely sealing, and placing into a water bath kettle preheated to 85 ℃.
And after 5 days, taking out the wet gel, sequentially washing the wet gel with 10 times of anhydrous ethanol and deionized water by volume of the gel elastomer for 5 times respectively, then placing the wet gel in a freeze dryer for freezing for 12 hours at (-51 ℃) and drying for 24 hours to obtain the gel elastomer. (see FIG. 2)
Density of the gel elastomer prepared: 1436.86mg/cm3(ii) a Modulus of elasticity: 6.62 MPa; the rebound resilience: and 64 percent.
Example 4
Pulverizing Chinese fir into 80 mesh powder, adding the Chinese fir powder and 5 times of phenol and 6% of catalyst phosphoric acid (phosphoric acid concentration is 85%) of the Chinese fir weight into a three-neck glass bottle, placing in an oil bath preheated to 160 ℃, installing a condenser, starting a stirring device (rotating speed 1058rpm) for liquefaction, and obtaining a liquefied substance after the liquefaction time is 2.5 hours. (see FIG. 1)
Adding absolute ethanol accounting for 46.8 percent of the weight of the wood liquefied substance and hexamethylene tetramine accounting for 5 percent of the weight of the wood liquefied substance into the wood liquefied substance, and stirring for 50min at a constant speed (750rpm) at 40 ℃ to obtain a completely dissolved mixed solution.
Adding formaldehyde into the completely dissolved mixed solution according to 48.9% of the weight of the liquefied substance, and performing ultrasonic dispersion (35 ℃, 30min) to obtain a uniformly dispersed solution.
Pouring the uniformly dispersed solution into a glass reaction bottle (high temperature resistant), completely sealing, and placing into a water bath kettle preheated to 85 ℃.
And after 4 days, taking out the wet gel, sequentially washing the wet gel with 10 times of anhydrous ethanol and deionized water by volume of the gel elastomer for 5 times respectively, then placing the wet gel in a freeze dryer for freezing for 12 hours at (-51 ℃) and drying for 24 hours to obtain the gel elastomer. (see FIG. 2)
Density of the gel elastomer prepared: 1403.31mg/cm3(ii) a Modulus of elasticity: 10.02 MPa; the rebound resilience: 59 percent.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and within the scope of the claims.
Claims (6)
1. A method for preparing a gel elastomer based on wood liquefacients is characterized in that the liquefacients and reactants of all components are prepared into uniformly dispersed solution to carry out sol-gel reaction, and the method comprises the following steps:
1) adding a concentration regulator, a catalytic cross-linking agent and a synthesis agent into the wood liquefied substance, wherein the catalytic cross-linking agent and the concentration regulator are respectively added according to the weight of 3-7% and 46.8-93.6% of the wood liquefied substance, stirring until the wood liquefied substance and the concentration regulator are completely dissolved, adding the synthesis agent according to the weight of 48.9-81.5% of the wood liquefied substance, and performing ultrasonic dispersion to obtain a uniformly mixed solution;
2) pouring the uniformly mixed solution into a sealed glass reaction container, and then putting the container into a water bath kettle at the temperature of 85-90 ℃ for gel reaction for 4-10 days;
3) and taking out the obtained wet gel, washing, and freeze-drying to obtain the gel elastomer.
2. The method as claimed in claim 1, wherein the concentration regulator in step 1) is absolute ethyl alcohol, the catalytic cross-linking agent is hexamethylenetetramine, and the synthetic agent is formaldehyde.
3. The method of claim 1, wherein the solvent to rinse the wet gel is: absolute ethyl alcohol and deionized water.
4. The method of claim 1, wherein the wet gel is rinsed by: the gel was rinsed 5 times with 10 gel elastomer volumes of absolute ethanol and deionized water, respectively.
5. The method according to claim 1, wherein the freezing temperature is-51 ℃, the freezing time is 12h, and the drying time is 24 h.
6. The wood liquefied product-based gel elastomer prepared by the method according to any one of claims 1 to 5, wherein the gel elastomer has the following specific characteristics:
density: 1403.31-1601.55 (mg/cm)3)；
Modulus of elasticity: 0.27 to 10.14 (MPa);
compression rebound resilience: 50-90 (%).
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