CN108755215B - Method for preparing nano cellulose whiskers by using peanut shells - Google Patents
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- CN108755215B CN108755215B CN201810422925.3A CN201810422925A CN108755215B CN 108755215 B CN108755215 B CN 108755215B CN 201810422925 A CN201810422925 A CN 201810422925A CN 108755215 B CN108755215 B CN 108755215B
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- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
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Abstract
The invention discloses a method for preparing nano-cellulose whiskers by using peanut shells, which is realized by the following steps in sequence: the preparation method comprises the steps of cleaning, drying and crushing waste peanut shells to obtain peanut shell powder with the particle size of less than 0.2mm, soaking the peanut shell powder in alkali liquor and EDTA solution in sequence, reacting the peanut shell powder in mixed solution of formic acid and hydrogen peroxide, decoloring the peanut shell powder by three sections of different temperature cooking processes, obtaining wet pulp with the pH value of 7 by a TEMPO oxidation method, filtering the wet pulp, and freeze-drying the wet pulp to obtain the peanut shell nanocellulose whisker. The method of the invention utilizes the waste peanut shell resource to prepare the nano-cellulose whisker, expands the range of raw materials for preparing the nano-cellulose whisker, has the advantages of environmental protection, higher degree of removing lignin, safety and capability of obtaining the cellulose whisker with high crystallinity.
Description
Technical Field
The invention relates to a preparation method of nano cellulose whiskers. In particular to a method for preparing nano cellulose whiskers by using waste peanut shells.
Background
With the development of society, resources and environment become two major topics restricting the development of human beings, and a renewable and pollution-free green new material is the direction of scientific and technical development and is the requirement of sustainable development. The cellulose is used as a natural polymer material which is most widely distributed and abundant in content in nature and has biodegradability, and has the characteristics of low price, degradability, environmental friendliness, no pollution and the like. Therefore, much attention is paid to research and development of cellulose in all countries of the world. The potential advantage of the plant fiber as the reinforcing material is more and more concerned by the market, and compared with the inorganic fiber, the plant fiber has the characteristics of small density, good mechanical and physical properties, excellent biodegradability, renewability and the like. In addition, cellulose is hydrolyzed by acid to obtain nano-cellulose whiskers (CNW) with transverse dimension within 20nm and length of about 200nm, and strength and Young's modulus are exponentially increased compared with that of common cellulose. The pure CNW has Young modulus of about 150GPa and tensile strength of about 10GPa, can replace ceramics and metal, and has great potential in the field of reinforced polymer composite materials.
At present, methods for preparing cellulose nanowhiskers mainly include an acid hydrolysis method, a biological enzyme method and a physical mechanical method, wherein the biological enzyme method and the physical mechanical method are not widely applied due to high price, need of special equipment and the like; a large amount of concentrated acid is needed in the use process of the acid hydrolysis method, so that the safety risk exists and raw material carbonization is easily caused. The oxidation method leads the glycosidic bond of the cellulose molecular chain to be catalytically broken, and destroys the amorphous area to degrade the cellulose, thus obtaining the nano-cellulose whisker.
The existing peanut planting area of Fujian province is about 10.74 ten thousand hm2(statistical data), mainly distributed in the coastal zone, is the third crop after rice and sweet potato. In recent years, the planting area of peanuts is gradually expanded year by year due to higher economic value, and the planting area is gradually expanded, so that the peanuts become one of important crops for adjusting a new planting structure. With the increasing of the peanut yield and the increasing of the total processing and utilization amount, the peanut processing always attaches importance to the kernels and neglects the utilization of byproducts such as peels, shells and the like. Except a small amount of peanut shells serving as coarse feed, a large amount of peanut shells are burnt or thrown away in white, so that the peanut shells are not fully and reasonably utilized, and resources are wasted. Therefore, research and development personnel adopt different chemical methods to extract cellulose by taking peanut shells as raw materials, but the existing chemical methods adopt a large amount of chlorine-containing compounds and concentrated sulfuric acid, so that the preparation method is not environment-friendly and has the problem of potential safety hazard in the preparation process.
Accordingly, the present inventors have made extensive studies on the above problems, and as a result, the present invention has been made.
Disclosure of Invention
The invention aims to provide a method for preparing nano cellulose whiskers by using waste peanut shells, which is environment-friendly, safe and high in efficiency, and can ensure that the cellulose whiskers have high crystallinity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing nano cellulose whiskers by using peanut shells is prepared by the following steps:
(1) cleaning and removing impurities from the waste peanut shells, drying, and crushing to obtain peanut shell powder with the particle size of less than 0.2 mm;
(2) pouring the peanut shell powder obtained in the step (1) into an alkali liquor with the mass fraction of 1% -10% to soak for 4-10 hours, immersing the peanut shell powder in the alkali liquor during soaking, cleaning with deionized water after soaking, draining, pouring the peanut shell powder into an EDTA solution with the mass fraction of 0.5% -2% after draining to soak for 4-10 hours, immersing the peanut shell powder in the EDTA solution during soaking, and cleaning with deionized water and drying to obtain treated powder;
(3) pouring the treated powder obtained in the step (2) into a mixed solution of formic acid and hydrogen peroxide, stirring for 1-2 hours at 20-30 ℃, heating to 40-60 ℃, continuing stirring for 1-2 hours, performing suction filtration, adding an equal amount of the mixed solution of formic acid and hydrogen peroxide after suction filtration, stirring for 1-2 hours at 20-30 ℃, washing with deionized water until the pH value is 7, and finally performing suction filtration and drying to obtain peanut shell cellulose;
(4) obtaining wet pulp with the pH value of 7 by using the peanut shell cellulose obtained in the step (3) through a TEMPO oxidation method; and then sequentially filtering and freeze-drying to obtain a dried substance, wherein the dried substance is the peanut shell nano cellulose whisker.
And (2) crushing the peanut shells in the step (1) by using a crusher, and sieving the crushed peanut shells with a 80-mesh sieve to obtain peanut shell powder with the particle size of less than 0.2 mm.
The alkali liquor in the step (2) is one of sodium hydroxide solution and potassium hydroxide solution.
The mixing ratio of the formic acid and the hydrogen peroxide is one of 0.5:1, 1:1 and 1:0.5, and the mixed solution of the formic acid and the hydrogen peroxide immerses the treated powder in the step (2).
The TEMPO oxidation method of the step (4) is realized by the following steps:
(a) adding the peanut shell cellulose obtained in the step (3) into a TEMPO oxidation reagent, stirring and dispersing, wherein the TEMPO oxidation reagent is prepared by dissolving TEMPO, NaBr and NaClO in Na in a dispersing way2CO3-NaHCO3The buffer solution is prepared, wherein the mass ratio of TEMPO, NaBr and NaClO is 1: 5-20: 500-1000, wherein each 1g of peanut shell cellulose needs 20-100 mL of TEMPO oxidizing reagent, and the use amount of TEMPO is 0.5-2% of the mass of the peanut shell cellulose;
(b) placing the reaction system in the step (a) in a constant-temperature water bath kettle, stirring and reacting for 2-4 hours at a constant temperature of 20-40 ℃, adding 10-50 mL of ethanol to terminate the reaction after the reaction is finished, and performing centrifugal separation to obtain oxidized slurry;
(c) and (c) acidifying the oxidation slurry obtained in the step (b) by using a 0.1-1 mol/L dilute hydrochloric acid solution for 0.5-1 hour, immersing the oxidation slurry in the dilute hydrochloric acid solution, and washing the oxidation slurry by using deionized water until the pH value is 7 after the acidification is finished.
In the step (c), the oxidized slurry is washed with deionized water and stored at 5-8 ℃ for later use.
In the step (4), the wet pulp is filtered by adopting an ultrafiltration membrane or a dialysis bag with the molecular weight cutoff of 8000-14000.
After the technical scheme is adopted, the method for preparing the nano-cellulose whiskers by using the peanut shells expands the range of raw materials for preparing the nano-cellulose whiskers by taking the waste peanut shells as the extraction source of the nano-cellulose whiskers, is favorable for accelerating the breakthrough of the limitation of the raw material source of the nano-cellulose whiskers, realizes the discharge of commercial products of the nano-cellulose whiskers as early as possible, and provides an innovative idea of utilizing the waste resources of the peanut shells at a high value; moreover, chlorine-free bleaching can be realized through a three-stage cooking mode of matching formic acid and hydrogen peroxide, the operation method is environment-friendly, and the lignin removal degree is high; in addition, the TEMPO oxidation method is mild, the problem of safe operation caused by using concentrated sulfuric acid in the traditional acid preparation method is solved, the whole preparation process is safe, and the cellulose whisker with high crystallinity can be obtained.
Drawings
FIG. 1 is a comparison of peanut shell material and peanut shell nanocellulose whiskers in accordance with the present invention;
wherein: a-peanut shell powder, B-peanut shell nano cellulose whisker
FIG. 2 is an X-ray diffraction pattern of peanut shell nanocellulose whiskers prepared in accordance with the present invention;
figure 3 is a graph comparing the X-ray diffraction patterns of the peanut shell nanocellulose whiskers of example one and the peanut shell nanocellulose whiskers of example two.
Wherein: a-X-ray diffraction of peanut shell nanocellulose whiskers, b-X-ray diffraction of peanut shell nanocellulose whiskers
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
The first embodiment is as follows:
the invention relates to a method for preparing nano-cellulose whiskers by using peanut shells, which comprises the following steps of:
(1) cleaning the waste peanut shells, removing impurities, drying, crushing by using a crusher after drying, and sieving by using a 80-mesh sieve to obtain peanut shell powder with the particle size of less than 0.2mm, wherein the peanut shell powder is shown as a picture A in figure 1;
(2) 50g of peanut shell powder obtained in the step (1) is poured into a sodium hydroxide solution with the mass fraction of 5% for soaking for 5 hours, hemicellulose and lignin are removed, the sodium hydroxide solution is ensured to be completely immersed into the peanut shell powder during soaking, deionized water is used for cleaning and draining after soaking, the sodium hydroxide solution is poured into an EDTA solution with the mass fraction of 1% for soaking for 5 hours after draining, calcium and magnesium ions are removed, the EDTA solution is ensured to be completely immersed into the peanut shell powder during soaking, and then deionized water is used for cleaning and drying, so that treated powder is obtained;
(3) and (3) pouring 10g of the treated powder obtained in the step (2) into 150mL of mixed solution, and reacting under mechanical stirring to obtain a reaction system, wherein the mixed solution is required to immerse the treated powder, the mixed solution is prepared by mixing formic acid and hydrogen peroxide, and the mixing ratio of the formic acid to the hydrogen peroxide is 1:1, heating the reaction system at a constant temperature of 25 ℃ and stirring for 1 hour, heating to 50 ℃, continuously stirring for 1 hour, then carrying out suction filtration, adding 150mL of the mixed solution again after the suction filtration, heating at 25 ℃ and continuously stirring for 1 hour, then washing with deionized water to be neutral (namely washing with deionized water until the pH value of the whole system is 7), finally carrying out suction filtration, drying and grinding to obtain powder, wherein the powder is peanut shell cellulose;
(4) taking 10g of the peanut shell cellulose obtained in the step (3), and obtaining wet pulp with the pH value of 7 by a TEMPO oxidation method; utensil for cleaning buttockIn this procedure, 0.0125g of TEMPO, 0.125g of NaBr, and 12.5g of NaClO were dissolved in Na2CO3-NaHCO3Preparing TEMPO oxidizing reagent in buffer solution, and adding Na2CO3-NaHCO3Adding buffer solution in an amount which enables a TEMPO oxidizing reagent to reach 1000mL, adding 10g of peanut shell cellulose into 1000mL of TEMPO oxidizing reagent, stirring and dispersing, then stirring at constant temperature in a constant-temperature water bath kettle at 25 ℃, stirring and reacting for 4 hours, adding 20mL of ethanol to stop the reaction after the reaction is finished, centrifuging by using a centrifugal separator after the reaction is finished to obtain oxidized pulp, acidifying the oxidized pulp by using dilute hydrochloric acid solution for 30min, wherein the function of the oxidized pulp is to convert sodium carboxylate in oxidized fibers into carboxylic acid, then washing by using deionized water to obtain wet pulp with the pH value of 7, and storing the wet pulp at 5-8 ℃ for later use; in this step, Na2CO3-NaHCO3The using amount of the buffer solution is that 20-100 mL of TEMPO oxidizing reagent is needed for every 1g of peanut shell cellulose, and the using amount of TEMPO is 0.5-2% of the mass of the peanut shell cellulose, so that the using amount of TEMPO and the using amount of TEMPO oxidizing reagent are correspondingly determined after the using amount of the peanut shell cellulose is determined, the using amounts of NaBr and NaClO are correspondingly determined after the using amount of TEMPO is determined, and finally Na is2CO3-NaHCO3The amount of buffer is also determined;
(5) filtering the wet pulp obtained in the step (4) by adopting a dialysis bag, and specifically: the wet pulp is put into a dialysis bag with the molecular weight cutoff of 8000-14000 for dialysis after centrifugal concentration (the dialysis bag needs to be treated firstly and then used, the treatment mode of the dialysis bag is that the dialysis bag is cut into small sections with the length of 10cm, then the cut small sections are put into boiling water to be boiled for 5 minutes, and then the small sections are cleaned by distilled water and then can be used), the dialysis time is 72 hours, a magnetic stirrer is used for stirring for 4 hours in the initial stage of dialysis to accelerate dialysis, water is changed every 12 hours in the dialysis process, and the pH value of the dialysate is controlled to be 7; and finally, cleaning the suspension obtained by dialysis in an ultrasonic cleaner for 10min, controlling the water temperature at 25 ℃ to obtain uniformly dispersed peanut shell cellulose nanowhisker suspension, and freeze-drying the peanut shell cellulose nanowhisker suspension for 1h at-10 ℃ to obtain a dried product, wherein the dried product is the peanut shell cellulose nanowhisker, as shown in a picture B in a figure 1.
As shown in fig. 2, the diffraction peak of the prepared cellulose whisker prepared by the method is 13-23 °, high and sharp, and has a large crystal surface area, which indicates that the cellulose whisker extracted from the peanut shell has high crystallinity, and shows obvious diffraction peaks at two positions of 2 θ of about 16.5 ° and 22.6 °, which are respectively diffraction characteristic peaks of a (110) crystal plane and a (002) crystal plane, and the structure is a typical cellulose I crystal form, the crystallinity of the cellulose whisker is calculated according to the Segal method, and the crystallinity of the cellulose whisker is 70.1% by calculating the intensity of the (002) crystal plane to represent the content of a crystal region and an amorphous region in the cellulose whisker, and the intensity of the (110) crystal plane to represent the content of an amorphous region in the cellulose whisker. This indicates that the original starch, lignin, etc. in the cellulose are eliminated during the preparation process, and that the crystal structure of the cellulose is not destroyed during the preparation process.
The method for preparing the nano-cellulose whiskers by using the peanut shells has the advantages that the waste peanut shells are used as the extraction source of the nano-cellulose whiskers, the range of raw materials for preparing the nano-cellulose whiskers is expanded, the limitation of the raw material source of the nano-cellulose whiskers is favorably accelerated to break through, the commercial product discharge of the nano-cellulose whiskers is realized early, and an innovative idea of utilizing the waste resources of the peanut shells at a high value is provided; furthermore, the chlorine-free bleaching can be realized through a three-stage cooking mode of matching formic acid and hydrogen peroxide, which is obtained through the research of the inventor, the operation method is environment-friendly, and the lignin removal degree is high; in addition, the TEMPO oxidation method is mild, the problem of safe operation caused by using a large amount of concentrated sulfuric acid in the traditional preparation method is solved, the whole preparation process is safe, and the cellulose whiskers with high crystallinity and large major diameter can be obtained.
Example two:
the invention relates to a method for preparing nano-cellulose whiskers by using peanut shells, which comprises the following steps of:
(1) cleaning waste peanut shells, removing impurities, drying, crushing by using a crusher, and sieving by using a 80-mesh sieve to obtain peanut shell powder with the particle size of less than 0.2 mm;
(2) pouring 50g of the peanut shell powder obtained in the step (1) into a sodium hydroxide solution with the mass fraction of 7% for soaking for 8 hours to remove hemicellulose and lignin, completely immersing the peanut shell powder in the sodium hydroxide solution during soaking, cleaning with deionized water after soaking, draining, pouring into an EDTA solution with the mass fraction of 2% for soaking for 8 hours after draining, removing calcium and magnesium ions, completely immersing the peanut shell powder in the EDTA solution during soaking, and then cleaning with deionized water and drying to obtain treated powder;
(3) and (3) pouring 10g of the treated powder obtained in the step (2) into 150mL of mixed solution, and reacting under mechanical stirring to obtain a reaction system, wherein the mixed solution is prepared by mixing formic acid and hydrogen peroxide, and the mixing ratio of the formic acid to the hydrogen peroxide is 2: 1, heating the reaction system at a constant temperature of 30 ℃ and stirring for 1 hour, heating to 60 ℃, continuously stirring for 1 hour, then carrying out suction filtration, then adding 150mL of the mixed solution again, heating at 30 ℃ and continuously stirring for 2 hours, then washing with deionized water to be neutral, finally carrying out suction filtration, drying and grinding to obtain powder, wherein the powder is peanut shell cellulose;
(4) taking 10g of the peanut shell cellulose obtained in the step (3), and obtaining wet pulp with the pH value of 7 by a TEMPO oxidation method; specifically, 0.025g of TEMPO, 0.25g of NaBr and 25g of NaClO were dissolved in Na2CO3-NaHCO3Preparing TEMPO oxidizing reagent in buffer solution, and adding Na2CO3-NaHCO3Adding 10g of peanut shell cellulose into 1000mL of TEMPO oxidation reagent, stirring and dispersing, placing the mixture in a constant-temperature water bath kettle at the temperature of 30 ℃ for stirring at constant temperature, stirring for reacting for 5 hours, adding 20mL of ethanol to stop the reaction after the reaction is finished, centrifuging by using a centrifugal separator after the reaction is finished to obtain oxidation slurry, acidifying the oxidation slurry by using a dilute hydrochloric acid solution for 30 minutes, wherein the action is to convert sodium carboxylate in the oxidation fiber into carboxylic acid, washing by using deionized water to obtain wet slurry with the pH value of 7, and storing the wet slurry at the temperature of 5-8 ℃ for later use;
(5) and (3) filtering the wet pulp obtained in the step (4) by using an ultrafiltration membrane with the molecular weight cutoff of 8000-14000, and freeze-drying the filtered filter residue for 1h at-10 ℃ to obtain a dried product, wherein the dried product is the peanut shell cellulose nanowhisker.
The peak of the crystallization characteristics of the peanut shell nanocellulose whisker prepared in the third example is similar to the XRD patterns of the peanut shell nanocellulose whiskers in the first and second examples by using an X-ray scanner, and the calculation shows that the degree of crystallization of the peanut shell nanocellulose whisker in the third example is as high as 65%.
The above embodiments are not intended to limit the scope of the present invention, and any suitable changes or modifications made by those skilled in the art should be construed as not departing from the scope of the present invention.
Claims (6)
1. A method for preparing nano cellulose whiskers by using peanut shells is characterized by comprising the following steps:
(1) cleaning and removing impurities from the waste peanut shells, drying, and crushing to obtain peanut shell powder with the particle size of less than 0.2 mm;
(2) pouring the peanut shell powder obtained in the step (1) into an alkali liquor with the mass fraction of 1% -10% to soak for 4-10 hours, immersing the peanut shell powder in the alkali liquor during soaking, cleaning with deionized water after soaking, draining, pouring the peanut shell powder into an EDTA solution with the mass fraction of 0.5% -2% after draining to soak for 4-10 hours, immersing the peanut shell powder in the EDTA solution during soaking, and cleaning with deionized water and drying to obtain treated powder;
(3) pouring the treated powder obtained in the step (2) into a mixed solution of formic acid and hydrogen peroxide, stirring for 1-2 hours at 20-30 ℃, heating to 40-60 ℃, continuing stirring for 1-2 hours, performing suction filtration, adding an equal amount of the mixed solution of formic acid and hydrogen peroxide after suction filtration, stirring for 1-2 hours at 20-30 ℃, washing with deionized water until the pH value is 7, and finally performing suction filtration and drying to obtain peanut shell cellulose; the mixing ratio of the formic acid to the hydrogen peroxide is one of 0.5:1, 1:1 and 1:0.5, and the mixed solution of the formic acid and the hydrogen peroxide is immersed in the treatment powder in the step (2);
(4) obtaining wet pulp with the pH value of 7 by using the peanut shell cellulose obtained in the step (3) through a TEMPO oxidation method; and then sequentially filtering and freeze-drying to obtain a dried substance, wherein the dried substance is the peanut shell nano cellulose whisker.
2. The method for preparing nano cellulose whiskers by using peanut shells as claimed in claim 1, wherein the method comprises the following steps: and (2) crushing the peanut shells in the step (1) by using a crusher, and sieving the crushed peanut shells with a 80-mesh sieve to obtain peanut shell powder with the particle size of less than 0.2 mm.
3. The method for preparing nano cellulose whiskers by using peanut shells as claimed in claim 1, wherein the method comprises the following steps: the alkali liquor in the step (2) is one of sodium hydroxide solution and potassium hydroxide solution.
4. The method for preparing nano cellulose whiskers by using peanut shells as claimed in claim 1, wherein the method comprises the following steps: the TEMPO oxidation method of the step (4) is realized by the following steps:
(a) adding the peanut shell cellulose obtained in the step (3) into a TEMPO oxidation reagent, stirring and dispersing, wherein the TEMPO oxidation reagent is prepared by dissolving TEMPO, NaBr and NaClO in Na in a dispersing way2CO3-NaHCO3The buffer solution is prepared, wherein the mass ratio of TEMPO, NaBr and NaClO is 1: 5-20: 500-1000, wherein each 1g of peanut shell cellulose needs 20-100 mL of TEMPO oxidizing reagent, and the use amount of TEMPO is 0.5-2% of the mass of the peanut shell cellulose;
(b) placing the reaction system in the step (a) in a constant-temperature water bath kettle, stirring and reacting for 2-4 hours at a constant temperature of 20-40 ℃, adding 10-50 mL of ethanol to terminate the reaction after the reaction is finished, and performing centrifugal separation to obtain oxidized slurry;
(c) and (c) acidifying the oxidation slurry obtained in the step (b) by using a 0.1-1 mol/L dilute hydrochloric acid solution for 0.5-1 hour, immersing the oxidation slurry in the dilute hydrochloric acid solution, and washing the oxidation slurry by using deionized water until the pH value is 7 after the acidification is finished.
5. The method for preparing nano cellulose whiskers by using peanut shells as claimed in claim 4, wherein: in the step (c), the oxidized slurry is washed with deionized water and stored at 5-8 ℃ for later use.
6. The method for preparing nano cellulose whiskers by using peanut shells as claimed in claim 1, wherein the method comprises the following steps: in the step (4), the wet pulp is filtered by adopting an ultrafiltration membrane or a dialysis bag with the molecular weight cutoff of 8000-14000.
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| CN103031356A (en) * | 2012-12-19 | 2013-04-10 | 青岛农业大学 | Method for applying peanut shells to synchronously prepare nanocellulose crystal and sugar |
| CN104762845A (en) * | 2015-04-13 | 2015-07-08 | 东华大学 | Method for extracting cellulose nanowhiskers from corn husks |
| CN105648816A (en) * | 2016-01-18 | 2016-06-08 | 东华大学 | Method for extracting plant cellulose nanowhisker |
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| CN103031356A (en) * | 2012-12-19 | 2013-04-10 | 青岛农业大学 | Method for applying peanut shells to synchronously prepare nanocellulose crystal and sugar |
| CN104762845A (en) * | 2015-04-13 | 2015-07-08 | 东华大学 | Method for extracting cellulose nanowhiskers from corn husks |
| CN105648816A (en) * | 2016-01-18 | 2016-06-08 | 东华大学 | Method for extracting plant cellulose nanowhisker |
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