CN110552224A - Method for separating and extracting cellulose nanocrystals and lignin from poplar wood powder - Google Patents
Method for separating and extracting cellulose nanocrystals and lignin from poplar wood powder Download PDFInfo
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- CN110552224A CN110552224A CN201910839929.6A CN201910839929A CN110552224A CN 110552224 A CN110552224 A CN 110552224A CN 201910839929 A CN201910839929 A CN 201910839929A CN 110552224 A CN110552224 A CN 110552224A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
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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
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/003—Pulping cellulose-containing materials with organic compounds
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
Abstract
The invention provides a method for separating and extracting cellulose nanocrystals and lignin from poplar wood powder, belonging to the field of separation and extraction of natural high polymer materials. According to the method, 1-6 parts by mass of poplar powder is treated by using a mixed acid system composed of 60-90 parts by mass of organic acid, 40 parts by mass of distilled water and 5-20 parts by mass of concentrated sulfuric acid with the mass fraction of 98%, the reaction temperature is 70-80 ℃, the reaction time is 6-8 hours, the organic acid is specifically one of oxalic acid, formic acid and acetic acid, and after the reaction is finished, alkali treatment is carried out on the obtained cellulose nanocrystal containing lignin, so that the separation of the cellulose nanocrystal and the lignin is realized. The method omits the step of preparing the cellulose nanocrystals to carry out pretreatment and delignification on the fiber raw material, and simultaneously obtains two products of the cellulose nanocrystals and the lignin, the process is simple, and the cost is reduced.
Description
Technical Field
The invention relates to the field of separation and extraction of natural polymer materials, in particular to a method for separating and extracting cellulose nanocrystals and lignin from poplar wood powder.
Background
The wood fiber raw material is the most abundant and cheap renewable biomass resource on the earth, mainly comprises three parts of cellulose, hemicellulose and lignin, and the environment-friendly and renewable wood fiber resource is widely applied in various fields along with the increasingly prominent problem of fossil resource shortage and the continuous aggravation of environmental pollution. The cellulose nanocrystal is rod-shaped cellulose with nanoscale, and has the characteristics of high strength, high modulus, high crystallinity, high specific surface area, low thermal expansion coefficient, good dispersibility, capability of biological decomposition and the like, so that the cellulose nanocrystal has great application potential in various fields of packaging printing, pulping and papermaking, sewage purification, electronic devices, daily chemicals, biological medicine, oil and gas field development and the like.
the lignin is a main component of non-carbohydrate in the wood fiber, is the most abundant natural aromatic high molecular substance in the nature, has rich structure and high molecular weight, can be used as a surfactant, a resin synthetic additive, an agricultural compound fertilizer, a potential petroleum substitute product and the like, and has great development potential. At present, most of raw materials selected for preparing the cellulose nanocrystals are pulp subjected to pretreatment to remove lignin, and a large amount of chemicals and energy consumption are needed in the pretreatment process of the raw materials, wherein the lignin is removed by high-temperature cooking of the wood raw materials through caustic soda by a chemical method, so that resource waste and economic loss are greatly caused, and excessive energy consumption is caused. If a novel method for preparing the cellulose nanocrystals can be developed, fiber raw materials which are not chemically pretreated are directly adopted, and are directly hydrolyzed through a mixed acid system, the cellulose nanocrystals containing lignin are prepared, then the lignin is separated through a simple mild alkali treatment process, and the preparation and separation of two products, namely the cellulose nanocrystals and the lignin are realized, so that the method has important significance for the effective utilization of resources and the saving of energy.
Disclosure of Invention
the invention mainly aims to develop a method for directly separating and extracting cellulose nanocrystals and lignin from wood raw material poplar wood powder without delignification, and realize the preparation and separation of the cellulose nanocrystals and the lignin with low energy consumption.
The method specifically comprises the following steps:
(1) Adding 60-90 parts by mass of organic acid and 40 parts by mass of water into a reactor at 15-35 ℃, then adding 5-20 parts by mass of 98% concentrated sulfuric acid, heating to 70-90 ℃, then mechanically stirring for 5-15 min to form a mixed acid system, then adding 1-6 parts by mass of poplar powder, continuing to react for 6-8 h at 70-90 ℃, and then adding 100-400 parts by mass of distilled water for dilution to obtain a mixed solution;
The organic acid is any one of oxalic acid, formic acid and acetic acid;
(2) centrifuging the mixed solution obtained in the step (1) for 5-15 min at the rotating speed of 8000-10000 r/min, pouring out supernatant liquid and reserving a precipitate part, dispersing the obtained precipitate by 200-400 parts by mass of distilled water, centrifuging for 5-15 min at the rotating speed of 8000-10000 r/min, repeating the centrifugal washing process for 3-6 times to obtain the cellulose nanocrystal containing lignin;
(3) Adding 25-35 parts by mass of 1mol/L NaOH solution into the cellulose nanocrystal containing lignin obtained in the step (2), mechanically stirring for 4-5 h at a stirring speed of 100-200 r/min, centrifuging for 5-15 min at a rotating speed of 8000-10000 r/min, and separating a supernatant and a precipitate;
(4) Adding 100-400 parts by mass of distilled water into the precipitate obtained by centrifugation in the step (3), uniformly stirring, centrifuging for 5-15 min at the rotating speed of 8000-10000 r/min, repeating the centrifugal washing operation for 2-4 times, and then performing freeze drying or spray drying to obtain cellulose nanocrystals;
(5) And (3) dropwise adding 6mol/L HCl solution into the supernatant obtained by centrifugation in the step (3), adjusting the pH value to 1.5-2.0 to separate out lignin dissolved in the solution, centrifuging for 5 min-15 min at the rotating speed of 8000 r/min-10000 r/min, pouring out the supernatant to keep a precipitate part, dispersing the obtained precipitate with 100-400 parts by mass of distilled water, centrifuging for 5 min-15 min at the rotating speed of 8000 r/min-10000 r/min, repeating the centrifugal washing process with distilled water for 2-4 times, and freeze-drying or spray-drying to obtain the lignin.
the particle size of the poplar wood powder is 0.1-3 mm.
In the step (1), the mechanical stirring is carried out at a speed of 100 r/min-200 r/min.
has the advantages that:
The method realizes the extraction and separation of the cellulose nanocrystals and the lignin, and two products are finally obtained through simple mixed acid treatment and mild alkali treatment, thereby greatly improving the economic benefit of production. Compared with the traditional route of preparing the cellulose nanocrystal by removing lignin firstly, the method has the advantages of milder conditions and obviously reduced energy consumption.
Detailed Description
the following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention.
Example 1
Adding 60g of formic acid and 40g of distilled water into a 500mL three-necked bottle at 25 ℃, adding 20g of concentrated sulfuric acid with the mass fraction of 98%, controlling the temperature by an oil bath, heating to 70 ℃, stirring for 5min to form a mixed acid system, adding 1.5g of absolute dry poplar powder with the particle size of 0.1-3 mm into the system, continuing to react for 6h at 80 ℃, adding 100g of distilled water after the reaction is finished, centrifuging for 5min at the rotating speed of 8000r/min, pouring out supernatant liquid to keep a precipitate part, dispersing the obtained precipitate with 200g of distilled water, centrifuging for 5min at the rotating speed of 8000r/min, and repeating the centrifugal washing process with distilled water for 3 times. Adding 25g of 1mol/L NaOH solution into the precipitate obtained after washing, mechanically stirring for 4h, centrifuging for 5min at the rotating speed of 8000r/min, and separating the supernatant and the precipitate: adding 100g of distilled water into the precipitate, uniformly stirring, centrifuging for 10min at the rotating speed of 8000r/min, repeating the centrifuging and washing operation for 2 times, and then freeze-drying to obtain cellulose nanocrystals; dripping 6mol/L HCl solution into the supernatant, adjusting pH to 1.5 to separate out lignin dissolved in the solution, centrifuging at 8000r/min for 5min, pouring out the supernatant to retain precipitate, dispersing the obtained precipitate with 100g distilled water, centrifuging at 8000r/min for 5min, repeating the centrifuging and washing process with distilled water for 2 times, and freeze drying to obtain lignin. The yield of the cellulose nanocrystal is 45%, and the length is 293 +/-65 nm; the yield of lignin was 18%.
Example 2
Adding 90g of formic acid and 40g of distilled water into a 500mL three-neck flask at 35 ℃, adding 5g of concentrated sulfuric acid with the mass fraction of 98%, controlling the temperature by an oil bath, heating to 90 ℃, stirring for 15min to form a mixed acid system, adding 6g of oven-dried poplar powder with the particle size of 0.1-3 mm into the system, continuing to react for 8h at 90 ℃, adding 400g of distilled water after the reaction is finished, centrifuging for 5min at the rotating speed of 8000r/min, pouring out supernatant liquid to keep a precipitate part, dispersing the obtained precipitate with 400g of distilled water, centrifuging for 5min at the rotating speed of 10000r/min, and repeating the centrifuging and washing process with distilled water for 6 times. Adding 35g of 1mol/L NaOH solution into the precipitate obtained after washing, mechanically stirring for 5h, centrifuging for 5min at the rotating speed of 8000r/min, and separating the supernatant and the precipitate: adding 400g of distilled water into the precipitate, uniformly stirring, centrifuging for 10min at the rotating speed of 8000r/min, repeating the centrifugal washing operation for 2 times, and then freeze-drying to obtain cellulose nanocrystals; dripping 6mol/L HCl solution into the supernatant, adjusting pH to 2.0 to separate out lignin dissolved in the solution, centrifuging at 8000r/min for 5min, pouring out the supernatant to retain precipitate, dispersing the obtained precipitate with 400g distilled water, centrifuging at 8000r/min for 5min, repeating the centrifuging and washing process with distilled water for 2 times, and freeze drying to obtain lignin. The yield of the cellulose nanocrystals was 48%, and the length was 305 ± 79 nm; the yield of lignin was 20%.
Example 3
Adding 90g of formic acid and 40g of distilled water into a 500mL three-necked bottle at 35 ℃, adding 20g of concentrated sulfuric acid with the mass fraction of 98%, controlling the temperature by oil bath, heating to 70 ℃, stirring for 5min to form a mixed acid system, adding 6g of oven-dried poplar powder with the particle size of 0.1-3 mm into the system, continuing to react for 6h at 70 ℃, adding 100g of distilled water after the reaction is finished, centrifuging for 5min at the rotating speed of 8000r/min, pouring out supernatant liquid to keep a precipitate part, dispersing the obtained precipitate with 200g of distilled water, centrifuging for 5min at the rotating speed of 10000r/min, and repeating the centrifuging and washing process with distilled water for 6 times. Adding 25g of 1mol/L NaOH solution into the precipitate obtained after washing, mechanically stirring for 4h, centrifuging for 5min at the rotating speed of 8000r/min, and separating the supernatant and the precipitate: adding 100g of distilled water into the precipitate, uniformly stirring, centrifuging for 10min at the rotating speed of 8000r/min, repeating the centrifuging and washing operation for 2 times, and then freeze-drying to obtain cellulose nanocrystals; dripping 6mol/L HCl solution into the supernatant, adjusting pH to 1.5 to separate out lignin dissolved in the solution, centrifuging at 8000r/min for 5min, pouring out the supernatant to retain precipitate, dispersing the obtained precipitate with 100g distilled water, centrifuging at 8000r/min for 5min, repeating the centrifuging and washing process with distilled water for 2 times, and freeze drying to obtain lignin. The yield of the cellulose nanocrystals was 48%, and the length was 305 ± 79 nm; the yield of lignin was 20%.
example 4
Adding 60g of acetic acid and 40g of distilled water into a 500mL three-necked bottle at 25 ℃, adding 10g of concentrated sulfuric acid with the mass fraction of 98%, controlling the temperature by oil bath, heating to 80 ℃, stirring for 5min to form a mixed acid system, adding 4.5g of oven-dried poplar powder with the particle size of 0.1-3 mm into the system, continuing to react for 6h at 80 ℃, adding 100g of distilled water after the reaction is finished, centrifuging for 5min at the rotating speed of 8000r/min, pouring out the supernatant to keep a precipitate part, dispersing the obtained precipitate with 200g of distilled water, centrifuging for 5min at the rotating speed of 8000r/min, and repeating the centrifugal washing process with distilled water for 3 times. Adding 35g of 1mol/L NaOH solution into the precipitate obtained after washing, mechanically stirring for 4h, centrifuging for 5min at the rotating speed of 8000r/min, and separating the supernatant and the precipitate: adding 100g of distilled water into the precipitate, uniformly stirring, centrifuging for 10min at the rotating speed of 8000r/min, repeating the centrifuging and washing operation for 2 times, and then freeze-drying to obtain cellulose nanocrystals; dripping 6mol/L HCl solution into the supernatant, adjusting pH to 1.5 to separate out lignin dissolved in the solution, centrifuging at 8000r/min for 5min, pouring out the supernatant to retain precipitate, dispersing the obtained precipitate with 100g distilled water, centrifuging at 8000r/min for 5min, repeating the centrifuging and washing process with distilled water for 2 times, and freeze drying to obtain lignin. The yield of the cellulose nanocrystal is 46 percent, and the length is 247 +/-95 nm; the yield of lignin was 19%.
Example 5
Adding 60g of oxalic acid and 40g of distilled water into a 500mL three-necked bottle at the temperature of 15 ℃, adding 10g of concentrated sulfuric acid with the mass fraction of 98%, controlling the temperature by oil bath, heating to 80 ℃, stirring for 5min to form a mixed acid system, adding 4.5g of absolute dry poplar powder with the particle size of 0.1-3 mm into the system, continuing to react for 8h at the temperature of 80 ℃, adding 100g of distilled water after the reaction is finished, centrifuging for 5min at the rotating speed of 8000r/min, pouring out supernatant liquid to keep a precipitate part, dispersing the obtained precipitate with 200g of distilled water, centrifuging for 5min at the rotating speed of 8000r/min, and repeating the centrifugal washing process with the distilled water for 3 times. Adding 25g of 1mol/L NaOH solution into the precipitate obtained after washing, mechanically stirring for 4h, centrifuging for 5min at the rotating speed of 8000r/min, and separating the supernatant and the precipitate: adding 100g of distilled water into the precipitate, uniformly stirring, centrifuging for 10min at the rotating speed of 8000r/min, repeating the centrifuging and washing operation for 2 times, and then freeze-drying to obtain cellulose nanocrystals; dripping 6mol/L HCl solution into the supernatant, adjusting pH to 2.0 to separate out lignin dissolved in the solution, centrifuging at 8000r/min for 5min, pouring out the supernatant to retain precipitate, dispersing the obtained precipitate with 100g distilled water, centrifuging at 8000r/min for 5min, repeating the centrifuging and washing process with distilled water for 2 times, and freeze drying to obtain lignin. The yield of the cellulose nanocrystal is 42 percent, and the length is 213 +/-77 nm; the yield of lignin was 22%.
Claims (3)
1. A method for separating and extracting cellulose nanocrystals and lignin from poplar wood flour comprises the following steps:
(1) Adding 60-90 parts by mass of organic acid and 40 parts by mass of water into a reactor at 15-35 ℃, then adding 5-20 parts by mass of 98% concentrated sulfuric acid, heating to 70-90 ℃, then mechanically stirring for 5-15 min to form a mixed acid system, then adding 1-6 parts by mass of poplar powder, continuing to react for 6-8 h at 70-90 ℃, and then adding 100-400 parts by mass of distilled water for dilution to obtain a mixed solution;
The organic acid is any one of oxalic acid, formic acid and acetic acid;
(2) Centrifuging the mixed solution obtained in the step (1) for 5-15 min at the rotating speed of 8000-10000 r/min, pouring out supernatant liquid and reserving a precipitate part, dispersing the obtained precipitate by 200-400 parts by mass of distilled water, centrifuging for 5-15 min at the rotating speed of 8000-10000 r/min, repeating the centrifugal washing process for 3-6 times to obtain the cellulose nanocrystal containing lignin;
(3) Adding 25-35 parts by mass of 1mol/L NaOH solution into the cellulose nanocrystal containing lignin obtained in the step (2), mechanically stirring for 4-5 h at a stirring speed of 100-200 r/min, centrifuging for 5-15 min at a rotating speed of 8000-10000 r/min, and separating a supernatant and a precipitate;
(4) adding 100-400 parts by mass of distilled water into the precipitate obtained by centrifugation in the step (3), uniformly stirring, centrifuging for 5-15 min at the rotating speed of 8000-10000 r/min, repeating the centrifugal washing operation for 2-4 times, and then performing freeze drying or spray drying to obtain cellulose nanocrystals;
(5) And (3) dropwise adding 6mol/L HCl solution into the supernatant obtained by centrifugation in the step (3), adjusting the pH value to 1.5-2.0 to separate out lignin dissolved in the solution, centrifuging for 5 min-15 min at the rotating speed of 8000 r/min-10000 r/min, pouring out the supernatant to keep a precipitate part, dispersing the obtained precipitate with 100-400 parts by mass of distilled water, centrifuging for 5 min-15 min at the rotating speed of 8000 r/min-10000 r/min, repeating the centrifugal washing process for 2-4 times, and freeze-drying or spray-drying to obtain the lignin.
2. the method for separating and extracting cellulose nanocrystals and lignin from poplar wood flour as claimed in claim 1, wherein the method comprises the following steps: the particle size of the poplar wood powder is 0.1-3 mm.
3. the method for separating and extracting cellulose nanocrystals and lignin from poplar wood flour as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the mechanical stirring is carried out at a speed of 100 r/min-200 r/min.
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| CN111116759A (en) * | 2020-01-10 | 2020-05-08 | 天津科技大学 | Surface functionalized cellulose nanocrystal and preparation method thereof |
| CN111440248A (en) * | 2020-03-02 | 2020-07-24 | 中科如米(北京)生态农业科技发展有限公司 | Preparation method of xylose residue cellulose nanocrystal and composite hydrogel thereof |
| CN111484405A (en) * | 2020-04-26 | 2020-08-04 | 苏州纳创佳环保科技工程有限公司 | Method for preparing aromatic acid monomer by comprehensively utilizing agricultural waste raw materials |
| CN116640232A (en) * | 2023-02-17 | 2023-08-25 | 南开大学 | Preparation method of cellulose nanocrystals |
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Cited By (5)
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