CN114908597B - Method for extracting alpha cellulose from tree wheels - Google Patents
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- CN114908597B CN114908597B CN202210554873.1A CN202210554873A CN114908597B CN 114908597 B CN114908597 B CN 114908597B CN 202210554873 A CN202210554873 A CN 202210554873A CN 114908597 B CN114908597 B CN 114908597B
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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
- D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
- D21B1/30—Defibrating by other means
- D21B1/303—Defibrating by other means using vibrating devices
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for extracting alpha cellulose from tree wheels, which belongs to the technical field of alpha cellulose extraction and comprises the following steps: cutting the tree wheel sample into pieces and uniformly mixing; (2) Ultrasonic extracting with chloroform-ethanol mixed solution, removing filtrate, mixing solid substance with ethanol, extracting at constant temperature, and filtering to obtain residual solid substance; (3) Adding hydrochloric acid solution and sodium chlorite, soaking for 2 hours, and filtering the solution to obtain a filtered solid substance; (4) Adding sodium hydroxide solution into the filtered solid substance, soaking for 2 hours, adding hydrochloric acid solution, and soaking for 1 hour at 70 ℃ to obtain the alpha cellulose. The method can efficiently, economically and environmentally-friendly extract the alpha cellulose from the tree wheels so as to be convenient for isotope analysis to acquire climate and environmental change information in the tree wheels, effectively improve the extraction efficiency of the alpha cellulose in the tree wheels, shorten the extraction time and save the consumption of organic solvents.
Description
Technical Field
The invention relates to the technical field of alpha cellulose extraction, in particular to a method for extracting alpha cellulose from tree wheels.
Background
Atmospheric CO absorbed by leaves of trees through photosynthesis 2 Is converted into self-organic matter and can therefore be converted into self-organic matter by stable isotope ratio (delta 13 C、δ 18 O) and radioisotope level (delta) 14 C) The method can record the climate, environmental information and changes thereof in the tree growth process, so that the tree wheel is widely applied to the research of stable isotopes and radioactive isotopes.
The main chemical components of trees are cellulose, hemicellulose, lignin and small amounts of extractables and ash. Wherein ash is an inorganic substance and the extractables are low molecular weight migratable organic substances such as waxes, fats, oils, resins, etc. Initially, studies on isotopes of tree rounds were performed using whole trees of tree rounds, but the results obtained were not ideal due to differences in the isotope ratios of components such as cellulose, lignin, extractables, etc. in tree rounds. Cellulose is a long-chain carbon-based polymer formed by connecting glucose molecules through beta-1, 4-glycosidic bonds, and once formed, carbon atoms and oxygen atoms in the structure cannot exchange with water or other compounds. Based on this stability, therefore, the alpha cellulose can record climate and environmental information during tree growth as compared to other components in the tree wheel, and researchers begin to trend in subsequent studies towards isotope analysis using alpha cellulose extraction from tree wheel samples, removing as much of the unstable, mobile, exchangeable other non-cellulose components as possible, in order to extract pure alpha cellulose. However, the α cellulose extracted by the usual plant cellulose extraction method always contains a trace amount of impurities (lignin, etc.). To ensure the accuracy of the isotope results, it is necessary to completely remove these impurities to obtain pure alpha cellulose or a substance having properties close to those of pure cellulose. In recent years, the method of extracting substances having properties closest to those of pure cellulose is to extract all cellulose by solvent extraction and bleaching, and then to extract insoluble alpha cellulose by immersing in 17.5% sodium hydroxide solution. Because of the relatively stable isotope ratio of alpha cellulose, single biosynthetic pathway, and low mobility in the tree rounds, most tree rounds of isotope studies currently utilize alpha cellulose extracted from the tree rounds.
The process for extracting the alpha cellulose in the tree wheel is tedious and tedious, and is completely different from the conventional extraction of chemical raw material cellulose of raw materials such as straw, sugarcane, waste paper and the like because the alpha cellulose is mostly used for laboratory analysis and the required purity is high. For many years, researchers have proposed various methods for extracting alpha cellulose, and the current method for completely removing other substances and extracting the alpha cellulose basically comprises three main steps of organic solvent extraction, sodium hypochlorite bleaching treatment and alkalization treatment, and can remove mobilizable substances such as resin, inorganic salts, soluble low-molecular organic matters such as some gums and the like, and simultaneously remove most of lignin and extract the alpha cellulose. Organic solvent extraction processes, although varying in the type of solvent used, mostly employ soxhlet extraction for extraction. The Soxhlet extraction method relies on the permeation process to extract the components in the plant sample, and has the advantages of good selectivity, low energy consumption and the like; the disadvantages are also obvious, namely large error, long extraction time, large organic solvent consumption, need of specific Soxhlet extractor, including extraction bottle, extraction tube, condenser, etc., and inability to process large-scale or number >15 samples, so Soxhlet extraction is complex and inefficient for isotope research. Therefore, there is a need for a simple and efficient method for extracting alpha cellulose from tree rounds without using large amounts of environmentally harmful organic solvents.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for extracting alpha cellulose from tree wheels, which can efficiently, economically and environmentally-friendly extract the alpha cellulose from the tree wheels so as to be convenient for isotope research, effectively improve the extraction efficiency of the alpha cellulose in the tree wheels, shorten the extraction time, save the consumption of organic solvents and simultaneously have higher extraction purity.
The invention solves the technical problems by the following technical means:
a method of extracting alpha cellulose from tree rounds comprising the steps of:
(1) Cutting the tree wheel sample into pieces and uniformly mixing;
(2) Placing the tree wheel sample in a glass test tube, adding a chloroform-ethanol mixed solution, performing ultrasonic extraction in an ultrasonic cleaner for 1h, performing extraction at 65 ℃ for 3.5h, repeating the cycle twice, removing filtrate, mixing solid matters with absolute ethyl alcohol, performing constant-temperature extraction at 80 ℃ for 8h, filtering out, mixing the solid matters with ultrapure water again, performing constant-temperature soaking at 80 ℃ for 8h, and filtering to obtain residual solid matters;
(3) Adding 1mol/L hydrochloric acid solution and sodium chlorite into the rest solid matters, uniformly mixing, soaking for 2 hours at 70 ℃, repeating the steps until the tree wheel sample becomes light yellow, and filtering the solution to obtain a filtered solid matters;
(4) Adding 2wt% sodium hydroxide solution into the filtered solid substance, soaking for 2 hours at 50 ℃, discarding the waste liquid, adding 0.5mol/L hydrochloric acid solution, and soaking for 1 hour at 70 ℃ to obtain the alpha cellulose.
Cutting up a dried tree wheel sample, respectively performing ultrasonic extraction and constant-temperature water bath extraction by using a chloroform-ethanol mixed solution, absolute ethyl alcohol and ultrapure water to remove mobilizable components such as resin, wax, fat, oil and the like and soluble low-molecular organic matters such as inorganic salts, gum and the like from the solid tree wheel sample, removing most lignin in the tree wheel by using hydrochloric acid and sodium chlorite, and finally removing hemicellulose and residual lignin by using a sodium hydroxide solution and hydrochloric acid respectively to obtain insoluble white solid which is alpha cellulose.
The alpha cellulose extracted from the tree wheel is used for isotope analysis, belongs to the field of laboratory extraction, and is extracted differently from the cellulose extraction of the chemical raw materials such as the conventional straw, the sugarcane, the waste paper and the like. Because other substances can influence the isotope results, the required purity and efficiency are completely different, and pure alpha cellulose can be extracted, so that the accuracy of isotope analysis results is ensured, and meanwhile, the extraction efficiency is improved as much as possible and the use of harmful reagents is reduced. Through cavitation and diffusibility of the ultrasonic extraction step, the organic solvent rapidly enters the solid tree wheel sample to accelerate extraction of the extractables to be removed; the combination of the method enables the generation of micro bubbles in the extractant to be continuously increased and broken, promotes the dispersion of the solid tree wheel sample, further increases the contact area of the extractant and the solid sample, and simultaneously accelerates the process of the soluble components in the tree wheel sample to be dispersed into the extractant due to the heat energy converted when the ultrasonic waves are conducted in the extractant.
Further, the volume-mass ratio of the chloroform-ethanol mixed solution in the step (2) to the sample is 1mL:2mg.
Further, the volume to mass ratio of the 2wt% sodium hydroxide solution to the filtered solid matter in the step (4) is 1mL:2mg.
Further, the volume-mass ratio of the 1mol/L hydrochloric acid solution to the rest solid matters in the step (3) is 1mL:2mg, wherein the volume mass ratio of the 0.5mol/L hydrochloric acid solution to the solid matters in the step (4) is 1mL:2mg.
Further, the ultrasonic electric power of the ultrasonic cleaner is 300W, and the frequency is 40kHz
Further, the chloroform-ethanol mixed solution is prepared from chloroform and absolute ethanol according to a volume ratio of 2:1 are mixed to prepare the composite material.
Further, the tree wheel samples were minced to 1-1.2mm.
Further, the alpha cellulose extracted according to the present invention is used for 14 C, analyzing to study climate and environment information in the tree growth process.
The beneficial effects of the invention are as follows:
compared with the traditional method, the alpha cellulose extracted by the method has complete shape, the isotope analysis result is close to the actual result, the environment information in the tree growth process can be reflected, and the recorded atmosphere can be accurately reflected when the isotope analysis is carried out on the alpha cellulose extracted by the method 14 And C, information. Meanwhile, the steps disclosed by the invention can save more than half of extraction time, and the use amount of the organic solvent is saved by about 95%, so that the method is more efficient, economical and environment-friendly.
Drawings
FIG. 1 is an alpha cellulose extracted from a pine cone of example 1;
Detailed Description
The invention will be described in detail below with reference to specific embodiments and accompanying drawings:
example 1: pine tree wheel alpha cellulose extraction
(1) Cutting dried Chinese pine wheel sample about 1950 into pieces about 1mm wide by a nicking tool, and mixing uniformly;
(2) Taking 20mg of a Chinese pine tree wheel sample, adding 10mL of chloroform-ethanol mixed solution (the volume ratio of chloroform to absolute ethanol is 2:1) into a glass test tube, uniformly mixing, placing the glass test tube with the sample into an ultrasonic cleaner with ultrasonic electric power of 300W and frequency of 40kHZ for ultrasonic extraction for 1h, then carrying out constant-temperature extraction for 3.5h at 65 ℃, circularly repeating the steps for two times, filtering the extraction solvent after cooling, adding 10mL of absolute ethanol into a solid substance, carrying out constant-temperature extraction for 8h at 80 ℃, cooling, filtering the extraction solvent after cooling, soaking the solid substance and 10mL of ultrapure water for 8h at 80 ℃, cooling, filtering, and filtering the solution to obtain the residual solid substance;
(3) Adding 10mL of 1mol/L hydrochloric acid solution and 0.1g of sodium chlorite into the residual solid matters, uniformly mixing, soaking for 2 hours at 70 ℃, repeating the steps until the tree wheel sample becomes light yellow, filtering the solution, and washing the residual solid matters with ultrapure water until the pH value is 5-6 to obtain filtered solid matters;
(4) 10mL of 2wt% sodium hydroxide solution is added into the filtered solid, soaking is carried out for 2 hours at 50 ℃, cooling is carried out, filtering is carried out, waste liquid is discarded, the rest solid is washed by ultrapure water until the pH value is 8-9, 10mL of 0.5mol/L hydrochloric acid solution is added into the solid, soaking is carried out for 1 hour at 70 ℃, cooling is carried out, solution is filtered, the rest white solid is washed to be neutral by ultrapure water again, and drying is carried out at 60 ℃, thus obtaining the alpha cellulose.
Comparative example 1: acid-base acid method for extracting alpha cellulose
Comparative example 1 is a comparison of a general cellulose extraction process with the extraction process of the present invention, and the specific extraction steps are as follows:
(1) Selecting the same Chinese pine sample as in example 1, cutting into pieces about 1mm wide by a nicking tool, and uniformly mixing;
(2) Taking 20mg of a pine cone sample in a glass test tube, adding 25mL of 1mol/L HCl solution, heating at 70 ℃ and soaking overnight;
(3) Adjusting the pH of the solution to 3, adding a proper amount of NaClO 2 Soaking at 70deg.C until the sample turns white, and filtering to remove solution;
(4) Washing the rest solid with ultrapure water to neutrality, and drying at 60deg.C to obtain alpha cellulose.
Comparative example 2: soxhlet extraction method for extracting alpha cellulose
Comparative example 2 is a soxhlet extraction of alpha cellulose, in contrast to the extraction method of the present invention, the specific extraction steps are as follows:
(1) Cutting the same sample of the pine cone as in example 1 with a nicking tool to pieces about 1mm wide, and mixing uniformly;
(2) Mixing 20mg of an oil pine tree wheel sample with 200mL of benzene-ethanol mixed solution (the volume ratio of benzene to absolute ethanol is 2:1), extracting for 16h by adopting a Soxhlet extraction method, filtering to obtain a solid substance, mixing the solid substance with 200mL of absolute ethanol solution, extracting for 16h by adopting the Soxhlet extraction method again, filtering to obtain the rest solid substance, using 1000mL of ultra-pure water for 8h, filtering, and removing the filtrate to obtain the solid substance;
(3) Adding 700mL of ultrapure water, 1mL of acetic acid and 8g of sodium chlorite into the solid substance, uniformly mixing, soaking for 12h at 70 ℃, treating every 2h by adopting the same method after 12h, repeating for three times, then soaking for 12h by adopting the same method, and filtering to obtain the solid substance;
(4) The solid matter was immersed in 100ml of 17.5wt% sodium hydroxide solution for 1 hour, cooled and filtered, the remaining solid was washed with ultrapure water until the pH was neutral, then immersed in 100ml of 10wt% acetic acid for 1 hour, washed with ultrapure water until the solid matter was neutral, and dried at 60 ℃ to obtain alpha cellulose.
Radioactive carbon in tree-wheel alpha cellulose extracted in example 1, comparative example 1 and comparative example 2 was detected 14 C) Content, the data obtained are shown in table 1:
TABLE 1
| Δ 14 C/‰ | Color of | Shape and shape | Integrity degree | |
| Example 1 | -23.9±1.9 | White color | Wide width of<1mm chip | Complete, with partial fine fragments |
| Comparative example 1 | 66.6±2.0 | Yellowish light yellow | Wide width of<1mm chip | Complete, with partial fine fragments |
| Comparative example 2 | -11.6±3.0 | White color | Wide width of<1mm small pieces | Finer and more fine fragments |
Note that: delta of tree wheel alpha cellulose 14 C is the radioactive carbon in the sample 14 C) Content, 0.2MV through the center of the Siemens accelerator mass spectrum 14 C dedicated Accelerator Mass Spectrometer (AMS) measurement.
Data analysis:
1. analysis of the alpha cellulose obtained in example 1 and comparative examples 1 and 2, comparative example 2, in which alpha cellulose was extracted using a conventional acid-base acid method 14 C (66.6+/-2.0%o) and approximately latitude of northern hemisphere in atmospheric synchronization delta 14 The large difference between the C data (-24.7+ -1.9%o) indicates that the acid-base acid method can not extract pure alpha cellulose, and impurities which have influence on analysis results exist. Compared with the traditional acid-base method (66.6+/-2.0%o) and the traditional methodSoxhlet extraction (-11.6+ -3.0% 14 C compared to the measured delta for the alpha cellulose of example 1 14 C (-23.9+ -1.9%o) atmospheric synchronization delta of approximate latitude of northern hemisphere 14 C data (-24.7+/-1.9%o) are closer to each other, which shows that the invention can extract pure alpha cellulose and accurately reflect the recorded atmosphere when performing isotope analysis 14 And C, information.
2. The method used in the embodiment 1 is compared with the traditional Soxhlet extraction method adopted in the comparative example 2, the Soxhlet extraction method is long in time consumption and consumes a large amount of organic solvent, and the extraction method disclosed by the invention saves more than half of time, remarkably improves the extraction efficiency, and is simpler, more convenient and quicker; the use amount of the organic solvent is saved by about 95 percent (the amount is reduced from 200 mL/sample to 10 mL/sample), and the method is more economical and environment-friendly. In addition, the traditional Soxhlet extraction method can process 10-15 samples at a time, and the invention can process about 70 samples in batches, so that the sample processing capacity is greatly increased. From the quality of the extracted alpha cellulose, the extraction method provided by the invention can collect and extract as much as possible, improve purity and remove impurities, prevent other substances in a sample from interfering an isotope analysis result, cause analysis errors and improve analysis accuracy.
3. The shape, color and integrity of the alpha cellulose obtained in comparative example 1 and comparative examples 1 and 2 show that the alpha cellulose extracted by the method of the invention has complete character and good quality.
4. Compared with the example 1, the comparative example 1 and the comparative example 2 show that in the tree wheel sample treatment step and the organic solvent extraction step, the treatment flow, the extraction method and the dosage selection of the extracted organic solvent have influence on the isotope analysis accuracy of the alpha cellulose, even the problems that the extract is light yellow and the impurities are obvious occur, so that the alpha cellulose extracted by the method disclosed by the invention has high purity, complete shape and high isotope analysis result accuracy, and is extremely suitable for isotope analysis to acquire climate and environment change information in the isotope analysis.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention. The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (6)
1. A method for extracting alpha cellulose from tree rounds, comprising the steps of:
(1) Cutting the tree wheel sample into pieces and uniformly mixing;
(2) Placing the tree wheel sample in a glass test tube, and adding a chloroform-ethanol mixed solution, wherein the volume mass ratio of the chloroform-ethanol mixed solution to the sample is 1mL:2mg, after ultrasonic extraction for 1h in an ultrasonic cleaner, extracting for 3.5h at 65 ℃, circularly repeating for two times, removing filtrate, mixing solid matters with ethanol, extracting at a constant temperature of 80 ℃ for 8h, filtering, mixing the solid matters with ultrapure water again, soaking at a constant temperature of 80 ℃ for 8h, and filtering to obtain residual solid matters;
(3) Adding 1mol/L hydrochloric acid solution and sodium chlorite into the rest solid matters, uniformly mixing, soaking for 2 hours at 70 ℃, repeating the steps until the tree wheel sample becomes light yellow, and filtering the solution to obtain a filtered solid matters;
(4) Adding 2wt% sodium hydroxide solution into the filtered solid substance, soaking for 2 hours at 50 ℃, discarding the waste liquid, adding 0.5mol/L hydrochloric acid solution, and soaking for 1 hour at 70 ℃ to obtain alpha cellulose;
the extracted alpha cellulose is used for 14 C, analysis.
2. The method for extracting alpha cellulose from tree rings according to claim 1, wherein the volume mass ratio of 2wt% sodium hydroxide solution to filtered solid matter in the step (4) is 1mL:2mg.
3. The method for extracting alpha cellulose from tree rings according to claim 1, wherein the volume/mass ratio of 1mol/L hydrochloric acid solution to the remaining solid matter in the step (3) is 1mL:2mg, wherein the volume mass ratio of the 0.5mol/L hydrochloric acid solution to the solid matters in the step (4) is 1mL:2mg.
4. The method for extracting alpha cellulose from tree rings according to claim 1, wherein the ultrasonic cleaner has an ultrasonic electric power of 300W and a frequency of 40kHz.
5. The method for extracting alpha cellulose from tree wheels according to claim 1, wherein the chloroform-ethanol mixed solution comprises chloroform and absolute ethanol according to a volume ratio of 2:1 are mixed to prepare the composite material.
6. A method of extracting alpha cellulose from tree rounds according to claim 1 wherein the tree round samples are shredded to 1-1.2mm.
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| AT152305B (en) * | 1935-10-31 | 1938-01-25 | Juljusz Saft | Process for the production of α-cellulose. |
| CA2744250C (en) * | 2010-05-04 | 2016-10-11 | Bahia Specialty Cellulose Sa | Method and system for pulp processing using cold caustic extraction with alkaline filtrate reuse |
| CN108660837B (en) * | 2018-05-29 | 2021-03-30 | 南京林业大学 | Method for separating cellulose, hemicellulose and lignin from plant fiber raw material |
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