CN114908597A - Method for extracting alpha cellulose from tree wheel - Google Patents

Method for extracting alpha cellulose from tree wheel Download PDF

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CN114908597A
CN114908597A CN202210554873.1A CN202210554873A CN114908597A CN 114908597 A CN114908597 A CN 114908597A CN 202210554873 A CN202210554873 A CN 202210554873A CN 114908597 A CN114908597 A CN 114908597A
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alpha cellulose
tree
extracting
soaking
extraction
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CN114908597B (en
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牛振川
黄云菲
冯雪
张贵前
梁单
吕梦妮
王国卫
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Institute of Earth Environment of CAS
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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
    • 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
    • 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
    • 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
    • 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 rings, which belongs to the technical field of alpha cellulose extraction and comprises the following steps: (1) cutting the tree wheel sample into pieces and uniformly mixing; (2) performing ultrasonic extraction with chloroform-ethanol mixed solution, removing filtrate, mixing the solid substance with ethanol, extracting at constant temperature, and filtering to obtain residual solid substance; (3) adding a hydrochloric acid solution and sodium chlorite, soaking for 2 hours, and filtering the solution to obtain a filtered solid substance; (4) and adding a sodium hydroxide solution into the filtered solid matter, soaking for 2 hours, then adding a hydrochloric acid solution, and soaking for 1 hour at 70 ℃ to obtain the alpha cellulose. The method can efficiently, economically and environmentally extract the alpha cellulose from the tree wheel so as to be convenient for isotope analysis to obtain climate and environmental change information in the tree wheel, effectively improve the extraction efficiency of the alpha cellulose in the tree wheel, shorten the extraction time and save the using amount of organic solvent.

Description

Method for extracting alpha cellulose from tree rings
Technical Field
The invention relates to the technical field of alpha cellulose extraction, in particular to a method for extracting alpha cellulose from tree rings.
Background
The trees absorb the atmospheric CO from the leaves through photosynthesis 2 Converted into self-organic matter and can pass through stable isotope ratio (delta) in tree wheel 13 C、δ 18 O) and radioisotope levels (. DELTA. 14 C) The tree wheel can record climate, environmental information and changes thereof in the growth process of trees, so 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 a small amount of extractables and ash. Wherein the ash is inorganic material and the extractable is low molecular migratable organic material such as wax, fat, oil, resin, etc. In the first place, studies on isotopes in tree rings were conducted using all trees in tree rings, but the results obtained were not satisfactory because of differences in the isotope ratios of cellulose, lignin, extractables, and other components in tree rings. Cellulose is a long-chain carbon-based polymer, which is formed by connecting glucose molecules through beta-1, 4-glycosidic bonds, and carbon atoms and oxygen atoms in the structure of the polymer are not exchanged with water or other compounds once formed. Thus based on this stability, alpha-cellulose allows recording of climate, environmental information during tree growth compared to other components in the tree wheel, and researchers have begun to prefer in subsequent studies to use isotopic analysis of alpha-cellulose extracted from tree wheel samples to remove as much as possible of the unstable, migratable, exchangeable other non-cellulosic components in the hope of extracting pure alpha-cellulose. However, α -cellulose extracted by a conventional extraction method for plant cellulose always contains a trace amount of impurities (lignin and the like). 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, holocellulose is extracted by a solvent extraction and bleaching process, and insoluble α -cellulose is extracted by soaking in a 17.5% sodium hydroxide solution. Due to the relatively stable isotope ratio of alpha cellulose, the single biosynthetic pathway, and the low mobility in tree rings, most tree ring isotope studies currently utilize alpha cellulose extracted from tree rings.
The process of extracting the alpha cellulose in the tree wheel is complicated and long, and the extraction process is completely different from the conventional extraction of the cellulose of chemical raw materials such as straws, sugarcanes, waste paper and the like because the alpha cellulose is mostly used for laboratory analysis and has high required purity. Researchers have proposed a variety of methods for extracting alpha cellulose for many years, and at present, the method for extracting alpha cellulose, which can completely remove other substances, basically comprises three main steps of organic solvent extraction, sodium hypochlorite bleaching treatment and alkalization treatment, can remove migratable substances such as resin and the like, inorganic salts, some soluble low molecular organic matters such as gum and the like, and can remove most of lignin and extract alpha cellulose. Organic solvent extraction processes, although different types of solvents are used, mostly employ soxhlet extraction for extraction. The Soxhlet extraction method relies on the permeation process to extract the components in the plant sample, although has the advantages of good selectivity, low energy consumption and the like; the disadvantages are also evident, i.e. large error in results, long extraction time, large amount of organic solvent used, special soxhlet extractor equipment including extraction bottle, extraction tube, condenser, etc., and inability to process large batches or quantities of >15 samples, so soxhlet extraction has been complicated and inefficient for isotope research. Therefore, there is a need to find a method for extracting alpha-cellulose from a tree ring simply and efficiently without using a large amount of an organic solvent harmful to the environment.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for extracting alpha cellulose from tree rings, which can efficiently, economically and environmentally extract the alpha cellulose from the tree rings so as to be convenient for isotope research, effectively improve the extraction efficiency of the alpha cellulose in the tree rings, shorten the extraction time, save the use amount 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 a tree ring comprising the steps of:
(1) cutting the tree wheel sample into pieces and uniformly mixing;
(2) placing a tree wheel sample in a glass test tube, adding a chloroform-ethanol mixed solution, performing ultrasonic extraction for 1h in an ultrasonic cleaner, then extracting for 3.5h at 65 ℃, repeating the process twice circularly, removing filtrate, mixing solid substances with absolute ethyl alcohol, performing constant-temperature extraction for 8h at 80 ℃, filtering, mixing the solid substances with ultrapure water again, performing constant-temperature soaking for 8h at 80 ℃, and filtering to obtain residual solid substances;
(3) adding 1mol/L hydrochloric acid solution and sodium chlorite into the residual solid matter, mixing uniformly, soaking for 2 hours at 70 ℃, repeating the steps until the tree wheel sample becomes light yellow, and filtering the solution to obtain filtered solid matter;
(4) adding 2 wt% sodium hydroxide solution into the filtered solid matter, soaking at 50 deg.C for 2 hr, discarding the waste liquid, adding 0.5mol/L hydrochloric acid solution, and soaking at 70 deg.C for 1 hr to obtain alpha cellulose.
After being cut up, a dried tree wheel sample is firstly subjected to ultrasonic and constant-temperature water bath extraction by adopting chloroform-ethanol mixed solution, absolute ethanol and ultrapure water respectively so as to remove migratable components such as resin, wax, fat, oil and the like and soluble low-molecular organic matters such as inorganic salt, gum and the like from the solid tree wheel sample, then most lignin in the tree wheel is removed by using hydrochloric acid and sodium chlorite, and finally hemicellulose and residual lignin are removed by using sodium hydroxide solution and hydrochloric acid respectively, so that the obtained insoluble white solid is alpha cellulose.
The alpha cellulose extracted from the tree wheel is used for isotope analysis, belongs to the extraction category of laboratories, and is different from the extraction of the chemical raw material cellulose of the conventional straw, sugarcane, waste paper and other raw materials. Because other substances can influence the isotope result, the required purity and efficiency are completely different, pure alpha cellulose can be extracted, the accuracy of the isotope analysis result is ensured, and meanwhile, the extraction efficiency is required to be improved and the use of harmful reagents is required to be reduced as much as possible. Through the cavitation and diffusibility of the ultrasonic extraction step, the organic solvent rapidly enters the solid tree wheel sample, and the extractable matter needing to be removed is extracted at an accelerated speed; the combination of the micro-bubbles generated in the extracting agent and the continuous growth and the breakage promotes the dispersion of the solid tree wheel sample, further increases the contact area of the extracting agent and the solid sample, and accelerates the process of diffusing the soluble components in the tree wheel sample to the extracting agent by the heat energy converted when the ultrasonic wave is conducted in the extracting agent.
Further, the volume-to-mass ratio of the chloroform-ethanol mixed solution to the sample in the step (2) is 1 mL: 2 mg.
Further, the volume mass ratio of the 2 wt% sodium hydroxide solution in the step (4) to the filtered solid matter is 1 mL: 2 mg.
Further, the volume mass ratio of the 1mol/L hydrochloric acid solution to the rest solid matters in the step (3) is 1 mL: 2mg, wherein the volume mass ratio of the 0.5mol/L hydrochloric acid solution to the solid matter in the step (4) is 1 mL: 2 mg.
Further, the ultrasonic electric power of the ultrasonic cleaner is 300W, and the frequency is 40kHz
Further, the chloroform-ethanol mixed solution is prepared by mixing chloroform and absolute ethanol according to a volume ratio of 2: 1, mixing and preparing.
Further, the tree wheel samples were chopped to 1-1.2 mm.
Further, the alpha cellulose extracted according to the present invention is used for 14 C, analyzing to research climate and environment information in the tree growth process.
The invention has the following beneficial effects:
compared with the traditional method, the alpha cellulose extracted by the method has complete shape and the isotope analysis result is close to the actual result, and can reflect the environmental information in the tree growth process, and the alpha cellulose extracted by the method can be quasi-analyzed during isotope analysisAtmosphere that does reflect its recording 14 And C, information. Meanwhile, the steps disclosed by the invention can save more than half of the extraction time, and the usage amount of the organic solvent is saved by about 95%, so that the method is more efficient, economic and environment-friendly.
Drawings
FIG. 1 is alpha cellulose extracted from the pine tree wheel of example 1;
Detailed Description
The invention will be described in detail with reference to specific embodiments and drawings, wherein:
example 1: extraction of alpha cellulose from pine cone
(1) Cutting dried pine cone sample of about 1950 into pieces with width of about 1mm with a nicking tool, and mixing;
(2) taking 20mg of an oil pine tree wheel sample, adding 10mL of chloroform-ethanol mixed solution (the volume ratio of chloroform to absolute ethyl alcohol is 2: 1), uniformly mixing, placing the glass test tube with the sample in an ultrasonic cleaner with the ultrasonic electric power of 300W and the frequency of 40kHZ for ultrasonic extraction for 1h, then extracting at the constant temperature of 65 ℃ for 3.5h, circularly repeating the steps for two times, cooling, filtering out the extraction solvent, adding 10mL of absolute ethyl alcohol into the solid matter, extracting at the constant temperature of 80 ℃ for 8h, cooling, filtering out the extraction solvent, soaking the solid matter and 10mL of ultrapure water at the temperature of 80 ℃ for 8h, cooling, filtering out the solution, and obtaining the residual solid matter;
(3) adding 10mL of 1mol/L hydrochloric acid solution and 0.1g of sodium chlorite into the residual solid matter, uniformly mixing, soaking at 70 ℃ for 2h, repeating the step until the tree wheel sample becomes light yellow, filtering the solution, washing the residual solid with ultrapure water until the pH value is 5-6, and obtaining the filtered solid matter;
(4) adding 10mL of 2 wt% sodium hydroxide solution into the filtered solid, soaking for 2h at 50 ℃, cooling, filtering, discarding waste liquid, washing the residual solid with ultrapure water until the pH value is 8-9, adding 10mL of 0.5mol/L hydrochloric acid solution into the solid, soaking for 1h at 70 ℃, cooling, filtering to remove the solution, washing the residual white solid with ultrapure water again until the white solid is neutral, and drying at 60 ℃ to obtain the alpha cellulose.
Comparative example 1: acid-base acid method for extracting alpha cellulose
Comparative example 1 is a comparison of a conventional cellulose extraction method with the extraction method of the present invention, and the specific extraction steps are as follows:
(1) selecting the same Chinese pine sample in the example 1, cutting the Chinese pine sample into fragments with the width of about 1mm by using a nicking tool, and uniformly mixing;
(2) taking 20mg of a pine cone sample, adding 25mL of a 1mol/L HCl solution into a glass test tube, heating at 70 ℃, and soaking overnight;
(3) adjusting the pH value of the solution to 3, and adding a proper amount of NaClO 2 Soaking at 70 deg.C until the sample turns white, and filtering to remove the solution;
(4) washing the residual solid with ultrapure water to neutrality, and drying at 60 ℃ to obtain the alpha cellulose.
Comparative example 2: soxhlet extraction method for extracting alpha cellulose
Comparative example 2 is a soxhlet extraction method for extracting alpha cellulose, and compared with the extraction method of the invention, the specific extraction steps are as follows:
(1) cutting the same sample of the pine tree wheel in the example 1 into fragments with the width of about 1mm by a nicking tool, and uniformly mixing;
(2) mixing 20mg of an oil pine cone sample with 200mL of benzene-ethanol mixed solution (the volume ratio of benzene to absolute ethanol is 2: 1), extracting for 16h by using a Soxhlet extraction method, filtering to obtain a solid matter, mixing the solid matter with 200mL of absolute ethanol solution, extracting for 16h by using the Soxhlet extraction method again, filtering, using 1000mL of ultrapure water bath for 8h to obtain the residual solid matter, filtering, and removing the filtrate to obtain the solid matter;
(3) adding 700mL of ultrapure water, 1mL of acetic acid and 8g of sodium chlorite into the solid matter, uniformly mixing, soaking for 12h at 70 ℃, treating once every 2h by using the same method after 12h, repeating for three times, soaking for 12h by using the same method, and filtering to obtain a solid matter;
(4) soaking the solid matter in 100mL of 17.5 wt% sodium hydroxide solution for 1h, cooling, filtering, washing the residual solid with ultrapure water until the pH value is neutral, then soaking in 100mL of 10 wt% acetic acid for 1h, washing the solid matter with ultrapure water until the solid matter is neutral, and drying at 60 ℃ to obtain the alpha cellulose.
Detection of radioactive carbon in Tachypoda cellulose extracted in example 1, comparative example 1 and comparative example 2: ( 14 C) Content, the data obtained are shown in table 1:
TABLE 1
Δ 14 C/‰ Colour(s) Shape of Degree of integrity
Example 1 -23.9±1.9 White colour Width of<1mm of fragments Intact, with some fine fragments
Comparative example 1 66.6±2.0 Light yellow Width of<1mm of fragments Intact, with some fine fragments
Comparative example 2 -11.6±3.0 White colour Width of<1mm small pieces Is finely crushed and has a plurality of fine fragments
Note: delta of tree-ring alpha cellulose 14 C is radioactive carbon (C) in the sample 14 C) Content, 0.2MV through the centre of mass spectrum of a Siemens accelerator 14 And C, calculating after measurement by using an Accelerator Mass Spectrometer (AMS).
And (3) data analysis:
1. the alpha cellulose obtained in example 1 and comparative examples 1 and 2 were analyzed, and comparative example 2 extracted alpha cellulose by conventional acid-base acid method 14 C (66.6 +/-2.0 thousandths) is synchronous with the latitude atmosphere similar to northern hemisphere by delta 14 The C data (-24.7 +/-1.9 permillage) have larger difference, which indicates that the acid-base acid method cannot extract pure alpha cellulose and impurities which influence the analysis result exist. And extracting alpha cellulose by traditional acid-base-acid method (66.6 + -2.0 ‰) and traditional Soxhlet extraction method (11.6 + -3.0 ‰) 14 C comparison, delta measured for alpha cellulose of example 1 14 C (-23.9 +/-1.9 ‰) and north hemisphere approximate latitude atmosphere synchronous period delta 14 The C data (24.7 +/-1.9 per mill) is more approximate, which shows that the invention can extract pure alpha cellulose and can accurately reflect the recorded atmosphere when carrying out isotope analysis 14 And C, information.
2. Compared with the traditional Soxhlet extraction method adopted in the comparative example 2, the method used in the example 1 consumes a long time and a large amount of organic solvent, but the extraction method saves more than half of the time, obviously improves the extraction efficiency, and is simpler, more convenient and faster; the use amount of the organic solvent is saved by about 95 percent (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 one time, but the method can process about 70 samples in batches, thereby greatly increasing the sample processing amount. From the quality of the extracted alpha cellulose, the extraction method provided by the invention can collect and extract as much as possible, improve the purity, remove impurities, prevent other substances in the sample from interfering the isotope analysis result, cause analysis errors and improve the analysis accuracy.
3. By comparing the shape, color and integrity of the alpha cellulose obtained in example 1 with those obtained in comparative examples 1 and 2, the alpha cellulose extracted by the method of the present invention has complete properties and good quality.
4. Compared with the example 1, the comparative examples 1 and 2 show that in the tree wheel sample processing step and the organic solvent extraction step, the selection of the processing flow, the extraction method and the amount of the extracted organic solvent all have influence on the isotope analysis accuracy of the alpha cellulose, even the extract is light yellow and the impurities are obvious, so that the alpha cellulose extracted by the method disclosed by the invention has high purity, complete shape and high accuracy of isotope analysis results, and is extremely suitable for isotope analysis to obtain climate and environmental change information in the alpha cellulose.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.

Claims (8)

1. A method for extracting alpha cellulose from a tree ring, comprising the steps of:
(1) cutting the tree wheel sample into pieces and uniformly mixing;
(2) placing a tree wheel sample in a glass test tube, adding a chloroform-ethanol mixed solution, performing ultrasonic extraction for 1h in an ultrasonic cleaner, then extracting for 3.5h at 65 ℃, repeating the steps twice in a circulating manner, removing filtrate, mixing solid substances with ethanol, performing constant-temperature extraction for 8h at 80 ℃, filtering, mixing the solid substances with ultrapure water again, performing constant-temperature soaking for 8h at 80 ℃, and filtering to obtain residual solid substances;
(3) adding 1mol/L hydrochloric acid solution and sodium chlorite into the residual solid matter, mixing uniformly, soaking for 2h at 70 ℃, repeating the steps until the tree wheel sample becomes light yellow, and filtering the solution to obtain filtered solid matter;
(4) adding 2 wt% sodium hydroxide solution into the filtered solid matter, soaking at 50 deg.C for 2 hr, discarding the waste liquid, adding 0.5mol/L hydrochloric acid solution, and soaking at 70 deg.C for 1 hr to obtain alpha cellulose.
2. The method for extracting alpha cellulose from tree trunks according to claim 1, wherein the volume-to-mass ratio of the chloroform-ethanol mixed solution to the sample in step (2) is 1 mL: 2 mg.
3. The method for extracting alpha cellulose from a tree ring as claimed in claim 1, wherein the volume mass ratio of the 2 wt% sodium hydroxide solution to the filtered solid substance in the step (4) is 1 mL: 2 mg.
4. The method for extracting alpha cellulose from a tree wheel as claimed in claim 1, wherein the volume mass ratio of the 1mol/L hydrochloric acid solution to the remaining solid matter in the step (3) is 1 mL: 2mg, wherein the volume mass ratio of the 0.5mol/L hydrochloric acid solution to the solid matter in the step (4) is 1 mL: 2 mg.
5. The method for extracting alpha cellulose from tree trunks according to claim 1, wherein the ultrasonic power of the ultrasonic cleaner is 300W and the frequency is 40 kHz.
6. The method for extracting alpha cellulose from a tree ring according to claim 2, wherein the chloroform-ethanol mixed solution is prepared by mixing chloroform and absolute ethanol in a volume ratio of 2: 1, mixing and preparing.
7. The method for extracting alpha cellulose from tree trunks according to claim 1, wherein said tree trunk samples are chopped to 1-1.2 mm.
8. A method for extracting alpha cellulose from tree branches according to any one of claims 1 to 7, characterized in that the extracted alpha cellulose is used for 14 And C, analyzing.
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Citations (3)

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Publication number Priority date Publication date Assignee Title
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CN108660837A (en) * 2018-05-29 2018-10-16 南京林业大学 The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT152305B (en) * 1935-10-31 1938-01-25 Juljusz Saft Process for the production of α-cellulose.
CN103003487A (en) * 2010-05-04 2013-03-27 巴伊亚特种纤维素公司 Method and system for high alpha dissolving pulp production
CN108660837A (en) * 2018-05-29 2018-10-16 南京林业大学 The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material

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Title
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