CN111975906B - Wood preservation modification treatment method and application thereof - Google Patents
Wood preservation modification treatment method and application thereof Download PDFInfo
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- CN111975906B CN111975906B CN202010847173.2A CN202010847173A CN111975906B CN 111975906 B CN111975906 B CN 111975906B CN 202010847173 A CN202010847173 A CN 202010847173A CN 111975906 B CN111975906 B CN 111975906B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/50—Mixtures of different organic impregnating agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/04—Combined bleaching or impregnating and drying of wood
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- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention discloses a wood preservative modification treatment method, which is used for treating wood by using a chemical agent containing quercetin and oxalic acid, wherein the quercetin is grafted on the cell wall of the wood through the oxalic acid. Weighing 5-20 parts of quercetin and 2-50 parts of oxalic acid, dissolving in 300 parts of absolute ethyl alcohol 150, and adding 0.4-2 parts of p-toluenesulfonic acid to form the chemical agent for treating wood; soaking the wood to be treated for 48-96h at normal temperature and normal pressure; and (3) treating the impregnated wood blocks in an environment at 120 ℃ for 2-8 h. The invention can combine the quercetin with the cell wall of the wood effectively, increase the durability of the wood, improve the anti-leaching performance of the wood, solve the technical problem that the quercetin as a plant source natural bacteriostatic component is difficult to be fixed and easy to be leached in the wood, and expand the application of the quercetin in the technical field of wood preservation.
Description
Technical Field
The invention belongs to the technical field of wood modification, and relates to a wood modification treatment method capable of improving the corrosion resistance of wood, and application of the method in modification treatment of wood.
Background
The wood as the traditional renewable biomass material has the advantages of natural degradation, easy processing, high strength-weight ratio, close pattern and color for people and good electric-thermal insulation and acoustic properties, and is always closely related to human life. However, as a natural material, wood is vulnerable to fungi such as rot fungi, soft rot fungi, and mold fungi, and the service life of the wood is shortened, resulting in significant economic loss. Wood preservation is a process of enhancing the durability of wood by treating the wood by physical or chemical means to protect it from decay fungi, insects, marine drilling animals, and the like. The wood preservation technology has important significance for prolonging the service life of the wood, reducing the consumption of the wood, keeping the good characteristics of the wood and promoting the sustainable development of forest resources.
At present, chemical agent corrosion prevention is a common corrosion prevention method, but most of traditional wood preservatives contain heavy metal salts and oxides such as copper, chromium, arsenic and the like, and the threat to human health and the pollution of the environment caused by the use of the wood preservatives are becoming a problem of worldwide concern. The growing public concern over the environment has prompted the development of new environmentally friendly wood preservatives, and green preservation of wood is rapidly becoming a current focus. The plant-derived natural bacteriostatic components are applied to the wood preservation, so that the research direction is hot, the natural bacteriostatic components extracted from the plants have the effects of inhibiting wood decay fungi and are green and environment-friendly, the service life of the wood is prolonged, adverse effects on the environment and human health are avoided, and the development and utilization prospects are wide.
Quercetin, chemical formula C15H10O7Quercetin, also known as quercetin, is a flavonoid compound, a plant secondary metabolite widely found in nature, and found in various vegetables and fruits, such as acai berry, broccoli, apple, etc. Quercetin has antioxidant and free radical scavenging effects, and also has anticancer, antiinflammatory and antibacterial physiological activities, and has been studied in antioxidant, antiinflammatory and antibacterial, antitumor and cardiovascular protection aspects. Until now, the effective application of quercetin in the technical field of wood processing is relatively less, and the team of the inventors of the present patent application has made a more intensive study on the application of quercetin in the field of wood modification treatment (especially preservative treatment), specifically see patent applications CN2018108014706 and CN 2019104623521.
Disclosure of Invention
The wood is a natural porous material, and the quercetin serving as a plant source natural bacteriostatic component is difficult to fix and easy to lose in the wood, which is one of the technical difficulties of applying the quercetin to wood preservation. Aiming at the technical difficulty, the invention provides a wood preservative modification treatment method, which has the core technical thought that oxalic acid containing dicarbonyl, which can be subjected to esterification reaction with quercetin and wood, is used for grafting the quercetin on the cell wall of the wood, so that the antibacterial activity of the quercetin is maintained, and the durability of the wood is improved. Based on the technical scheme, the flavonol compounds including quercetin can be grafted on the cell wall of the wood by adopting the same or similar technical scheme, so that the application of the flavonol compounds including quercetin and the like in the field of wood preservation is further expanded, and the wide application prospect is shown.
In order to achieve the purpose of the invention, the wood preservative modification treatment method uses a chemical agent containing quercetin and oxalic acid to treat wood, wherein the quercetin is grafted on the cell wall of the wood through the oxalic acid, and the related chemical reaction formula is as follows.
In a preferred embodiment of the method for wood preservation and modification treatment, the chemical agent contains p-toluenesulfonic acid as a catalyst. The above chemical reaction formula is more preferably as follows.
As one of the preferable embodiments of the wood preservation and modification treatment method, the method comprises the steps of dissolving quercetin and oxalic acid in ethanol, and adding p-toluenesulfonic acid to form the chemical agent for treating wood; and soaking the wood to be treated in the chemical agent at normal temperature and normal pressure.
Specifically, 5-20 parts of quercetin and 2-50 parts of oxalic acid are weighed and dissolved in 300 parts of anhydrous ethanol 150, and 0.4-2 parts of p-toluenesulfonic acid is added to form the chemical agent for treating wood; soaking the wood to be treated for 48-96h at normal temperature and normal pressure; and (3) treating the impregnated wood blocks in an environment at 120 ℃ for 2-8 h.
As one of the preferable embodiments of the wood preservation and modification treatment method, the method comprises the steps of dissolving quercetin and oxalic acid in ethanol, and adding p-toluenesulfonic acid to form the chemical agent for treating wood; and soaking the wood to be treated in the chemical agent, and carrying out vacuum pressurization treatment.
Specifically, 5-20 parts of quercetin and 2-50 parts of oxalic acid are weighed and dissolved in 300 parts of anhydrous ethanol 150, and 0.4-2 parts of p-toluenesulfonic acid is added to form the chemical agent for treating wood; treating the wood to be treated for 10-15min under the vacuum condition of 525-600mmHg (0.07-0.08Mpa), then pressurizing to 0.7-0.9Mpa and carrying out pressure-maintaining impregnation for 20-24 h; and (3) treating the impregnated wood blocks in an environment at 120 ℃ for 2-8 h.
In addition, the invention further provides the application of the wood preservation and modification treatment method in the aspect of wood modification.
In addition, the wood can be subjected to preservative treatment by adopting the wood preservative modification treatment method.
Compared with the prior art, the wood preservation modification treatment method has the advantages or beneficial effects mainly reflected in the following aspects.
1) The common technicians in the field can easily know that wood can be damaged by decay fungi to shorten the service life of the wood in outdoor or humid environment, most of the existing wood preservatives can be used for performing preservative treatment on the wood, but the existing wood preservatives are not combined with wood components through firm chemical bonds, so that the wood preservatives are easy to lose, and the long-lasting and effective preservative effect is difficult to achieve.
2) Quercetin is a natural bacteriostatic component of plant origin. The wood is treated by the chemical agent containing quercetin and oxalic acid, and the chemical agent does not contain heavy metal salts and oxides such as copper, chromium, arsenic and the like, and does not threaten the health of people and the environment, so that the chemical agent used in the invention belongs to a novel environment-friendly wood preservative.
3) In order to effectively fix the quercetin in the wood and improve the anti-losing performance of the preservative, the invention utilizes oxalic acid which can generate esterification reaction with the quercetin and hydroxyl on the wood cell wall to graft the quercetin on the wood cell wall, so that effective chemical bond links are formed between the quercetin and the oxalic acid and between the oxalic acid and the wood cell wall, and the durability of the preservative is improved.
4) Under the technical conditions (parameters) set by the invention, the anti-corrosion technology of the quercetin grafted modified wood is simple. Compared with other technologies for improving the durability of the preservative, the technology disclosed by the invention is simple in process and easy to realize, and has better durability due to the chemical bond connection with the wood. Experiments prove that the quercetin has a remarkable inhibiting effect on wood decay fungi such as Gloeophyllum trabeum and Coriolus versicolor.
Drawings
FIG. 1 is a scanning electron micrograph of untreated Chinese white poplar (Populus tomentosa).
FIG. 2 is a scanning electron microscope image of modified Populus tomentosa grafted with quercetin obtained in example 2 of the present invention after a loss test.
FIG. 3 is an X-ray photoelectron spectrum of untreated Chinese white poplar (Populus tomentosa).
FIG. 4 is an X-ray photoelectron spectrum of modified Populus tomentosa grafted with quercetin obtained in example 2 of the present invention after a leaching test.
FIG. 5 is an infrared spectrum of quercetin, untreated Chinese white poplar (Populus tomentosa) and modified Chinese white poplar obtained in example 2 subjected to a loss test.
Detailed Description
In order to better understand the technical features of the present invention, the present invention will be further described with reference to specific examples. It should be noted that the given examples are not intended to limit the scope of the invention.
Example 1
Weighing 17g of quercetin and 7.1g of oxalic acid dihydrate, dissolving in 188mL of absolute ethyl alcohol to prepare a solution with the molar ratio of the quercetin to the oxalic acid dihydrate being 1:1, adding 1.54g of p-toluenesulfonic acid into the solution, stirring uniformly, and then adding Chinese white poplar (Populus tomentosa) wood blocks.
The system is subjected to impregnation treatment for 15min under the vacuum condition of 525-600mmHg (0.07-0.08Mpa), then pressurized to 0.8Mpa and subjected to pressure-maintaining impregnation for 24 h. And (3) after the ethanol solvent is completely volatilized, putting the impregnated wood block into a 120 ℃ drying oven for treatment for 8 hours to obtain the modified wood grafted with the quercetin.
Example 2
Weighing 12g of quercetin and 10g of oxalic acid dihydrate, dissolving in 188mL of absolute ethyl alcohol to prepare a solution with the molar ratio of the quercetin to the oxalic acid dihydrate being 1:2, adding 1.54g of p-toluenesulfonic acid into the solution, stirring uniformly, and then putting the Chinese white poplar blocks.
The system is subjected to impregnation treatment for 15min under the vacuum condition of 525-600mmHg (0.07-0.08Mpa), then pressurized to 0.8Mpa and subjected to pressure-maintaining impregnation for 24 h. And (3) after the ethanol solvent is completely volatilized, putting the impregnated wood block into a 120 ℃ drying oven for treatment for 6 hours to obtain the modified wood grafted with the quercetin.
Example 3
Weighing 15g of quercetin and 18.8g of oxalic acid dihydrate, dissolving in 188mL of absolute ethyl alcohol to prepare a solution with the molar ratio of the quercetin to the oxalic acid dihydrate being 1:3, adding 1.54g of p-toluenesulfonic acid into the solution, stirring uniformly, and then putting the Chinese white poplar blocks. The system is subjected to immersion treatment for 48 hours under the vacuum condition of 525 and 600mmHg (0.07-0.08 Mpa). And (3) after the ethanol solvent is completely volatilized, putting the impregnated wood block into a 120 ℃ drying oven for treatment for 4 hours to obtain the modified wood grafted with the quercetin.
Example 4
This example presents a test of the preservative performance of lost wood for wood preservation techniques. The test method comprises the following steps: the modified populus tomentosa obtained in the example 1-3 is put into a drying oven at 40-60 ℃ to be dried to constant weight, then the dried populus tomentosa is put into a beaker to be subjected to a loss test, deionized water is added to ensure that the test material is immersed below the liquid level of the deionized water, and the stirring is continuously carried out. The deionized water is replaced once every 6h, 24h and 48h, and then replaced once every 48h, and the total time is 14 d.
The modified Chinese white poplar obtained in examples 1 to 3 after the runoff test was subjected to a decay resistance test. The test strains were Gloeophyllum trabeum (Gloeophyllum trabeum) and Coriolus versicolor (Coriolus versicolor), and Populus alba (Populusto mentosa) was used as test material. The control was an unmodified treated aspen (Populus tomentosa) specimen.
GB/T13942.1-2009 part 1 of durability of wood: the test was carried out according to the method of the natural corrosion resistance laboratory test methods, and the test results are shown in Table 1.
Mass loss rate R1The calculation formula of (2):
R1％＝(M1-M2)/M1％
in the formula: m1-the total dry mass of the modified wood after the loss resistance test;
M2the quality of the modified wood after the anti-flow test and the decay resistance test is completely dry.
TABLE 1 Corrosion resistance test results of corrosion-resistant treated Populus tomentosa
As shown in Table 1, the control was a sample not subjected to preservative treatment, and the mass loss rate under the exposure to Coriolus versicolor (Coriolus versicolor) was 44.51%, and the mass loss rate under the exposure to Gloeophyllum trabeum (Gloeophyllum trabeum) was 38.41%. After the modified wood obtained in examples 1-3 is subjected to a loss test, the mass loss rates of the modified wood respectively exposed to coriolus versicolor and plectomyces densicola are reduced to different degrees and reach above grade II corrosion resistance. This demonstrates that the modified aspen obtained by the wood preservative modification treatment method described in examples 1-3 can still improve the decay resistance of aspen wood after the runoff test.
FIG. 1 shows a scanning electron micrograph of untreated aspen. The scanning electron micrograph of the modified Chinese white poplar obtained in example 2 and grafted with quercetin through the loss test treatment is shown in fig. 2. Comparing fig. 1 and 2, it can be seen that the modified aspen (B) obtained in example 2 through the loss-through test has a thicker cell wall than the untreated aspen (a), indicating that the modified aspen obtained in example 2 contains quercetin in the cell wall.
FIG. 3 shows the X-ray photoelectron spectrum of untreated Chinese white poplar. FIG. 4 is an X-ray photoelectron spectrum of modified Populus tomentosa grafted with quercetin obtained in example 2 of the present invention after a leaching test. Table 2 shows the relative intensities (%) of the C1s components obtained from the X-ray photoelectron spectroscopy of the untreated chinese white poplar and the modified chinese white poplar obtained in example 2 subjected to the loss tangent test. Fig. 4 and table 2 show that the relative strengths of C1 and C4 of the quercetin-grafted modified chinese white poplar obtained in example 2 after the runoff test were enhanced compared to the virgin chinese white poplar, indicating that wood contained O-C ═ O (ester group), -C-H and-C-after the modification treatment.
TABLE 2 relative intensity (%) -of C1s components obtained from X-ray photoelectron spectroscopy of untreated Chinese white poplar and modified Chinese white poplar obtained in example 2 subjected to loss test
FIG. 5 shows the IR spectra of quercetin, untreated aspen and modified aspen obtained in example 2 by loss testing. As can be seen from FIG. 5, the modified Populus tomentosa grafted with quercetin obtained in example 2 after the runoff test was rinsed with ethanol several times at 1768cm after the rinsing, compared with the untreated material and quercetin-1(stretching vibration of C ═ O in O-C ═ O) shows that a new peak is generated, which indicates that a new functional group ester group is generated on the wood cell wall; the treated material is 1515cm-1(stretching vibration of benzene ring skeleton) 1319cm-1(═ C-O-C antisymmetric and symmetric stretching vibration) and 807cm-1(para-substituted benzene ring out-stretching vibration) three quercetin characteristic peaks were enhanced compared to the untreated material, indicating that quercetin was grafted on the modified treated material. This demonstrates that quercetin forms an effective chemical bond with the hydroxyl groups of the wood cell wall.
Claims (3)
1. A wood preservation modification treatment method is characterized in that wood is treated by a chemical agent containing quercetin and oxalic acid, the quercetin is grafted on the cell wall of the wood through the oxalic acid, and the related chemical reaction formula is
Weighing 5-20 parts of quercetin and 2-50 parts of oxalic acid, dissolving in 150-300 parts of absolute ethyl alcohol, and adding 0.4-2 parts of p-toluenesulfonic acid to form the chemical agent for treating wood;
soaking the wood to be treated for 48-96h at normal temperature and normal pressure;
and (3) treating the impregnated wood in an environment at 120 ℃ for 2-8 h.
2. The wood preservative modification treatment method according to claim 1, comprising,
weighing 5-20 parts of quercetin and 2-50 parts of oxalic acid, dissolving in 150-300 parts of absolute ethyl alcohol, and adding 0.4-2 parts of p-toluenesulfonic acid to form the chemical agent for treating wood;
treating the wood to be treated for 10-15min under the vacuum condition of 525-;
and (3) treating the impregnated wood in an environment at 120 ℃ for 2-8 h.
3. Use of the method of wood preservation modification treatment according to claim 1 or 2 for the modification of wood.
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| CN114789490B (en) * | 2022-04-18 | 2023-08-08 | 中山市伍氏大观园家具有限公司 | Redwood furniture production line |
| CN114701029B (en) * | 2022-04-18 | 2023-06-02 | 中山市伍氏大观园家具有限公司 | Pretreatment process of rosewood |
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| US4883689A (en) * | 1987-02-20 | 1989-11-28 | Rhone Poulenc, Inc. | Method of preserving wood with lanthanide derivatives |
| US20150306002A1 (en) * | 2012-12-13 | 2015-10-29 | Merck Patent Gmbh | 3-hydroxy-4-oxo-4h-pyran- or 3-hydroxy-4-oxo-1,4-dihydropyridine derivatives as protein-adhesive active substances |
| CN103433988A (en) * | 2013-08-27 | 2013-12-11 | 东北林业大学 | Method for performing functional improvement on wood by using polybasic carboxylic acid |
| CN103709131A (en) * | 2013-12-31 | 2014-04-09 | 南昌大学 | Quercetin derivatives and synthetic method thereof |
| CN108328635B (en) * | 2018-03-21 | 2020-01-21 | 上海应用技术大学 | Method for preparing alumina aerogel |
| CN108972789B (en) * | 2018-07-20 | 2020-11-27 | 西北农林科技大学 | Wood modifier, preparation method thereof and method for modifying and treating wood by using modifier |
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