CN116533342A - Method for inducing wood self-densification by using solvent swelling and evaporation - Google Patents
Method for inducing wood self-densification by using solvent swelling and evaporation Download PDFInfo
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- CN116533342A CN116533342A CN202310368895.3A CN202310368895A CN116533342A CN 116533342 A CN116533342 A CN 116533342A CN 202310368895 A CN202310368895 A CN 202310368895A CN 116533342 A CN116533342 A CN 116533342A
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- 239000002023 wood Substances 0.000 title claims abstract description 161
- 230000008961 swelling Effects 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000001704 evaporation Methods 0.000 title claims abstract description 28
- 230000008020 evaporation Effects 0.000 title claims abstract description 27
- 239000002904 solvent Substances 0.000 title claims abstract description 26
- 238000000280 densification Methods 0.000 title claims abstract description 22
- 230000001939 inductive effect Effects 0.000 title claims abstract description 20
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 210000002421 cell wall Anatomy 0.000 claims abstract description 29
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- 210000004027 cell Anatomy 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- 210000001724 microfibril Anatomy 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 16
- 229920002678 cellulose Polymers 0.000 claims abstract description 15
- 239000001913 cellulose Substances 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 230000006798 recombination Effects 0.000 claims abstract description 14
- 238000005215 recombination Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 10
- 206010042674 Swelling Diseases 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 230000009471 action Effects 0.000 claims description 26
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 230000002776 aggregation Effects 0.000 claims description 13
- 238000004220 aggregation Methods 0.000 claims description 13
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 13
- 150000004056 anthraquinones Chemical class 0.000 claims description 13
- 235000010265 sodium sulphite Nutrition 0.000 claims description 13
- 238000005056 compaction Methods 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000935 solvent evaporation Methods 0.000 claims description 2
- 239000011121 hardwood Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 abstract description 3
- 238000007493 shaping process Methods 0.000 abstract description 3
- 229920006351 engineering plastic Polymers 0.000 abstract description 2
- 229910001234 light alloy Inorganic materials 0.000 abstract description 2
- 230000006835 compression Effects 0.000 description 10
- 238000007906 compression Methods 0.000 description 10
- 238000007731 hot pressing Methods 0.000 description 8
- DIRFUJHNVNOBMY-UHFFFAOYSA-N fenobucarb Chemical compound CCC(C)C1=CC=CC=C1OC(=O)NC DIRFUJHNVNOBMY-UHFFFAOYSA-N 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 229920005610 lignin Polymers 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 240000007182 Ochroma pyramidale Species 0.000 description 3
- 241000219000 Populus Species 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- -1 anthrahydroquinone ion Chemical class 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000018185 Betula X alpestris Nutrition 0.000 description 1
- 235000018212 Betula X uliginosa Nutrition 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910001095 light aluminium alloy Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
- B27K5/06—Softening or hardening of wood
-
- 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
- B27K3/16—Inorganic impregnating agents
- B27K3/20—Compounds of alkali metals or ammonium
-
- 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
-
- 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
- B27K3/36—Aliphatic compounds
-
- 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
- B27K3/38—Aromatic compounds
-
- 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
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention discloses a method for inducing wood self-densification by using solvent swelling and evaporation, which comprises the following steps: 1. softening the wood by adopting a softening mixed solution; 2. swelling the softened wood by adopting dimethyl sulfoxide solution; 3. after dimethyl sulfoxide is fully replaced by deionized water, wood is placed in air, capillary force formed in the water evaporation process is utilized to induce wood cell shrinkage at normal temperature and normal pressure, and meanwhile, along with dynamic recombination of hydrogen bonds among cellulose molecules, cell wall microfibrils are highly oriented and aggregated, so that the wood is highly self-compacted. The densification process does not need high temperature and high pressure, secondary heat treatment shaping is not needed, and the processing energy consumption is obviously reduced. Meanwhile, the advantage of the mechanical strength of the microfibrils arranged in a directional manner of the wood is fully exerted, the grain-following tensile strength of the self-compacting wood prepared by the method is 5-45 times that of the natural wood, and the specific strength of the self-compacting wood is even higher than that of some engineering plastics and light alloy materials.
Description
Technical Field
The invention relates to a method for inducing self-densification of wood by utilizing swelling and evaporation of a solvent, belonging to the technical field of wood material modification.
Background
The fast-growing wood has the advantages of high growth speed, soft texture, low strength, easy deformation and the like, so that the application field of the fast-growing wood is greatly limited, and the mechanical property of the fast-growing wood, especially for structural materials, can be improved by a specific modification method so as to meet the bearing requirement of the structural members.
In the longitudinal view of the existing production technology, the method for reinforcing and modifying the fast-growing wood mainly adopts hot-pressing compression reinforcement. The hot-pressing compression enhancement is to soften the fast-growing wood by physical and chemical or the combination of the two to improve the plasticity of the wood, and then compress the wood under certain temperature and pressure to densify the wood, thereby improving the mechanical strength of the wood. Compression reinforcement relies mainly on the viscoelastic and plastic response of wood under the combined action of wet-heat-force, and generally comprises the steps of cell wall wet-heat softening treatment, wood hot-pressing compression treatment, deformation fixation for avoiding elastic recovery and the like. This process is accompanied by energy intensive processing techniques such as long-term (typically 10-30 hours) wood softening and hot-pressing at high temperatures (typically 160-220 ℃) so that large-scale applications are often limited by high energy consumption. In addition, the compressed wood generally requires a secondary heat treatment to solve the elastic recovery problem due to the release of compressive stress and the strong hygroscopic property of cellulose. Although the method can realize industrial production, the method cannot be applied to large scale in industrial production because of the problems of harsh process conditions, high equipment requirements, high production energy consumption and the like. Meanwhile, due to the limitation of equipment conditions, the compression rate of wood is generally less than 50% (too high compression rate can cause crushing of wood cell walls and can reduce mechanical properties of wood), and the degree of densification is not fully exerted by the action of microstructure units with ultrahigh strength in the wood, namely oriented microfibrils (the grain-oriented tensile strength of which is generally more than 480 MPa), so that the degree of improvement of mechanical strength of the fast-growing wood subjected to conventional hot-pressing compression densification is limited. Therefore, if the processing energy consumption can be reduced and the processing technology can be optimized on the basis of the traditional wood hot-pressing compression densification enhancement technology, such as avoiding the high-temperature hot-pressing compression technology and the secondary shaping heat treatment, and fully playing the advantages of the wood with super-strong structural units to realize the wood densification enhancement, the method has more practical significance for realizing the high-attachment application of the fast-growing wood.
Disclosure of Invention
The invention aims to utilize the microstructure characteristics of a super-strong structural unit, namely microfibrils, of the wood cell wall and the chemical characteristics of the microstructure, induce the wood cell shrinkage and the highly oriented aggregation of the cell wall microfibrils through solvent swelling and evaporation, realize the densification of the wood at normal temperature and normal pressure, and achieve the aim of greatly improving the mechanical strength of the wood.
The technical solution of the invention is as follows: the method for inducing the self-densification of the wood by utilizing the swelling and evaporation of the solvent is completed by the following steps:
1. softening wood:
the wood is put into a softening mixed solution prepared from sodium hydroxide, sodium sulfite and anthraquinone, then added with a solvent with low surface tension and low viscosity, stirred for 10 minutes, and then placed into a stainless steel reaction vessel for softening treatment after being uniformly mixed.
The softening mixed solution is prepared from sodium hydroxide, sodium sulfite and anthraquinone according to the mass ratio of 100-300:300-500:1. The sulfite ion and the anthrahydroquinone ion under the alkaline condition can break the beta-aromatic ether bond of the macromolecular chain of lignin in the wood, so that the lignin is fragmented, and the aim of softening the wood is fulfilled.
The low surface tension and low viscosity solvent is methanol, ethanol, butanol, glycol or acetone, and the addition amount is 10-30wt%. The addition of the organic solvent can convert the solid-liquid interface between the wood and the softening solution into a liquid-liquid interface between the softening solution and the organic solvent, thereby reducing the Laplace pressure of the softening solution entering the wood and enabling the cell walls of the wood to be uniformly softened.
The softening treatment temperature of the wood is 150-180 ℃ and the treatment time is 1-6 h.
2. Swelling treatment of wood solvent:
after the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in dimethyl sulfoxide solution (analytically pure, AR) under normal temperature conditions for swelling treatment. Swelling of dimethyl sulfoxide can weaken strong cohesive force among wood cell wall microfibrils, further improve the plasticity of wood cell walls, and provide space for solvent replacement.
The swelling treatment time of the wood solvent is 12-24 hours.
3. And (3) wood solvent evaporation self-densification treatment:
and after the swelling treatment is finished, the deionized water is repeatedly used for fully replacing the dimethyl sulfoxide, and the deionized water is replaced every 6 hours, wherein the replacement period is 3 times. And then placing the wood in an air environment to naturally evaporate the water in the wood. The capillary force formed in the water evaporation process is utilized to induce the wood cells to shrink at normal temperature and normal pressure, and the cell wall microfibrils shrink along the capillary force action direction and are simultaneously accompanied with the dynamic recombination of hydrogen bonds among cellulose molecules, so that the cell wall microfibrils are highly oriented and aggregated, and the high self-compaction of the wood is realized.
The principle of the wood self-densification method provided by the invention is as follows: the sulfite ions and the anthrahydroquinone ions under the alkaline condition can break the beta-aromatic ether bond of the lignin macromolecular chain in the wood cell wall, so that lignin macromolecules are rapidly degraded into soluble micromolecular fragments, the rigid lignin depolymerizes to soften the wood cell wall, and the elastic modulus of the wood cell wall is obviously reduced; then, the swelling of the wood cell wall is realized by utilizing the permeation of dimethyl sulfoxide molecules among microfibrils, and the plasticity and the deformability of the softened and swelled wood cell wall are greatly improved; and then introducing moisture into the cell cavities and cell walls of the swelled wood, wherein capillary force action and hydrogen bond action of cellulose intermolecular recombination generated in the moisture evaporation process induce wood cell shrinkage and highly oriented aggregation of cell wall microfibrils, so that the high self-compaction of the wood is realized at normal temperature and normal pressure.
The invention has the beneficial effects that:
1. the high-temperature high-pressure is not needed in the wood densification process, the cell shrinkage and the highly oriented aggregation of cell wall microfibrils of the wood are induced through the swelling and the evaporation of the solvent, the high self-densification of the wood is realized at normal temperature and normal pressure, the energy consumption in the processing process is obviously reduced, the processing technology and equipment are simplified, and the tree species and the specification size of the processed wood are not limited.
2. Fully plays the advantage of the mechanical strength of the wood ultrastructural unit, namely the oriented microfibrils, and greatly improves the strength of the densified wood. The grain-oriented tensile strength of the self-densified wood prepared by the method reaches more than 400MPa, which is 5-45 times that of natural wood, and the specific strength of the self-densified wood is even more than that of some engineering plastics and light alloy materials, such as acrylonitrile-butadiene-styrene copolymer (30.92 MPa cm) 3 g -1 ) Stainless steel (66.35 MPa cm) 3 g -1 ) 4Ni-Cr-Mo steel (198.03 MPa cm) 3 g -1 ) Light aluminum alloy (178.52 MPa cm) 3 g -1 ) 4Sn-4Al-4Mo-0.5Si alloy (309.15 MPa cm) 3 g -1 )。
3. The water molecule evaporation process causes recombination of hydrogen bonds among cellulose molecules, and a strong hydrogen bond network formed in molecules and among molecules ensures tight arrangement among wood microfibrils, so that rebound deformation of the densified wood is obviously inhibited, the problem that the traditional hot-pressing compression densified wood is poor in dimensional stability and needs secondary heat treatment for shaping is solved, and the processing technology is further simplified.
Drawings
FIG. 1 is a scanning electron microscope image of a cross section of a wood material when a solvent (moisture) is evaporated for 0h under normal temperature and pressure conditions in a self-densified wood material according to embodiment 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a cross section of a self-densified wood of example 1 of the present invention when the solvent (water) is evaporated for 10 hours at ambient temperature and pressure.
FIG. 3 is a scanning electron micrograph of a cross section of a self-densified wood of example 1 of the present invention when the solvent (water) is evaporated for 20 hours at ambient temperature and pressure.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and the following examples are only for more clearly illustrating the technical aspects of the present invention, and are not to be construed as limiting the scope of the present invention.
Example 1
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 100:300:1, and 10wt% ethanol (analytically pure, AR) is added and fully stirred for 10 minutes. The bassa was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 150 ℃ for 1h. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood. As shown in FIG. 1, the cross-section scanning electron microscope image of the self-compacting wood is obtained by evaporating the solvent (water) for 0h under the condition of normal temperature and normal pressure. Before the water begins to evaporate, the balsa wood cells are in a honeycomb-like porous structure, and the cell cavity diameter is in the range of 50-100 mu m. FIG. 2 is a scanning electron microscope image of the cross section of the self-compacting wood after the water is evaporated for 10 hours under the condition of normal temperature and normal pressure. The balsa wood cells shrink under the action of capillary force, the cell cavity is obviously reduced, the diameter is within the range of 5-20 mu m, and the balsa wood cells are in a flat porous structure. Fig. 3 is a scanning electron microscope image of the cross section of the self-densified wood after the moisture of the self-densified wood is evaporated for 20 hours at normal temperature and normal pressure. As the moisture evaporates completely, the porous structure of the wood cells disappears, the wood cells are sufficiently densified, and the wood cell wall structure is not destroyed.
Example 2
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 100:300:1, and 10wt% ethanol (analytically pure, AR) is added and fully stirred for 10 minutes. Then putting the fast-growing poplar into the mixed solution and putting the fast-growing poplar and the mixed solution into a stainless steel reaction vessel together, and treating the fast-growing poplar for 1h at the temperature of 150 ℃. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Example 3
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 100:300:1, and 10wt% ethanol (analytically pure, AR) is added and fully stirred for 10 minutes. Birch was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 150 ℃ for 1h. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Example 4
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 300:500:1, and 10wt% ethanol (analytically pure, AR) is added and fully stirred for 10 minutes. The bassa was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 150 ℃ for 1h. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Example 5
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 300:500:1, and 30wt% ethanol (analytically pure, AR) is added and fully stirred for 10 minutes. The bassa was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 150 ℃ for 1h. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Example 6
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 300:500:1, 30wt% of methanol (analytically pure, AR) is added, and the mixture is fully stirred for 10 minutes. The bassa was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 150 ℃ for 1h. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Example 7
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 300:500:1, 30wt% of methanol (analytically pure, AR) is added, and the mixture is fully stirred for 10 minutes. The bassa was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 180 ℃ for 1h. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Example 8
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 300:500:1, 30wt% of methanol (analytically pure, AR) is added, and the mixture is fully stirred for 10 minutes. The bassa was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 180 ℃ for 3 hours. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 24 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Example 9
Sodium hydroxide, sodium sulfite and anthraquinone are prepared into a softened mixed solution according to the mass ratio of 300:500:1, 30wt% of methanol (analytically pure, AR) is added, and the mixture is fully stirred for 10 minutes. The bassa was then placed in the mixed solution and placed together in a stainless steel reaction vessel and treated at 180 ℃ for 3 hours. After the softening treatment is finished and cooled to room temperature, the softened wood is sufficiently washed with water to remove the reaction residual reagent, and then the wood is soaked in a dimethyl sulfoxide solution (analytically pure, AR) at room temperature for swelling treatment for 12 hours. And repeatedly using deionized water to fully replace dimethyl sulfoxide after the swelling treatment is finished, wherein the deionized water is replaced every 6 hours, and the replacement period is 3 times. And then placing the wood in an air environment, and inducing the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils by utilizing capillary force action formed by natural evaporation of water and hydrogen bond action of recombination between cellulose molecules at normal temperature and normal pressure to realize the highly self-compaction of the wood.
Examples 1, 2, 3, 4, 5, 6, 7, 8, 9 (different tree species, different proportions of softening mixture, different organic solvents, different softening treatment times, different swelling times) were prepared and the results of the measurements of the grain-following tensile strength, density and specific strength of the obtained self-densified wood are shown in the following table:
note that:
(1) the tensile strength results were obtained by testing with a universal mechanical tester (Instron 5966) at a test speed of 5mm min -1 Test environment (25±1 ℃,50% rh);
(2) wood density testing methods were tested according to the standard of wood density determination method (GB/T1933-2009).
Claims (6)
1. A method for inducing wood self-densification by using solvent swelling and evaporation is characterized in that: the method comprises the following steps:
step one: softening wood: placing wood into a softened mixed solution prepared from sodium hydroxide, sodium sulfite and anthraquinone, adding a low-surface tension and low-viscosity solvent, stirring for 10 minutes, uniformly mixing, and placing into a stainless steel reaction vessel for softening treatment;
step two: swelling treatment of wood solvent: after the softening treatment is finished and the wood is cooled to room temperature, fully washing the softened wood to remove a reaction residual reagent, and soaking the wood in a dimethyl sulfoxide solution (analytically pure, AR) under the normal temperature condition for swelling treatment;
step three: and (3) wood solvent evaporation self-densification treatment: and after the swelling treatment is finished, the deionized water is repeatedly used for fully replacing the dimethyl sulfoxide, the deionized water is replaced every 6 hours, the replacement period is 3 times, then the wood is placed in an air environment, so that the moisture in the wood is naturally evaporated, and the capillary force action and the hydrogen bond action of cellulose intermolecular recombination formed in the moisture evaporation process are utilized to induce the shrinkage of wood cells and the highly oriented aggregation of cell wall microfibrils at normal temperature and normal pressure, so that the high self-compaction of the wood is realized.
2. A method for inducing self-densification of wood by means of swelling and evaporation of a solvent according to claim 1, characterized in that: the softened mixed solution in the first step is prepared from sodium hydroxide, sodium sulfite and anthraquinone according to the mass ratio of 100-300:300-500:1.
3. A method for inducing self-densification of wood by means of swelling and evaporation of a solvent according to claim 1, characterized in that: the low surface tension and low viscosity solvent in the first step is methanol, ethanol, butanol, glycol or acetone, and the addition amount is 10-30wt%.
4. A method for inducing self-densification of wood by means of swelling and evaporation of a solvent according to claim 1, characterized in that: the softening treatment temperature of the wood in the first step is 150-180 ℃ and the treatment time is 1-6 h.
5. A method for inducing self-densification of wood by means of swelling and evaporation of a solvent according to claim 1, characterized in that: the wood in the first step is coniferous wood or hardwood.
6. A method for inducing self-densification of wood by means of swelling and evaporation of a solvent according to claim 1, characterized in that: and step two, the swelling treatment time of the wood solvent is 12-24 hours.
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