CN114953074B - Wood heat treatment method capable of carrying out in-situ restoration and modified wood obtained by same - Google Patents
Wood heat treatment method capable of carrying out in-situ restoration and modified wood obtained by same Download PDFInfo
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- CN114953074B CN114953074B CN202210580334.5A CN202210580334A CN114953074B CN 114953074 B CN114953074 B CN 114953074B CN 202210580334 A CN202210580334 A CN 202210580334A CN 114953074 B CN114953074 B CN 114953074B
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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
- B27K5/0085—Thermal treatments, i.e. involving chemical modification of wood at temperatures well over 100°C
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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
- B27K3/16—Inorganic impregnating agents
Abstract
The invention belongs to the technical field of wood modificationIn particular to a wood heat treatment method capable of carrying out in-situ restoration and modified wood obtained by the same, which comprises the following steps: carrying out high-temperature heat treatment on raw material wood to obtain heat-treated wood; subjecting the obtained heat-treated wood to a treatment containing Ca 2+ Vacuum negative pressure dipping in the ionic salt solution, and drying to obtain dipped wood A; placing the obtained impregnated wood A in a gas containing CO 3 2‑ Vacuum negative pressure dipping in the ionic salt solution to obtain dipped wood B; and (4) desalting the obtained impregnated wood B, and drying to obtain the required modified wood. The method provided by the invention is scientific and reasonable in design, the prepared modified wood has excellent surface hardness, bending strength and thermal stability, the calcium carbonate can be effectively attached to the interior of the thermal modified wood, the effect of in-situ repairing and heat-treating the wood cell wall is achieved, and the method has important values for wood utilization and processing and wood material diversification.
Description
Technical Field
The invention belongs to the technical field of wood modification, and particularly relates to a wood heat treatment method capable of carrying out in-situ restoration and modified wood obtained by the same.
Background
The basic principle of wood heat treatment is that wood is treated at high temperature for a certain time, the cell wall substances of the wood are pyrolyzed and recombined in molecular structures, and the components of the wood are permanently chemically changed, so that the moisture absorption of the treated wood is reduced, the dimensional stability and the weather resistance of the treated wood are improved, and the wood heat treatment is suitable for outdoor floors, outdoor decorative wallboards, garden furniture, wood fences and the like.
The commercial application of the wood heat treatment technology mainly starts in European countries, but in recent years, the domestic heat treatment technology and the commercial popularization and application are obviously improved, and the heat treatment technology or the process is gradually mature. Because of the serious shortage of natural forest resources in China, part of wood processing enterprises begin to turn the attention to the development and utilization of the fast-growing wood of the artificial forest with rich resources, but the artificial forest wood has low density, poor strength grade and low dimensional stability due to high growth speed, and although the dimensional stability of the artificial forest wood can be improved by a heat treatment technology, the strength of the wood is further reduced if the artificial forest wood is directly subjected to heat treatment, so that the use requirement cannot be well met. Aiming at the problems that the wood of the artificial forest has low density and poor strength and is not suitable for being directly used for heat treatment modification, the integrated technology of heat treatment and chemical enhancement modification technology or heat treatment and physical enhancement modification technology combined modification is promoted.
In the prior art, a wood heat treatment method capable of repairing cracks and holes of heat-treated wood cell walls in situ is not found, which causes certain loss of surface strength and bending strength of heat-treated wood, and cannot strengthen heat stability to a certain extent, thereby being not beneficial to the commercial popularization and application of the wood heat treatment technology.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a wood heat treatment method capable of carrying out in-situ restoration and the obtained modified wood.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the wood heat treatment method capable of carrying out in-situ restoration comprises the following steps:
s1, performing high-temperature heat treatment on raw material wood to obtain heat-treated wood;
s2, placing the obtained heat-treated wood in a container containing Ca 2+ Vacuum negative pressure dipping in the ionic salt solution, and drying to obtain dipped wood A;
s3, placing the obtained impregnated wood A in a container containing CO 3 2- Vacuum negative pressure impregnation is carried out in the ionic salt solution to obtain impregnated wood B;
and S4, desalting the obtained impregnated wood B, and drying to obtain the required modified wood.
Further, in the above wood heat treatment method, in step S1, the raw material wood is selected from artificial forest wood.
Further, in the wood heat treatment method as described above, in step S1, the raw material wood is placed in a heat treatment test box, the temperature is slowly raised to a target temperature, and heat preservation is continuously performed at the same temperature, so that the heat-treated wood is obtained.
Further, according to the wood heat treatment method, in the step S1, the raw material wood is protected by steam in a heat treatment test box, the temperature is slowly raised to 100 ℃, and the temperature is kept for 30min; continuously slowly heating to 120-220 ℃ at the heating rate of 5-20 ℃/min, and keeping the temperature for 1-4 h.
Further, as described above, in the heat treatment method for wood, in step S2, the vacuum negative pressure impregnation operation is: will contain Ca 2+ The salt solution of the ions is introduced into the heat-treated wood by a negative pressure vacuum-pumping impregnation method, the temperature is 30-60 ℃, the vacuum degree is-0.09-0.01 MPa, and the salt solution contains Ca 2+ The concentration of the ionic salt solution is 0.4-2.0 mol.L -1 The number of times of vacuum pumping is 1-10.
Further, in the heat treatment method of wood as described above, in step S2, ca is contained 2+ The salt solution of the ions is CaCl 2 、CaBr 2 、CaI 2 One of the solutions.
Further, as described above, in the heat treatment method for wood, in step S3, the vacuum negative pressure impregnation operation is: will contain CO 3 2- The ionic salt solution is introduced into the heat-treated wood by a negative pressure vacuum-pumping impregnation method, the temperature is 30-60 ℃, the vacuum degree is-0.09-0.01 MPa, and the salt solution contains CO 3 2- The concentration of the ionic salt solution is 0.4-2.0 mol.L -1 The number of times of vacuum pumping is 1-10.
Further, the heat treatment method of wood as described above, in step S3, contains CO 3 2- The salt solution of the ions is Na 2 CO 3 、K 2 CO 3 、NH 4 CO 3 One in solution.
Further, as the above-described wood heat treatment method, in step S4, the desalting treatment operation is: and (4) washing the wood subjected to the dipping treatment with water until no by-product is detected.
A modified wood is obtained by the wood heat treatment method.
The invention has the beneficial effects that:
1. the modified wood prepared by the method has excellent surface hardness, bending strength and thermal stability, and the calcium carbonate can be effectively attached to the interior of the thermal modified material, so that the effect of in-situ repairing and heat-treating the wood cell wall is achieved.
2. The wood heat treatment method provided by the invention has the advantages of scientific and reasonable design, simple and convenient overall operation, strong feasibility and important value for wood utilization and processing and wood material diversification.
Of course, it is not necessary for any product to achieve all of the above advantages at the same time in the practice of the invention.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a block diagram of a heat treatment process for wood according to the present invention;
FIG. 2 is CaCO for heat-treated wood in an example of the invention 3 A fill ratio comparison graph;
FIG. 3 is a graph comparing the surface hardness of examples of the present invention and comparative examples;
FIG. 4 is a graph comparing bending strengths of examples of the present invention and comparative examples;
FIG. 5 is a graph showing a comparison of thermal stability of examples and comparative examples of the present invention;
FIG. 6 is a scanning electron micrograph (magnification: 1000) of example 1 of the present invention;
FIG. 7 is a scanning electron micrograph (at 6000 magnifications) of example 1 of the present invention;
FIG. 8 is a scanning electron micrograph (magnification is 1000) of example 2 of the present invention;
FIG. 9 is a scanning electron micrograph (at 6000 magnification) of example 2 of the present invention;
FIG. 10 is a scanning electron micrograph (at 1000 magnifications) of comparative example 1 of the present invention;
FIG. 11 is a scanning electron micrograph (at 1000 magnifications) of comparative example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the present invention provides a wood heat treatment method capable of performing in-situ restoration, comprising the following steps:
s1, performing high-temperature heat treatment on raw material wood to obtain heat-treated wood;
s2, placing the obtained heat-treated wood in a container containing Ca 2+ Vacuum negative pressure dipping in the ionic salt solution, and drying to obtain dipped wood A;
s3, placing the obtained impregnated wood A in a container containing CO 3 2- Vacuum negative pressure dipping in the ionic salt solution to obtain dipped wood B;
and S4, desalting the obtained impregnated wood B, and drying to obtain the required modified wood.
The specific embodiment of the invention is as follows:
example 1
The embodiment provides a wood heat treatment method capable of performing in-situ remediation, which specifically comprises the following operations:
raw materials: sawing poplar into samples with the dimensions as follows: 100mm long, 20mm wide and 5mm thick. The poplar was placed at room temperature for 7 days, and then placed in a drying oven, and dried at 103 ℃ for 6 hours, so that the moisture content of the wood was reduced to 10% (moisture content is less than or equal to 15% and is suitable for the embodiment).
And (3) heat treatment:
1) Placing the dried wood in a heat treatment test box (Shanghai-constant technology Co., ltd., PXR-9), heating to raise the temperature to 200 ℃ at a temperature raising rate of 20 ℃/min, and carrying out heat treatment for 1.5 hours; the water vapor is used as protective gas (the water vapor is generated by adding enough water in a water tank in a heat treatment test box, and the water is volatilized along with the rise of the temperature in the box, so that the protective gas is protected. After the heat preservation treatment is finished, stopping heating, and taking out the wood after the temperature of the wood is reduced to room temperature; and (3) placing the wood in a constant temperature and humidity test box, carrying out humidity conditioning treatment, and adjusting the water content of the wood to 10% to obtain the heat-treated wood.
2) Soaking the heat-treated wood in the solution with the concentration of 0.4 mol.L -1 、0.8mol·L -1 、1.2mol·L -1 、1.6mol·L -1 、2.0mol·L -1 CaCl of 2 Placing the solution in a vacuum test chamber (Shanghai-constant technology Co., ltd., DZF-6020), and performing vacuum negative pressure dipping treatment; the solution concentration is 60 ℃, the times of vacuum pumping are 4 times, the vacuum degree is-0.09 Mpa, and the pressure maintaining time is 4 hours. After the pressure maintaining is finished, releasing the pressure, and drying for 6 hours at 60 ℃;
3) Placing the dried wood into a container with the concentration of 0.4 mol.L -1 、0.8mol·L -1 、1.2mol·L -1 、1.6mol·L -1 、2.0mol·L -1 Na (b) of 2 CO 3 Placing the solution in a vacuum test box, and carrying out vacuum negative pressure dipping treatment; the solution concentration is 60 ℃, the times of vacuum pumping are 4 times, the vacuum degree is-0.09 Mpa, and the pressure maintaining time is 4 hours. And after the pressure maintaining is finished, releasing the pressure, and drying for 6 hours at 60 ℃.
4) Placing the dried wood in water for desalination treatment until no chloride ions are detected; and (3) drying the wood subjected to the desalting treatment for 6 hours at the temperature of 60 ℃ to obtain the modified wood.
In this example, the scanning electron microscope results of the modified wood are shown in fig. 6 and 7.
Example 2
This example was the same as example 1 except that the heat treatment was carried out for 3 hours in step 1).
In this example, the scanning electron microscope results of the modified wood are shown in fig. 8 and 9.
Comparative example 1
Raw materials: sawing poplar into samples with the dimensions as follows: 100mm long, 20mm wide and 5mm thick. Placing poplar at room temperature for 7 days, then placing the poplar in a drying oven, and drying the poplar at 103 ℃ for 6 hours to reduce the water content of the wood to 10%. (Water content. Ltoreq.15% is applicable to this example)
And (3) heat treatment:
1) Placing the dried wood in a heat treatment test box, heating to raise the temperature, raising the temperature to 200 ℃ at a temperature rise rate of 20 ℃/min, and carrying out heat treatment for 1.5 hours; the water vapor is used as the protective gas (the water in the water tank in the heat treatment test box is added with enough water, and the water is volatilized to generate the water vapor along with the rise of the temperature in the box, so that the protective gas is protected. And after the heat preservation treatment is finished, stopping heating, and taking out the wood after the temperature of the wood is reduced to room temperature to obtain the heat-treated wood.
In this comparative example, the scanning electron microscope results of the heat-treated wood are shown in FIG. 10.
Comparative example 2
This comparative example was the same as comparative example 1 except that the heat-treating step 1) was carried out for a heat-preserving time of 3 hours.
In this comparative example, the scanning electron microscope results for the heat-treated wood are shown in FIG. 11.
The correlation performance of the invention is detected as follows:
1. CaCO 3 Filling rate
The test pieces of example 1 and example 2 were measured to have dimensions of 200mm × 150mm × 30mm (length × width × thickness); depending on the poor quality of the wood before and after treatment,calculation of CaCO 3 Filling ratio (WPG,%):
wherein, M 0 For the absolute dry weight of the wood before modification treatment, M 1 The average of the results measured and calculated for the oven-dry weight of the modified wood is shown in fig. 2. As can be seen from fig. 2:
1) Modified Wood prepared in example 1 and example 2, caCO thereof 3 Filling rate with CaCl 2 And NaCO 3 The solution concentration increases.
2) When the concentration of the solution exceeds 1.2 mol.L -1 Post-modified wood CaCO 3 The filling rate amplification is not increased significantly any more.
2. Modified wood surface hardness
The modified wood obtained in example 1 (CaCl) was taken out separately 2 The solution concentration is 1.2 mol.L -1 ，Na 2 CO 3 The solution concentration is 1.2 mol.L -1 And, as test pieces, the materials obtained in comparative example 1 and comparative example 2 were 100mm × 20mm × 5mm (length × width × thickness);
test specimen surface Hardness (HD) using shore durometer: the tested wood sample is placed in a constant temperature and humidity box with the relative humidity of 65 percent and the temperature of 20 ℃ for balancing the moisture content. After the water content of the sample is balanced, the surface of the sample is subjected to hardness test by using a Shore durometer (HS-D, winzhoubao instrument). The test was performed by randomly selecting 10 positions on the surface of each sample, and each experimental group was repeated 3 times. The surface hardness value HD calculation formula is as follows:
in the formula: l is the displacement of the relative pressure foot face of tip when the pressure foot of shore durometer is laminated completely with the sample surface, the unit: mm.
The measurement results are shown in table 1.
Table 1 surface shore hardness of modified wood
| Numbering | Density (kg/cm) 3 ) | Surface Shore hardness (average value) |
| Example 1 | 443.11 | 49.65 |
| Example 2 | 418.08 | 50.38 |
| Comparative example 1 | 410.88 | 41.95 |
| Comparative example 2 | 392.07 | 43.30 |
From table 1, it can be seen that:
compared with comparative example 1 and comparative example 2, the density and surface Shore hardness of the modified wood prepared in example 1 are obviously improved.
3. Bending strength of modified wood
As can be seen from fig. 3:
the modified wood prepared in example 1 has a significantly improved bending strength as compared to comparative example 1 and comparative example 2.
4. Thermal stability of modified wood
As can be seen from fig. 4: compared with comparative example 1 and comparative example 2, the maximum thermal degradation rate of the modified wood prepared in example 1 is reduced by 2.95%/min and 2.54%/min respectively; the carbon residue rate is obviously increased, and the thermal stability of the modified wood is improved.
The surface strength of the modified wood is obviously improved by CaCO 3 Compared with the non-repaired heat-treated wood, the heat-treated wood after in-situ repair is improved by about 18 percent, the bending strength of the wood is improved by about 14 percent, the maximum mass loss rate in the thermal degradation process is reduced by about 19 percent, the pyrolysis residual weight rate is improved by about 9 percent, and the utilization value of the heat-treated wood is greatly improved.
The preferred embodiments of the present invention disclosed above are intended to facilitate the explanation of the present invention only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand the invention for and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. The wood heat treatment method capable of carrying out in-situ restoration is characterized by comprising the following steps:
s1, performing high-temperature heat treatment on raw material wood to obtain heat-treated wood;
the raw material wood is protected by steam in a heat treatment test box, slowly heated to 100 ℃, and kept for 30min; continuously heating to 120-220 ℃ at the heating rate of 5-20 ℃/min, and keeping the temperature for 1-4 h;
s2, placing the obtained heat-treated wood in a container containing Ca 2+ Vacuum negative pressure dipping in the ionic salt solution, and drying to obtain dipped wood A;
the vacuum negative pressure impregnation operation comprises the following steps: will contain Ca 2+ Introducing the ionic salt solution into the heat-treated wood by a negative-pressure vacuum-pumping impregnation method, wherein the temperature is 30 to 60 ℃, and the vacuum degree isCa of-0.09 to-0.01 MPa 2+ The concentration of the ionic salt solution is 0.4 to 2.0 mol.L -1 Vacuumizing for 1 to 10 times;
s3, placing the obtained impregnated wood A in a gas containing CO 3 2- Vacuum negative pressure dipping in the ionic salt solution to obtain dipped wood B;
the vacuum negative pressure impregnation operation comprises the following steps: will contain CO 3 2- Introducing the ionic salt solution into the heat-treated wood by a negative-pressure vacuum-pumping impregnation method, wherein the temperature is 30 to 60 ℃, the vacuum degree is-0.09 to-0.01 MPa, and the salt solution contains CO 3 2- The concentration of the ionic salt solution is 0.4 to 2.0 mol.L -1 Vacuumizing for 1 to 10 times;
and S4, desalting the obtained impregnated wood B, and drying to obtain the required modified wood.
2. The wood heat treatment method according to claim 1, characterized in that: in step S1, the raw material wood is selected from artificial forest wood.
3. The wood heat-treatment method according to claim 1, characterized in that: in step S2, ca is contained 2+ The salt solution of the ions is CaCl 2 、CaBr 2 、CaI 2 One of the solutions.
4. The wood heat-treatment method according to claim 1, characterized in that: in step S3, CO is contained 3 2- The salt solution of the ions is Na 2 CO 3 、K 2 CO 3 、（NH 4 ） 2 CO 3 One of the solutions.
5. The wood heat treatment method according to claim 1, characterized in that: in step S4, the desalting process operation is: and (4) washing the wood subjected to the dipping treatment with water until no by-product is detected.
6. A modified wood obtained by the method for heat-treating wood according to any one of claims 1 to 5.
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| FI114920B (en) * | 2002-09-09 | 2005-01-31 | Upm Kymmene Corp | Wood preservatives and process for making the same |
| CN102241032B (en) * | 2011-06-03 | 2013-12-25 | 西北农林科技大学 | Pretreatment method for improving dimension stability of timber |
| CN104890069B (en) * | 2015-06-25 | 2017-04-05 | 安徽农业大学 | A kind of CaCO3/ Wood composite material and preparation method thereof |
| CN104985657B (en) * | 2015-07-06 | 2017-05-17 | 中南林业科技大学 | Enhanced high-temperature heat treated wood and manufacturing method thereof |
| CN105538444B (en) * | 2015-11-27 | 2017-10-24 | 安徽农业大学 | One kind contains CaCO3/Mg(OH)2High-strength anti-flaming composite wood and preparation method thereof |
| CN108297220A (en) * | 2017-12-20 | 2018-07-20 | 宜华生活科技股份有限公司 | Fast growing wood is inorganic modified and microwave treatment combines method of modifying |
| SI25943A (en) * | 2019-12-24 | 2021-06-30 | Zavod Za Gradbeništvo Slovenije | Wood mineralization procedure with acetoacetate solutions for essential wood properties improvement |
| CN113733273A (en) * | 2021-08-24 | 2021-12-03 | 广西大学 | Wood weight increasing and hardening method |
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