KR20150120028A - Heat treatment method of wood and wood-based materials in order to increase decay resistance and durability - Google Patents

Abstract

The present invention relates to a method for heat treatment of woody and woody materials having increased durability and inner appearance, and more particularly, to a woody or woody material which is heat-treated and heat-treated (carbonized) Of wood and woody materials. In addition, since the charcoal significantly increases the durability and internal decay resistance due to the low temperature heat treatment while maintaining the adsorption property, the humidity shielding property, the electromagnetic wave shielding property, the flame retardancy and the air purification function of the charcoal, (Carbonized) wood or ligneous material can be usefully used in various fields using carbonized wood (charcoal) such as eco-friendly materials for ecological restoration and construction materials.

Description

TECHNICAL FIELD [0001] The present invention relates to a heat treatment method for wood and wood-based materials having increased durability and inner appearance,

The present invention relates to a method for the heat treatment of woody and woody materials having increased durability and inner appearance, and a method for producing carbonized wood and woody materials comprising a heat treatment catalyst and heat treatment on wood.

At present, the risk of destruction of natural ecosystem due to indiscreet development is rising in Korea as well as natural disasters. Such ecosystem destruction is expected to have adverse effects not only on the degraded areas but also on surrounding ecosystems, resulting in enormous economic losses. Damaged areas can be stabilized by physical means, but these are costly and do not last as long. Therefore, it is urgent to develop a rapid and effective restoration technology for degraded soils and forests.

Recently, various technologies related to the establishment of vegetation growth have been developed with the aim of ecological restoration of the damaged area. However, most of these ecological restoration materials are mostly inorganic materials such as concrete and metals, and wood preservatives treated with organic chemicals are often used as ecological restoration materials, but there is no specific alternative.

In addition, generally known charcoal (carbonized wood) has far-infrared radiation function, anion emission function, anti-corruption prevention function and deodorization function, and through this function, not only deodorization effect but also harmful heavy metal adsorption removal effect , And various inventions utilizing charcoal have been disclosed. However, since it is known that charcoal has excellent function and role, it is required to manufacture charcoal by treating the charcoal at a high temperature of 300 ° C or higher. There is a disadvantage that it is difficult to do.

On the other hand, domestic restoration and construction contractors are demanding cheap wood materials having functionality such as environment-friendly and excellent durability. Therefore, many researchers are striving to develop wood or lumber materials having environment-friendly and excellent durability , Eco-friendly ecological restoration materials with increased durability, decay resistance and various functions are not known.

On the other hand, Japanese Patent No. 03086058 discloses an improved method of forming a wood by circulating a mixed gas of formaldehyde source and sulfur dioxide under a temperature of 120 캜, as a prior art on a method of producing wood having increased durability or internal consistency And Korean Patent Registration No. 2012-224708 discloses a method for producing a liquefied wood characterized by directly dissolving vegetable organic substances such as wood in an organic solvent and an acid catalyst without pretreatment, Korean Patent Laid-Open No. 10-2011-0012754 discloses a wood carbonized by heat treatment, but there is no known carbonized wood which is improved in durability and internal durability by simultaneously applying a heat treatment catalyst and a heat treatment.

As a result of efforts to develop eco-friendly materials for ecological restoration or construction materials, the present inventors have found that carbonized wood using a heat treatment catalyst and a heat treatment method can preserve the natural environment by using wood as an eco-friendly material, Can be used as wood and lumber materials, and the durability and internal decay resistance are significantly increased while maintaining charcoal's adsorption property, humidity control property, electromagnetic wave shielding property, flame retardance property and air purification function, The carbonized wood or woody material produced by the catalyst and the heat treatment method can be effectively used in various fields using existing carbonized wood (charcoal) such as environmentally friendly ecological restoration material and building material.

It is an object of the present invention to provide a method of heat treatment of woody and woody materials with increased durability and interior finish.

Also provided is a heat-treated catalyst and a carbonized wood and woody material heat-treated at a temperature of 80 to 300 ° C for 10 to 100 minutes, and a method for producing the same.

In addition,

1) treating the wood with a thermal treatment catalyst;

2) heat treating the wood or woody material treated with the thermal catalyst of step 1); And

3) introducing the heat-treated catalyst of step 2) and the heat-treated carbonized wood or lignocellulosic material into the ecological restoration ground.

In order to solve the above-mentioned object, the present invention provides a method for heat-treating (carbonizing) wood and ligneous materials comprising a heat treatment catalyst and heat treatment on wood.

The present invention also provides a method for producing carbonized wood and ligneous material, comprising a heat treatment catalyst and heat treatment on wood.

The present invention also provides a heat treated catalyst and a carbonized wood and woody material heat treated at a temperature of 80 to 300 DEG C for 10 to 300 minutes.

In addition,

1) treating the wood with a thermal treatment catalyst;

2) heat treating the wood or woody material treated with the thermal catalyst of step 1); And

3) introducing the heat-treated catalyst and the heat-treated carbonized wood or lignocellulosic material of step 2) into an ecological restoration site.

The present invention relates to a method for heat treatment of woody and woody materials having increased durability and inner appearance, and more particularly, to a woody or woody material which is heat-treated and heat-treated (carbonized) Of wood and woody materials. In addition, since the charcoal significantly increases the durability and internal decay resistance due to the low temperature heat treatment while maintaining the adsorption property, the humidity shielding property, the electromagnetic wave shielding property, the flame retardancy and the air purification function of the charcoal, (Carbonized) wood or ligneous material can be usefully used in various fields using carbonized wood (charcoal) such as eco-friendly materials for ecological restoration and construction materials.

Fig. 1 is a graph showing the relationship between the compressive strength test specimen (20 mm x 20 mm x 60 mm spec) according to KS F 2006 of Korea Industrial Standard (KS) and the internal test specimen (KS M 1701 of KS) 20 mm x 20 mm x 20 mm dimensions).
FIG. 2 is a graph showing experimental results in which various conditions (temperature, time, catalyst concentration) are combined with a heat treatment operation using a catalyst.
FIG. 3 is a graph showing the degree of carbonization depth through a combination of various conditions (temperature, time, catalyst concentration) of a heat treatment operation using a catalyst.
Fig. 4 is a diagram showing a visual appearance after 3, 7, 15, and 60 days of post-operation of pine and larch pine which were heat-treated using a catalyst.
5 is a graph showing a visual appearance after 3, 7, 15, and 60 days of pest control of a pine tree subjected to heat treatment (105 ° C, 90 minutes) using a catalyst (2.5%, 5%, 10%).
6 is a diagram showing a visual appearance after 3, 7, 15, and 60 days of thrush operation of larchas heat-treated with a catalyst.
Fig. 7 is a SEM photograph showing a cross section of a normal specimen of pine tree and a specimen not subjected to heat treatment after 60 days of operation.
1 and 2: vertical saddle (X500);
3 and 4: preparation (X500); And
5 and 6: full (X500).
Fig. 8 is a SEM photograph showing the radiating section and the tangential section of the wood specimen after 60 days of operation of the normal test piece of pine tree and the non-heat treated test piece.
Radiometric
1 and 2: wall (X500);
3 and 4: wall (X1000);
Tangential
1 and 2: spinning tissue (X500); And
3 and 4: Radial tissue (X1000).
Fig. 9 is a SEM photograph showing a cross-sectional view of a wood specimen after 60 days of loosening of a larch; Fig.
1 and 2: vertical saddle (X500); And
3 and 4: Joe (X500).
FIG. 10 is a SEM photograph showing a radiating section and a tangential section of a wood test piece after 60 days of loosening of the larch. FIG.
Radiometric
1 and 2: wall (X500);
3 and 4: wall (X1000);
Tangential
1 and 2: spinning tissue (X500); And
3 and 4: Radial tissue (X1000).
FIG. 11 is a SEM photograph showing a cross-sectional view of a pine test piece heat-treated with a catalyst. FIG.
FIG. 12 is a SEM photograph showing a spinning section and a tangential section of a pine test piece heat-treated with a catalyst. FIG.
Fig. 13 is a graph showing the weight loss rate of wood after 60 days of plowing operation of pine and larch pine which is heat treated (105 ° C, 90 minutes) according to the catalyst concentration (2.5%, 5%, 10%).
FIG. 14 is a graph showing the weight reduction rate of wood after 60 days of plowing operation of pine and larch pine which is heat treated (90 minutes) by temperature (80 ° C, 105 ° C, 130 ° C) using a catalyst (5%).
FIG. 15 is a graph showing the weight reduction rate of wood after 60 days of post-operation of pine and larch pine, which were heat treated (105 ° C) by time (45 minutes, 90 minutes, 180 minutes) using catalyst (5%).
FIG. 16 is a graph showing the compressive strength and elastic modulus of wood after 60 days of pest control of pine and larch pine, which were heat-treated (105 ° C, 90 minutes) according to catalyst concentrations (2.5%, 5%, and 10%).
FIG. 17 is a graph showing the compressive strength and the elastic modulus of wood after 60 days of plowing operation of pine and larch pine which is heat treated (90 minutes) by temperature (80 ° C, 105 ° C, 130 ° C) using a catalyst (5%).
FIG. 18 is a graph showing the compressive strength and the elastic modulus of wood after 60 days of post-operation of pine and larch pine which was heat treated (105 ° C) by time (45 minutes, 90 minutes, 180 minutes) using catalyst (5%).
19 is a view showing a wood which is selectively carbonized at a portion to be carbonized through the catalyst-use heat treatment method.
FIG. 20 is a view showing a problem caused by an experiment result of combining various conditions (temperature, time, catalyst concentration) with a heat treatment operation using a catalyst.

Hereinafter, the present invention will be described in detail.

The present invention provides a wood and wood material heat treatment (carbonization) method comprising a heat treatment catalyst and heat treatment on wood.

The present invention also provides a method for producing carbonized wood and ligneous material, comprising a heat treatment catalyst and heat treatment on wood.

The wood is pine ( Pinus densiflora ), larch ( Larix kaempferi), wood, veneer (Veneer), plywood (Plywood), PB (Particle Board ), MDF (Medium Density Fiberboard), HDF (High Density Fiberboard), OSB (Oriented Strand Board), flake boards (Flake board), laminating It is preferable to use a block board, a solid wood veneer, a corrugated board, a paper board, a laminate flooring board, a plywood flooring board, a woody louver board and a woody siding board. It is not limited.

The carbonized wood and woody material are preferably used for restoration of ecology and wood for construction, but are not limited thereto.

The heat treatment catalyst is preferably a strong acid, more preferably sulfuric acid, hydrochloric acid or nitric acid, most preferably sulfuric acid, and the heat treatment is preferably heating the wood treated with sulfuric acid.

It is preferable that the heat treatment catalyst is 4 to 12% sulfuric acid, and when the sulfuric acid is 4% or less, carbonization layer formation is not significantly formed, and when the sulfuric acid is treated with 12% The thermal treatment catalyst is preferably 4 to 12% sulfuric acid, more preferably 5 to 10% sulfuric acid, but is not limited thereto.

The heat treatment is preferably performed at a temperature of 80 to 300 ° C for 10 to 300 minutes, more preferably a temperature of 110 to 140 ° C for a time of 80 to 100 minutes, but is not limited thereto. When the heat treatment is performed at a temperature of 80 ° C or lower, when the heat treatment is carried out at a temperature of 300 ° C or higher without exhibiting significant internal resistance and charcoal adsorption, humidity control, electromagnetic wave shielding, flame retardancy, Since the durability which is a disadvantage of general carbonized wood (charcoal) sharply decreases and splitting of wood occurs (cracking), it can not be used as a material for building material and ecological restoration. Therefore, To 300 minutes, and it is more preferable to perform the heat treatment at a temperature of 110 to 140 占 폚 for 80 to 100 minutes.

It is preferable that the carbonized wood has an increased internal durability and decay resistance and it is desirable to maintain the adsorption, humidity control, electromagnetic wave shielding, flame retardancy and air purification function of carbonized wood (charcoal) And increasing durability, the carbonized wood can be used as an eco-friendly material for ecological restoration and construction, but is not limited thereto.

In a specific embodiment of the present invention, the present inventors have observed through visual inspection after the internal test of KS F 2206 of Korea Industrial Standard (KS) after heat treatment with a catalyst on a test piece of wood. As a result, It was confirmed that the growth of mycelium was very slow in all of the larch and the hypha was thinly covered (refer to Figs. 4 to 6).

In addition, the inventors of the present invention found that a test piece subjected to a post-brittle operation for 60 days and a normal test piece that has not been subjected to brittle operation treatment were subjected to a field emission scanning electron microscope As a result, it was confirmed that the mycelial growth was distributed in the vertical skein of the pine specimen in the cross section of the pine specimen. Also, it was confirmed that the mycelium was contained in the lumen of the pine specimen. It was confirmed that mycelium was contained in the lumen and wall pore, and the wall pore was destroyed, and the movement of mycelium through the wall pore was observed. In addition, it was confirmed that mycelial growth was distributed in the spinning structure at the tangential cross section of the post-treated test piece, and perforation occurred in the wall of the canal was observed by mycelium (see FIGS. 7 and 8). In the case of the larch specimens, it was confirmed that the mycelium grows more in the vertical skein than in the normal specimen in the cross section, and the mycelium is contained in the lumen of the cell. And it was observed that the wall of the field and the wall were destroyed. In addition, it was confirmed that mycelial growth was distributed in the radial tissue at the tangential cross section subjected to the post-mortem treatment, and perforation occurred in the wall of the conduit tube by mycelium (see Figs. 9 and 10).

In addition, the present inventors observed the cross section, the radiation cross section, and the tangential cross section of the pine and larch wood treated with the catalytic agent for 60 days by a field emission scanning electron microscope. As a result, No hyphae were observed in the lumen of the heat treated specimens and in the vertical resinous sphere. In the radiated section of the heat treated specimens with high catalyst concentration, there was almost no damage due to hyphae. In the tangential section of the heat treated specimens, (See Figs. 11 and 12).

The inventors of the present invention found that the concentration of the catalyst (2.5%, 5%, 10%) was determined by fixing the heat treatment temperature to 150 ° C. and the heat treatment time to 90 minutes after the heat treatment of the pine and larch timber specimens was performed using a catalyst, . As a result, the weight change rate of treated pine trees was 20.02%, 12.23%, and 10.05% in the condition 1, 2 and 3 treated with the catalyst concentration than the weight reduction rate of 25.51% The weight loss rate of the treated larvae was lower than that of the untreated control group (21.09%) by 8.2%, 2.67% and 2.59%, respectively. (See Table 2 and Fig. 13). The weight change of the treated pine specimen was determined by the change of the weight of the treated pine specimen with that of the normal control group The reduction rate of the weight loss rate of 24.5% was lower than that of 24.05% at 12.59%, 8.50% and 5.47%, respectively. In the case of lumber test specimens, the weight loss rate of 20.98% The weight reduction rates of the treated conditions 1, 2, and 3 were 5.64%, 5.26%, and 3.14%, respectively, indicating that the reduction rate was low under all treatment conditions (see Table 2 and FIG. 14). The weight change of the treated pine specimens was determined by the change of the weight of the treated pine specimens after the heat treatment (45, 90, 180 minutes) by fixing the catalyst concentration to 5% and the heat treatment temperature to 105 ℃. The reduction rate of the weight loss rate of 19.76% was lower than that of 19.76% at 9.77%, 9.91% and 10.03%, respectively. In the case of the larch specimens, the weight loss rate was 14.46% The weight reduction ratios of treated condition 1, 2, and 3 were 8.49%, 5.36%, and 6.08%, respectively, indicating that the reduction rate was low under all treatment conditions (see Table 2 and FIG.

The inventors of the present invention found that the concentration of the catalyst (2.5%, 5%, 10%) was determined by fixing the heat treatment temperature to 150 ° C. and the heat treatment time to 90 minutes after the heat treatment of the pine and larch timber specimens was performed using a catalyst, As a result, the compressive strengths of pine trees were higher than those of the normal control group of 8.18 Mpa. Compressive strengths of 12.96, 26.62, and 24.09 Mpa were higher than those of the control, The compressive modulus of the treated specimens 1, 2, and 3 was higher than that of normal control specimens 2.98 Gpa, 3.98 Gpa, 4.50 Gpa, and 3.97 Gpa, respectively. The compressive strengths of the treated and untreated lobes were 34.73 MPa and 37.52 MPa, respectively, compared to the compressive strength of 32.61 MPa of the normal control except for the compressive strength of 32.23 MPa. The compressive elastic modulus of 4.51 Gpa and 4.97 Gpa were higher than the compressive elastic modulus of 4.51 Gpa of the normal control except for the compressive elastic modulus of 4.39 Gpa (Table 3 and FIG. 16). In addition, the compressive strength and elastic modulus according to the heat treatment temperature (80 ° C, 105 ° C, 150 ° C) were shown by fixing the concentration of the catalyst for heat treatment to 5% and the heat treatment time to 90 minutes. As a result, The compressive strengths of the control specimens 1, 2, and 3 were higher than those of the control specimens 1, 2 and 3 at 25.15 MPa, 27.67 MPa, and 29.03 MPa, respectively. The compressive modulus of elasticity was 34.37 MPa , And compressive modulus of 41.32 MPa, 39.18 MPa and 40.58 MPa, respectively. Compressive strengths of L. lambs were higher than those of normal controls (16.37 Gpa, 41.32 MPa, 39.18 MPa, and 40.58 MPa, respectively) and the compressive modulus was 5.70 Gpa It was confirmed that the compressive elastic modulus of treated condition 1, 2, 3 was high at 6.26 Gpa, 5.99 Gpa and 5.87 Gpa (Table 3 and FIG. 17). In addition, the compressive strength and elastic modulus of the heat treated catalysts were determined by the heat treatment time (45 min, 90 min, 180 min) with the concentration of 5% and the heat treatment temperature of 105 ℃. As a result, The compressive strength of the untreated control group was higher than the compressive strength of 25.12 MPa. The compressive strengths of 1, 2 and 3 were 14.22 MPa, 30.12 MPa and 31.40 MPa, respectively. The compressive elastic modulus was higher than the compressive modulus of 3.40 MPa , And compressive modulus of 4.98 Gpa, 5.07 Gpa and 5.05 Gpa, respectively, were found to be high. The compressive strength of the lumber test specimens was higher than that of the normal control specimens of 17.35 MPa, 39.13 MPa, 37.98 MPa, and 39.03 MPa, respectively. The compressive moduli of 5, It was confirmed that the compressive modulus values 5.54 Gpa, 5.46 Gpa and 5.46 Gpa of the conditions 1, 2 and 3 were all high (Table 3 and FIG. 18).

Therefore, the carbonized wood and woody material using the heat treatment catalyst and the heat treatment method of the present invention can preserve natural environment by using wood which is an eco-friendly material, and it is possible to maintain the natural environment by using the heat treatment catalyst and heat treatment, The carbonized wood and the lignocellulous material can be usefully used for eco-friendly restoration or building materials because it keeps the electromagnetic wave shielding property, the flame retardancy and the air purifying function, and significantly increases the durability and the internal decay resistance.

The present invention also provides a heat treated catalyst and a carbonized wood and woody material heat treated at a temperature of 80 to 300 DEG C for 10 to 300 minutes.

The carbonized wood is preferably used for restoration of ecology or wood for building materials, but is not limited thereto.

The wood may be selected from the group consisting of Pinus densiflora , Larix kaempferi , wood, veneer, plywood, PB, MDF (medium density fiberboard), HDF (high density fiberboard) Strand Board, Flake board, Block board, Solid wood veneer, Corrugated board, Paper, Laminate flooring, Plywood flooring, Woody louver, , Woody siding, but is not limited thereto.

The heat treatment catalyst is preferably a strong acid, more preferably sulfuric acid, hydrochloric acid or nitric acid, most preferably sulfuric acid, and the heat treatment preferably heats the wood treated with the heat treatment catalyst.

The heat treatment catalyst is preferably 4 to 12% sulfuric acid, more preferably 5 to 10% sulfuric acid, but is not limited thereto.

The heat treatment is preferably performed at a temperature of 100 to 160 ° C for 60 to 100 minutes, more preferably at a temperature of 110 to 140 ° C for 80 to 100 minutes, but is not limited thereto.

The ecological restoration wood is preferably, but not limited to, increased internal decay resistance and durability of the wood.

The carbonized wood and ligneous material using the heat treatment catalyst and the heat treatment method of the present invention can preserve natural environment by using wood which is an eco-friendly material, and because of the heat treatment catalyst and the heat treatment, the charcoal has adsorption, humidity control, , Flame retardancy and air purifying function, and significantly increases durability and decay resistance. Therefore, the carbonized wood and the woody material can be usefully used for eco-friendly restoration or construction materials.

In addition,

1) treating the wood with a thermal treatment catalyst;

2) heat treating the wood or woody material treated with the thermal catalyst of step 1); And

3) introducing the heat-treated catalyst of step 2) and heat-treated carbonized wood or lignocellulosic material into an ecological restoration site.

The carbonized wood is preferably used for restoration of ecology or wood for building materials, but is not limited thereto.

The wood may be selected from the group consisting of Pinus densiflora , Larix kaempferi , wood, veneer, plywood, PB, MDF (medium density fiberboard), HDF (high density fiberboard) Strand Board, Flake board, Block board, Solid wood veneer, Corrugated board, Paper, Laminate flooring, Plywood flooring, Woody louver, , Woody siding, but is not limited thereto.

The heat treatment catalyst is preferably a strong acid, more preferably sulfuric acid, hydrochloric acid or nitric acid, most preferably sulfuric acid, and the heat treatment preferably heats the wood treated with the heat treatment catalyst.

The heat treatment catalyst is preferably 4 to 12% sulfuric acid, more preferably 5 to 10% sulfuric acid, but is not limited thereto.

The heat treatment is preferably performed at a temperature of 100 to 160 ° C for 60 to 100 minutes, more preferably at a temperature of 110 to 140 ° C for 80 to 100 minutes, but is not limited thereto.

The ecological restoration wood is preferably, but not limited to, increased internal decay resistance and durability of the wood.

The ecosystem restoration area is preferably a mountainous area, a special area undamaged area, or an urban area ecosystem, but is not limited thereto.

Therefore, the carbonized wood and woody material using the heat treatment catalyst and the heat treatment method of the present invention can preserve natural environment by using wood which is an eco-friendly material, and it is possible to maintain the natural environment by using the heat treatment catalyst and heat treatment, The carbonized wood and the lignocellulous material can be usefully used for eco-friendly restoration or building materials because it keeps the electromagnetic wave shielding property, the flame retardancy and the air purifying function, and significantly increases the durability and the internal decay resistance.

Hereinafter, the present invention will be described in detail by way of examples.

However, the following examples are illustrative of the present invention, and the contents of the present invention are not limited by the examples.

< Example  1> Manufacture of wood test specimens

Pinus densiflora and Larix kaempferi were cut and processed for 4 months or longer and natural drying was carried out. Test specimens of 20 mm x 20 mm x 60 mm specimens were prepared in accordance with KS F 2206 of Korea Industrial Standard (KS) for the production of compressive strength performance test specimens. KS Test specimens of 20 mm x 20 mm x 20 mm were prepared on the basis of M 1701 (Fig. 1).

< Example  2> Method of heat treatment of wood using catalyst

<2-1> Investigation of optimum treatment condition of heat treatment method using catalyst

In order to determine the optimal conditions for the catalytic heat treatment, the parts to be carbonized by various concentrations of sulfuric acid (H ₂ SO ₄ ) were immersed and then heat treated at various temperatures and treatment times.

Specifically, each heat treatment schedule consisted of three steps. In the first step, the heat treatment temperature was set to 130 ° C., the heat treatment time was set to 30 minutes, and the concentration of the catalyst (sulfuric acid) for heat treatment was treated at 2.5%, 5% and 10% Respectively. In the second step, the concentration of the heat treatment catalyst was fixed at 5% and the treatment time was set at 30 minutes. Treatment temperatures were 100 ° C, 130 ° C and 160 ° C. In the third step, the concentration of the catalyst for thermal treatment was fixed to 5% and the treatment temperature was fixed to 130 ° C., and the treating time was divided into 10 minutes, 30 minutes and 60 minutes, and the appearance of the treated state was visually observed. The depth was measured.

As a result, as shown in Fig. 2, it was confirmed that the test piece treated with 2.5% of the catalyst had a lower degree of carbonization than the test piece treated with 5% and 10%. As a result of the treatment according to the carbonization temperature, it was necessary to confirm whether a proper carbonization layer is formed under all the conditions of 100 ° C., 130 ° C. and 160 ° C. and a proper carbonization layer is formed even at a lower temperature. Under the conditions of the carbonization treatment time, the carbonized layer was not formed properly under the conditions of 10 minutes and 30 minutes. Therefore, in order to find the optimal condition, it is necessary to check whether a carbonized layer is formed under a longer time condition (FIG. 2).

Further, as shown in Fig. 3, the carbonization depth measured by the respective treatments showed that the pine wood had a carbonization depth of 5% and 10%, compared with the test pieces treated with 2.5% It was confirmed to be weak. According to the results of treatment by carbonization temperature, proper carbonization depth was formed under all conditions of 100 ° C., 130 ° C. and 160 ° C., and carbonization depth was not formed properly under the condition of carbonization treatment time at 10 minutes and 30 minutes. It was confirmed that the carbonization depth was weak and the carbonization layer was not formed properly regardless of concentration, carbonization temperature, and treatment time, and the catalyst was not sufficiently absorbed during 10 minutes of immersion time when compared with pine trees (FIG. 3) . Further, as shown in FIG. 19, when the heat treatment catalyst of the present invention is subjected to heat treatment after being treated on the wood part to be carbonized, the carbonized part of the wood and the thickness (Fig. 19).

Also, in order to measure the strength reduction rate of the heat treated specimen using the catalyst, the following experiment was conducted.

Specifically, using the strength test specimen prepared in Example 1, the heat treatment temperature was fixed at 130 ° C. and the heat treatment time was set at 60 minutes in the first step, and the concentration of the heat treatment catalyst was adjusted to 2.5%, 5%, and 10% Respectively. In the second step, the concentration of the catalyst for thermal treatment was fixed at 5% and the treatment time was fixed at 60 minutes. Treatment temperatures were 100 ° C, 130 ° C and 160 ° C. In the third step, the concentration of the catalyst for thermal treatment was fixed to 5%, the treatment temperature was set to 130 ° C, and the treating time was divided into 30 minutes, 60 minutes and 180 minutes.

As a result, as shown in FIG. 20, in the case of the test specimen heat-treated with the catalyst, when the concentration of the catalyst was low, the carbonized layer was not adequately formed. On the contrary, when the carbonization temperature was too high, 160 ° C., (Fig. 20). In order to reduce the problem of splitting (cracking of wood) after treatment of catalyst with heat treatment, we selected conditions in which proper catalyst concentration and carbonization temperature were avoided and proper carbonization layer was formed.

&Lt; 2-2 > Method of heat treatment using catalyst

For the heat treatment experiment using the catalyst for the improvement of the internal consistency of the wood, Pinus densifloea ) and larch ( Larix kaempferi ) were tested in the following manner.

Specifically, sulfuric acid (H ₂ SO ₄ ) was used as the catalyst used in the heat treatment method using the catalyst, and a temperature test chamber (MF-22GH) was used as the heat treatment apparatus for the catalyst-based heat treatment method. As shown in Table 1, in order to search for optimal conditions depending on the concentration of the catalyst, the heat treatment temperature was fixed at 105 ° C., the heat treatment time was set at 90 minutes, and the concentration of the catalyst for heat treatment was treated at 2.5%, 5% In order to investigate the optimal conditions depending on the heat treatment temperature, the treatment temperature was fixed to 80 ℃, 105 ℃ and 130 ℃, and the optimal conditions for the heat treatment time were investigated. The treatment temperature was fixed at 5 ° C and the treatment time was 45 minutes, 90 minutes and 180 minutes, respectively (Table 1).

< Example  3> Malfunctioning

In order to test the internal consistency of the wood treated as in the above Example <2-2>, the following operation was carried out.

Specifically, it is known that the common fungus, Fomitopsis palustris) to receive pre-sale from the Forest Research Institute and cultured in PDA (Potato Dextrose Agar, Becton, Dickinson and Comoany sparks, MD 21152) medium on the basis of KS M 2213 regulation. The wood test piece (20 x 20 x 60 mm) prepared in Example 1 was autoclave sterilized at 121 ° C for 15 minutes by autoclave (AC-12, 65L) and allowed to cool for 30 minutes in a desiccator After that, the plastic netting which had been sterilized in an autoclave was put on the plate, and the wood specimens were placed on the autoclave for 60 days at a temperature of 15 ° C with the fiber direction being perpendicular. Observation and photography were performed on days 1, 3, 5, and 7, and then at 7 days intervals.

< Example  4> of wood Internal fertility  evaluation

<4-1> Scanning electron microscope Scanning electron microscope , SEM ) observe

A scanning electron microscope was used to observe the interior of the wood.

Specifically, the specimen was fabricated to a size of 3 x 10 x 3 mm, deposited on the surface of the specimen with Au, and observed under a 15 kV accelerating electron microscope using a scanning electron microscope. The accelerated electron beam is injected onto the sample, and the secondary electrons protruding from the sample are detected by using the secondary electrons, the backscattering electrons, and the X-rays. The detected secondary electrons are transferred to the photomultiplier tube, video amplifier) and analyzed the components of the micron by using a fine X - ray of the surface of the sample in the cathode ray tube (CRT).

<4-2> Measurement of weight reduction rate

In order to measure the weight loss rate of the wood treated by the method of Example <2-2>, the KS F 2206 (weatherability of wood) of Korean Wood Specification (KS) was tested and measured.

Specifically, after the endurance test is completed, the cells attached to the surface of the test piece are wiped clean with a soft brush from flowing water, dried in air for about 20 hours, dried at 60 ± 2 ° C, and the weight (W2) , And the weight loss rate was calculated according to the following formula (1).

[Equation 1]

W1: Weight before dewatering; And

W2: Weight after dewatering.

<4-3> Measurement of strength reduction rate

In order to measure the strength reduction rate of wood treated by the method of Example <2-2>, the following experiment was conducted.

Specifically, the treated specimens for compressive strength performance test were subjected to a humidity-treated test piece in a constant temperature and humidity chamber (temperature 8 ± 1 ° C., humidity 65 ± 3%) and KS F 2206 (wood compression test method) The compressive load was applied parallel to the fiber direction of the test piece. The cross section of the specimen was moved up and down between the load blocks using a universal tensile strength tester (Shimadzu, model EHF-ED10-20L) at a crosshead speed of 1.0 mm / min in accordance with KS F 2206 And a test was conducted so that a uniform load was applied to the cross section. The fiber direction compressive modulus (E _c ) was calculated from the relationship between load and deformation, and the compressive strength (σ _cmax ) in the fiber direction was determined from the maximum load. The compressive strength in the fiber direction and the compressive elastic modulus in the fiber direction were calculated using Equation 2 and Equation 3. The compressive strength (σ ₂ ) and the modulus of elasticity (E ₂ ) of the test specimens subjected to the brittle operation under the same conditions of the compressive strength (σ ₁ ) and the modulus of elasticity (E ₁ ) And 5, respectively.

&Quot; (2) &quot;

P _max : maximum load; And

A: Cross section.

&Quot; (3) &quot;

E _C : compressive modulus of elasticity;

ΔP: maximum load;

l: gauge length; And

Δ _l : compression strain for ΔP.

&Quot; (4) &quot;

σ ₁ : Strength of specimen not subjected to brittle operation; And

σ ₂ : Strength of specimen subjected to post-mortem.

&Quot; (5) &quot;

E ₁ : modulus of elasticity of test piece not subjected to brittle operation; And

E ₂ : Modulus of elasticity of test specimens subjected to brittle operation.

< Example  5> Through gross observation of wood Internal fertility  effect

The wood samples of pine and larch forests which were heat treated with catalysts were visually observed after the internal test carried out in accordance with KS F 2206 of the Korean Industrial Standard (KS).

The specific experimental method was the same as that of the example <2-2> in the case of the heat treatment method using the catalyst, and the boil was operated in the same manner as in <Example 3>.

As a result, as shown in Fig. 4 to Fig. 6, it was confirmed that mycelial growth was very slow in both pine and larch and mycelium was thinly covered (Figs. 4 to 6).

< Example  6> Through anatomical observation of wood Internal fertility  effect

In order to observe the anatomical changes of the wood caused by buufu, the specimens treated with pestle and larch wood for 60 days were treated with field emission scanning electron microscope The cross section, the radiating section, and the tangential section were observed. In addition, the same experiment was carried out on the pine and larch papers which were heat treated with a catalyst, and were subjected to post-operation.

As a specific experimental method, the heat treatment using the catalyst was carried out in the same manner as in Example <2-2>, and all the post-treatment was carried out in the same manner as in <Example 3>. The scanning electron microscopic observation was carried out in the same manner as in Example <4-1>.

As a result, as shown in FIG. 7, it was confirmed that the cross-section of the pine specimen treated with the 60-day post-mortem treatment showed more hyphal distribution in the vertical resinous grooves than the normal specimens not subjected to the thawing treatment. , The cell wall was deteriorated and the cut surface was not cut cleanly, and many wrinkles and dents were generated, and it was confirmed that mycelium was also contained in the cell lumen (FIG. 7). In addition, as shown in FIG. 8, it was confirmed that the pine specimen treated with the 60-day post-treatment for 60 days contained hyphae throughout the intracellular lumens and wall pores, compared with the normal test pieces not subjected to the post- The mycelial migration was observed. In addition, in the tangential section, it can be confirmed that mycelium grows in the spinous tissue as compared with the normal test piece which is not subjected to the post-brittleness treatment.

In addition, as shown in Fig. 9, it can be seen that the cross-section of the Larix test specimens subjected to the post-operation treatment for 60 days has more hyphal distribution than that of the normal test specimens not subjected to the buffing treatment treatment. Even though the section was cut, the cell wall was deteriorated and the cut surface was not cut cleanly, and many wrinkles and dents were generated, and hyphae were also contained in the cell lumen (FIG. 9). In addition, as shown in Fig. 10, it can be seen that the mycelial growth is distributed in the intracellular lumen of the lanceolate test piece subjected to the post-operation treatment for 60 days as compared with the normal test piece not subjected to the post-blooming treatment, . In addition, in the tangential section, it can be confirmed that mycelium grows in the radial tissues compared with the normal test pieces which are not subjected to the buffing treatment.

In addition, as shown in Fig. 11, in the cross section of the test piece subjected to the post-operation treatment for 60 days, it was confirmed that the hypha column, the vertical plastic grooves, and the cell lumen were filled with hyphae as compared with the test piece subjected to the post- And no hyphae were observed in the intracellular lumen and vertical resinous sphere of the heat-treated test pieces having a high catalyst concentration among the test pieces subjected to the post-treatment for 60 days of the heat-treated test pieces using the catalyst (FIG. 11). In addition, as shown in Fig. 12, compared to the test piece subjected to the post-operation treatment for 60 days, compared with the test piece subjected to the post-operation treatment for 60 days in the heat treatment test piece using the catalyst, the mycelium breaks the hole and travels from the conduit to the conduit through the hole Among the test specimens which were subjected to 60 days post-treatment of heat-treated specimens with catalytic agent, there was almost no damage caused by hyphae in the radiative section of the heat-treated specimen with high catalyst concentration. In addition, in the tangential section, the specimen treated with the buffing operation compared to the normal test specimen not subjected to the brittle operation was able to confirm that the hyphae destroyed the radiating structure and filled the radiating tissue, and the heat treatment specimen using the catalyst was subjected to the brittle operation Among the treated specimens, there was almost no damage caused by hyphae on the tangential cross-section of the heat-treated specimen having a high catalyst concentration (Fig. 12).

< Example  7> Through physical observation of wood Internal fertility  effect

<7-1> Weight reduction rate

Pine and larch wood specimens were heat - treated with a catalyst and then subjected to a thaw operation to determine weight loss.

As a specific experimental method, the heat treatment using the catalyst was carried out in the same manner as in Example <2-2>, and all the post-treatment was carried out in the same manner as in <Example 3>. The weight loss rate was measured in the same manner as in Example <4-2>.

As a result, as shown in Table 2 and FIG. 13, the heat treatment temperature was fixed at 105 占 폚 and the heat treatment time was fixed at 90 minutes to show the weight change depending on the catalyst concentration (2.5%, 5%, 10% (10%, 105 ℃, 90 minutes), Condition 2 (5%, 105 ℃, 90 minutes) and Condition 3 (10%, 105 ℃, 90 minutes) The weight reduction ratio of the control group was 20.02%, 12.23%, and 10.05%, respectively, which were less than the weight reduction ratio of 25.51%. The effect of heat treatment of pine wood on heat treatment was found to be greater than that of the control group, and it was confirmed that the internal consistency of the treated specimen was the highest at 10% concentration of catalyst.

In the case of larch, the reduction rate of weight loss of non-treated normal control group was 8.29%, 2.67% and 2.59%, respectively, which was lower than that of control group by 21.09%. In the heat treatment method using the catalyst of lariant, the effect of internal repellency was higher than that of the untreated control, and the concentration of the catalyst was 10%, which indicated that the internal repellency of the treated specimen was the highest (Table 2 and Fig. 13).

Further, as shown in Table 2 and Fig. 14, the weight change was observed according to the heat treatment temperature (80 DEG C, 105 DEG C, 130 DEG C) by fixing the concentration of the catalyst for heat treatment to 5% and the heat treatment time to 90 minutes, The weight change of pine specimen according to Condition 1 (5%, 80 ℃, 90 min), Condition 2 (5%, 105 ℃, 90 min) The weight reduction rates of the control groups 1, 2 and 3 were 12.59%, 8.50% and 5.47%, respectively, which were lower than the weight reduction rate of 24.05% in the control group. The effect of heat treatment on the catalytic use of pine wood was confirmed to be higher than that of the normal control group without treatment, and it was confirmed that the inner resistance of the treated specimens treated at the heat treatment temperature of 130 ° C was the highest.

In the case of the larch specimens, the weight reduction rate of the untreated control group was 5.64%, 5.26%, and 3.14%, respectively, which were lower than those of 20.98%. The heat treatment method using the catalyst of lariant showed that the effect of internal repellency was higher than that of the untreated control, and that the internal resistance of the treated specimen at the heat treatment temperature of 130 ° C was the highest (Table 2 and Fig. 14).

Further, as shown in Table 2 and FIG. 15, the weight change with the heat treatment time (45 minutes, 90 minutes, 180 minutes) was shown by fixing the concentration of the catalyst for heat treatment to 5% and the heat treatment temperature to 105 ° C., The weight change of the pine specimen according to Condition 1 (5%, 105 ° C, 45 min), 2 (5%, 105 ° C, 90 min) It was confirmed that the weight reduction rate of 9.77%, 9.91%, and 10.03% of the weight reduction ratio of 1, 2, and 3 treated at the heat treatment time was lower than that of the weight reduction ratio of 19.76%. The heat treatment method using pine wood showed higher internal effect than the untreated control, and it was confirmed that the internal resistance of the treated specimens was the highest at the heat treatment time of 45 min.

In the case of the larch specimens, the weight reduction ratio of the untreated control group was 8.49%, 5.36%, and 6.08%, respectively, which was lower than that of 14.46% of the untreated control group. The heat treatment method using the catalytic agent of larians showed a higher effect of internal repulsion than the untreated control, and it was confirmed that the inner specimen treated with the heat treatment time of 90 minutes was the highest, but there was no significant difference (Table 2 and Fig. 15 ).

&Lt; 7-2 >

The compressive strength and elastic modulus of the pine and larch wood specimens were tested by post - heat treatment after catalytic treatment.

As a specific experimental method, the heat treatment using the catalyst was carried out in the same manner as in Example <2-2>, and all the post-treatment was carried out in the same manner as in <Example 3>. The weight loss rate was measured in the same manner as in Example <4-3>.

As a result, as shown in Table 3 and FIG. 16, the heat treatment temperature was fixed at 105 占 폚 and the heat treatment time was fixed at 90 minutes, and the compressive strength and elastic modulus according to the concentrations (2.5%, 5%, and 10% , The compressive strength of pine trees according to the conditions 1 (2.5%, 105 ° C, 90 min), condition 2 (5%, 105 ° C, 90 min) and condition 3 (10% The compressive strength of 12.96 Mpa, 26.62 Mpa, and 24.09 Mpa were higher than the compressive strength of 8.18 Mpa in the untreated control group. Compressive elastic moduli were higher than those of normal control, 2.98 Gpa, 3.98 Gpa, 4.50 Gpa and 3.97 Gpa, respectively. The heat treatment method using pine wood showed higher strength than the untreated control, and the strength of the specimen treated with 5% catalyst was the highest.

The compressive strength of the treated larvae was 34.73 Mpa and 37.52 Mpa, respectively, compared with the compressive strength of 32.61 Mpa in the normal control, except for the compressive strength of 32.23 MPa. The compressive modulus of elasticity was 4.51 Gpa and 4.97 Gpa, respectively, which were higher than the compressive modulus of 4.51 Gpa of the normal control, except for the compressive modulus of 4.39 Gpa. The heat treatment method using the catalyst of larians showed no significant difference compared to the untreated control group (Table 3 and Fig. 16).

Further, as shown in Table 3 and FIG. 17, the compressive strength and the elastic modulus according to the heat treatment temperatures (80 ° C, 105 ° C and 130 ° C) were shown by fixing the concentration of the catalyst for heat treatment to 5% and the heat treatment time to 90 minutes, The compressive strength of pine specimens according to heat treatment temperature condition 1 (5%, 80 ℃, 90 min), condition 2 (5%, 105 ℃, 90 min) Compressive Strength of Uncontrolled Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength at 1, 2, 3, The compressive modulus of 1, 2 and 3 was 41.32 MPa, 39.18 MPa and 40.58 MPa, respectively. The strength of the treated specimens treated at 130 ℃ was the highest in the heat treatment method using pine wood.

Compressive Strength of Lumber 1, 2, and 3 treated with Lumber 16.37 Gpa was 41.32 Mpa, 39.18 Mpa, and 40.58 Mpa, respectively, and the compressive modulus of normal control The compressive modulus of compressive modulus of 1, 2, and 3 was higher than that of 5.70 Gpa at 6.26, 5.99, and 5.87 Gpa, respectively. It was confirmed that the heat treatment method using the catalyst of larians showed higher strength than the untreated control, and the heat treatment temperature was the highest at 130 ° C. (Table 3 and FIG. 17).

Further, as shown in Table 3 and FIG. 18, the compressive strength and the modulus of elasticity were shown by the heat treatment time (45 minutes, 90 minutes, 180 minutes) with the concentration of the catalyst for heat treatment being fixed at 5% The compressive strength of pine specimen according to heat treatment time condition 1 (5%, 105 ℃, 45min), 2 (5%, 105 ℃, 90min) Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength of Compressive Strength of 1, 2, 3, , And compressive modulus of 4.98 Gpa, 5.07 Gpa, and 5.05 Gpa were higher than those of the others. The heat treatment method using pine wood showed higher strength than the untreated control, and the strength of the treated specimen treated for 180 min was the highest.

The compressive strengths of the lumber test specimens were 39.13 MPa, 37.98 MPa, and 39.03 MPa, respectively, which were higher than those of the untreated control group (17.35 Mpa). The compressive elastic modulus of the control group The modulus of elasticity of 5.54 Gpa, 5.46 Gpa and 5.46 Gpa were higher than those of 5.12 Gpa. The heat treatment method using the catalyst of lariant showed higher strength than that of the untreated control, and it was confirmed that the strength of the test piece treated with the heat treatment time of 180 minutes was the highest (Table 3 and FIG. 18).

Claims (16)

A method of heat treatment (carbonization) of wood and woody materials comprising a heat treatment catalyst and heat treating the wood.
The method of claim 1, wherein the wood is selected from the group consisting of Pinus densiflora , Larix kaempferi , wood, veneer, plywood, PB, medium density fiberboard (MDF), high density fiberboard (HDF), OSB (Oriented Strand Board) Flake board, block board, solid wood veneer, corrugated board, paper, laminate flooring, plywood flooring, woody louver and woody siding (Carbonization) method for wood and woody materials.
The method of claim 1, wherein the heat treatment catalyst is sulfuric acid, hydrochloric acid, nitric acid.
The method of claim 1, wherein the heat treatment heats the wood.
The method of claim 1, wherein the heat treatment catalyst is 4 to 12%.
The method of claim 1, wherein the heat treatment is performed at a temperature of 80 to 300 ° C for 10 to 300 minutes.
The method of claim 1, wherein the method increases the internal decay resistance and durability of wood and woody materials.
The method according to claim 1, wherein the method further comprises the step of heat-treating the wood and lumber material, characterized in that at least one selected from the group consisting of adsorption, humidity control, electromagnetic wave shielding, flame retardancy, )Way.
A method for producing carbonized wood and woody materials comprising a thermal treatment catalyst and heat treatment on wood.
10. The method of claim 9, wherein the carbonized wood and ligneous material is wood for ecological restoration and building materials.
10. The method of claim 9, wherein the carbonized wood and ligneous material is one or more selected from the group consisting of internal consistency, durability, adsorption, humidity control, electromagnetic shielding, flame retardancy, Method of manufacturing wood and woody materials.
A heat treated catalyst, and a carbonized wood and ligneous material heat treated at a temperature of 80 to 130 DEG C for 10 to 300 minutes.
The carbonized wood and wood material according to claim 12, wherein the heat treatment catalyst is sulfuric acid.
13. Carbonized timber and lumber material according to claim 12, characterized in that the carbonized timber and lumber material is a timber for ecological restoration and building material.
13. The method of claim 12, wherein the carbonized wood and ligneous material is one or more selected from the group consisting of internal repellency, durability, adsorption, humidity control, electromagnetic shielding, flame retardancy, Wood and wood materials.
1) treating the wood with a thermal treatment catalyst;
2) heat treating the wood or woody material treated with the thermal catalyst of step 1); And
3) introducing the heat-treated carbonized wood or lignocellulous material using the heat treatment catalyst of step 2) into the ecological restoration paper.

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