CN101745951B - Modified planted forest timber and preparation method thereof - Google Patents
Modified planted forest timber and preparation method thereof Download PDFInfo
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- CN101745951B CN101745951B CN 200910243390 CN200910243390A CN101745951B CN 101745951 B CN101745951 B CN 101745951B CN 200910243390 CN200910243390 CN 200910243390 CN 200910243390 A CN200910243390 A CN 200910243390A CN 101745951 B CN101745951 B CN 101745951B
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Abstract
The invention discloses impregnation reinforcement-thermal treatment modifying technology for planted forest timber. The technology comprises the following steps in order: 1) impregnating the timber by adopting impregnation liquid which uses modified urea resin as a main agent of the impregnation liquid; and 2) thermally treating the impregnated timber in vacuum. The timber prepared by the methodhas high dimensional stability and high strength; the bulking resistance and the corrosion resistance of the timber are improved; the added value of the thermally-treated timber is improved; and the application range of the thermally-treated timber is expanded.
Description
Technical field
The present invention relates to a kind of modification processing method of timber, particularly a kind of timber pickling-heat-treating methods.
Background technology
Along with the development of national economic development and the raising of living standards of the people, people are increasing to the demand of timber.And the enforcement of wildwood protected project makes that the timber disparities between supply and demand are more outstanding.For alleviating imbalance between supply and demand, China has built large-area Industrial Plantation.Though artificial forest wood has advantages such as fast growing, the physical and mechanical property of artificial fast-growing woods timber is relatively poor, and density is low, and material is soft, easily produces dry-shrinkage deformed.
In order to expand the range of application of artificial forest wood, improve the economic worth of artificial forest wood, people in all sorts of ways artificial fast-growing woods timber are carried out modification.What research was more at present is to adopt thermosetting resin that timber is carried out impregnation process, and thermoset synthetic resin resistance to water after curing is strong, do not run off, and also the intensity height, cannot not be heated softeningly, be applicable to impregnated timber.The synthetic resin that is used for impregnated timber must have the low characteristics of viscosity, otherwise can't fully flood timber.The height of the degree of polymerization is the principal element of decision tree impregnate with tallow treatment effect quality, so should adopt the initial stage resin of low polymerization degree.At present existing many dissimilar resins can be successfully in the timber interior polymeric, as phenolic resins (PF), Lauxite (UF), melamino-formaldehyde (MF) and isocyanates etc.Concrete impregnation process mode be with timber pickling in the resin solution of water-soluble low molecular weight, resin diffuses in the wood cell and makes the timber increase-volume, drying is removed moisture, resin is owing to heating is solidified, generate water-insoluble polymer, deposition is filled in the cell, or crosslinked with the wood components generation, and density of wood increase, hardness and intensity improve, the dimensionally stable property improvement thereby make.
Enhancing along with people's environmental consciousness, the Wooden modifying expert invests the heat treatment wood of comparatively environmental protection to sight, is mainly carbonized wood, utilizes high temperature (about 200 ℃) to handle timber, improved wood dimensional stability, following four kinds of Technologies for Heating Processing wherein more typically arranged:
1. the Thermwood technology of Finland
The Thermwood process divides 3 stages to carry out: the phase I, and adopt heat and steam to make timber intensification in the dry kiln, and at high temperature drying make the humidity of timber reduce to zero, the temperature of dry kiln is rapidly heated to about 100 ℃, steadily is warming up to 130 ℃ afterwards; Second stage is the high-temperature heat treatment timber stage, and promptly the temperature in the dry kiln raises and remains 185 ℃～230 ℃, after reaching target temperature, remains on heat treatment 2h～3h under this temperature; Phase III, timber was lowered the temperature with water injection system after the heat treatment soon processing stage of being cooling and damping; When temperature is reduced to 80 ℃～90 ℃, readjusts humidity and make moisture content reach 4%～7%.It is pine, China fir, poplar and birch that Thermwood technology is mainly handled seeds.Timber after the heat treatment is mainly used in outdoor, for example: deck, fence, garden furniture, door, window etc.Indoor as kitchen furniture, main hall and panel etc.
2. He Lan Plato Wood technology
Plato Wood technology not only can be handled greenwood but also can handle air-dired wood, this technology divided for four steps carried out: the first step, hydrothermal treatment consists (hydrothermolysis): under the condition of normal pressure, it is 160 ℃～190 ℃ wet environment that timber is placed temperature, handles 4h～5h; Second step, the drying of wood:, the drying of wood to moisture content is lower than 10% with traditional drying technology with 3 days～5 day time; In the 3rd step, heat treatment: timber is heated to 170 ℃～190 ℃, and the processing time is 14h～16h; The 4th step, normally wood equilibrium moisture content is improved, make it with atmospheric environment in quite.This processing method by Arnhem (Holland) factory application in commercially producing, yearly productive capacity reaches 35000m
3
3. state-owned two kinds of production technologies of method: Rectification technology and Boisperdure technology
Rectification technology is to handle timber in 200 ℃～240 ℃ nitrogen, and the moisture content of handling material is 12%; And Boisperdure technology is rapid draing greenwood in 200 ℃～240 ℃ steam.
4. De Guo OHT treatment process
The OHT treatment process adopts oil as heat-treatment medium, at high temperature handles timber.At first timber is put into a closed container that is full of deep fat and handled 18h～24h.Oil has good heat conduction and anoxybiotic ability.But unfavorable conditions is that oil will immerse timber inside makes timber weight increase by 50%～70%, and heat-treated wood has greasy smell.
Above-mentioned four kinds of heat treatment process are numerous and diverse, the process conditions harshness, the control difficulty, the stability of product quality is difficult to guarantee, the treatment process that has also needs special heat-treatment medium, for example: the Rectification arts demand nitrogen of France, the OHT treatment process of Germany need oil as heat-treatment medium.
Though timber can improve its size stability after the heat treatment modification, equilibrium moisture content in the timber descends, corrosion resistant performance also increases to some extent, bonding capacity improves, and wood color deepens, and has improved the relatively poor timber outward appearance of outward appearance, yet the physical and mechanical property of the timber after the heat treatment descends, it is bigger that the strength of wood value descends, as: bending strength reduces, degradation under the surface wettability, has limited the range of application of carbonized wood to a great extent.
Summary of the invention
The objective of the invention is problem, a kind of improved wood and preparation method thereof is provided at the prior art existence, its dimensional stability height of timber of this method preparation, the strength of wood height, bloated performance of moisture-resistant and decay resistance increase.
For realizing purpose of the present invention, one aspect of the present invention provides a kind of preparation method of improved wood, comprises following step in sequence: 1) modified cyanurotriamide Lauxite, water and auxiliary agent are mixed, make timber pickling liquid; 2) timber is carried out the vacuum pressed impregnation process, make timber absorption maceration extract; 3) timber after the impregnation process is heat-treated under vacuum state.
Wherein, the auxiliary agent described in the step 1) is dextrin, nano silicon and nano titanium oxide.
Particularly, the weight portion proportioning of described modified cyanurotriamide Lauxite, water, dextrin, nano silicon and nano titanium oxide is 10-40: 50-83: 5-10: 1-10: 1-10.
Wherein, the preparation of the described modified cyanurotriamide Lauxite of step 1) comprises the steps:
A) prepare raw material according to following weight portion proportioning:
Melamine 350～470
Methyl alcohol 170～240
Formaldehyde 500～540
Urea 50～170
B) melamine and formaldehyde are added in the reactor, the pH value that the back adding NaOH that stirs is regulated melamine and formaldehyde mixed solution, heat temperature raising reacts, make reactant liquor, wherein, pH value after the adjusting is 9.0～9.5, and reaction temperature is 75 ℃～85 ℃, and the reaction time is 30～50min;
C) reacting liquid temperature in the reactor is reduced and remain 65 ℃～75 ℃, add pH value 〉=12 of sodium hydroxide solution conditioned reaction liquid then;
D) in reactor, add methyl alcohol and first urea and carry out modified-reaction, reduce the temperature to 60 ℃ of reactor～70 ℃ behind reaction 50～70min, obtain cooling fluid;
E) add hydrochloric acid, regulate pH value to 8.5～9.5 of cooling fluid, add the urea of surplus then, stir, make the urea dissolving, obtain mixed liquor;
F) add pH value to 7～8 that hydrochloric acid is regulated mixed liquor, cooling then, making mixed liquor is that to add sodium hydroxide solution adjusting pH value after reacting 30～90min under 50 ℃～65 ℃ the condition in reactor be 10～11 in temperature, cooling discharge.
The addition of first urea particularly, step D) be urea total amount 0～89%; Step
F) reaction time described in is 60-90min.
Especially, step B) and step F) described in the mass percent concentration of NaOH be chosen as 15%～25%; The mass percent concentration of NaOH step C) is chosen as 30%～50%; Step e), the mass percent concentration of hydrochloric acid is chosen as 10%～15% step F).
Wherein, the impregnation process step 2) comprises the steps:
A) timber in the impregnating autoclave is carried out decompression vacuum pumping and handles, wherein for the first time the relative pressure handled of decompression vacuum pumping be-0.07MPa～-0.09MPa, vacuumizing the processing time is 0.5h～1.5h;
B) add the cyanurotriamide modified urea resin maceration extract in impregnating autoclave, carry out impregnating by pressure and handle, wherein the relative pressure of impregnating by pressure processing is 0.7～2.5MPa, and the processing time is 1.5h～2.5h.
Particularly, step 2) comprise the steps: C) timber carried out second time decompression vacuum pumping handle, wherein, for the second time the relative pressure handled of decompression vacuum pumping be-0.07MPa～-0.09MPa, vacuumizing the processing time is 0.5h～1.0h.
Especially, after carrying out before the second time, decompression vacuum pumping handled, also being included in pressurized treatments, release, making the relative pressure in the impregnating autoclave is 0MPa, and is under the 0MPa condition at relative pressure, maceration extract soaks timber 0.2h～0.5h.
Particularly, the solids content of cyanurotriamide modified urea resin maceration extract is 10%～50% step B).
Wherein, the timber after the impregnation process is heat-treated under vacuum state described in the step 3) comprises the steps:
A) timber after the impregnation process is carried out drying, make dry impregnated timber, wherein, baking temperature is 50 ℃-100 ℃, and be 10 days～20 days drying time;
B) dry impregnated timber being carried out vacuum heat, wherein heat treated relative pressure is-0.07～-0.096MPa, heat treatment temperature is 160-240 ℃, heat treatment time is 2-10h.
Particularly, steps A) drying described in is to adopt the gradient increased temperature mode to carry out described drying, and baking temperature is from 50 ℃ of gradient increased temperatures to 100 ℃, and wherein, per 10 ℃ is a heating gradient, 2 days～3 days drying time of the baking temperature of each gradient;
Particularly, step B) vacuum heat described in is at first timber to be placed the vacuum high-temperature heat treatment box to carry out decompression vacuum pumping, make relative pressure reach-0.07～-0.096MPa; Heat temperature raising is to described heat treatment temperature then, and wherein, heating rate is 30-50 ℃/h.
Wherein, described timber is artificial forest wood, for example tertia eucalyptus, poplar, masson pine, China fir, paulownia etc.The moisture content of described timber≤15%.
The present invention provides a kind of modified artificial forest wood that is prepared from according to the method described above on the other hand.
Advantage applies of the present invention is in the following areas:
1, the timber of the inventive method preparation, its dimensional stability height, anti-bulking factor, anti-contract with dry rate and decay resistance increase, timber mechanics performance height, intensity height, the added value of raising heat-treated wood, the range of application of expansion heat-treated wood.
2, the improved wood of the inventive method preparation, its dimensional stability height, not yielding, anti-drying shrinkage ability increases, and radially absolutely dry shrinkage is 6.4-6.8%; Tangential absolutely dry shrinkage is 8.2-8.5%.The moisture-resistant ability that expands increases, and radially bulking factor is 6.3-6.7%; Tangential bulking factor is 8.3-8.8%.The improved wood of the inventive method preparation radially, tangential contract with dry rate respectively less than material radially, tangential contract with dry rate; Radially, tangential bulking factor respectively less than material radially, tangential bulking factor.
3, bending strength (MOR) height of the improved wood of the inventive method preparation has reached 131.5-161.7MPa; Bending resistance elastic modelling quantity (MOE) height has reached 16290-17770MPa, compare with material, the mechanical strength height of the improved wood of the inventive method preparation, basic mechanical property with material is suitable, have in addition also have raising.
4, the heat of immersion of the inventive method preparation is handled its mechanical property of improved wood and is improved with respect to the timber of only heat-treating, and dimensional stability is with respect to material and only heat-treat timber significantly raising is arranged.
The specific embodiment
The handled timber of the present invention both can be selected wildwood timber for use, can select the artificial forest fast growing wood for use again, was the preparation process that example describes improved wood of the present invention in detail with tertia eucalyptus (Eucalyptus pellita) in the embodiment of the invention.The tertia eucalyptus is picked up from eucalyptus center, China forest-science academy, Zhanjiang, Guangdong; Making size is respectively 330mm (rift grain direction) * 40mm (tangential) * 40mm () wooden unit radially, thickness direction is according to standard GB 1928-2009 sawing.
Embodiment 1
1, preparation maceration extract stoste
1), preparation maceration extract host
A) prepare raw material according to following weight portion proportioning
Melamine 350g
Methyl alcohol 220g
Formaldehyde 520g
Urea 170g
Wherein: the mass percent concentration of formaldehyde is 37%～40%; The mass percent concentration of methyl alcohol is 99.5%;
B) melamine and formaldehyde are added in the reactor, the back adding mass percent concentration that stirs is 20% sodium hydroxide solution, and the pH value of regulating melamine and formaldehyde mixed solution is 9.2;
C) heating makes the temperature rising of reactor and remains 80 ℃, reacts 40min under this temperature, makes reactant liquor;
D) reacting liquid temperature in the reactor is reduced and remain that to add mass percent concentration after 70 ℃ be 40% sodium hydroxide solution, the pH value of conditioned reaction liquid reaches 13;
E) in reactor, add the urea of 140g and whole methyl alcohol, be cooled to 65 ℃ behind the reaction 60min, obtain cooling fluid;
F) adding mass percent concentration in cooling fluid is 10% hydrochloric acid, after the pH value of regulating cooling fluid is 9.2, adds the urea of surplus, stirs, and urea is dissolved, and obtains mixed liquor;
G) adding mass percent concentration in mixed liquor is after pH value that 10% hydrochloric acid is regulated mixed liquor is 7.5, at 60 ℃ of following stirring reaction 60min, in reactor, add mass percent concentration then and be 20% sodium hydroxide solution regulator solution pH value and be 10.5 back cooling discharges, make modified cyanurotriamide resin solution, i.e. maceration extract host.
Adopt GB/T 14074-2006 " wood adhesive and the resin method of inspection thereof " to detect the main liquid of dipping that is obtained, the performance indications of product are as follows:
The appearance colorless transparency liquid
PH value 10.5
Viscosity (MPa*s, 23 ± 0.5 ℃) 15～17
Solids content (%) 51.3
Water Combination (doubly) 6
Storage period (my god) 〉=60
2), in maceration extract host, add entry and auxiliary agent dextrin, sodium rice silica, sodium rice titanium dioxide, stir and promptly get maceration extract stoste, wherein, the weight portion proportioning of maceration extract host, dextrin, nano silicon, nano titanium oxide and water is 40: 10: 5: 5: 83.
2, impregnation process timber
1) add water in maceration extract stoste and regulate its solids content, stir evenly, making its solids content is 25%, obtains maceration extract;
2) tertia Eucalyptus material is put into impregnating autoclave, the timber that is opposite in the impregnating autoclave carries out the decompression vacuum pumping processing, make the relative pressure in the impregnating autoclave be-0.09MPa, vacuumize handle 1h after, open charging valve, be in 25% the maceration extract suction impregnating autoclave with solids content, after in maceration extract is full of impregnating autoclave, soak behind the timber 0.5h with the high-pressure pump pressurization, relative pressure in the reactor is reached and remain 1.1MPa, timber makes impregnated timber behind the pressurized treatments 2h with this understanding.
3, the drying of timber
Impregnated timber is taken out, gas is done to wood surface maceration extract drying, place then and carry out the gradient increased temperature drying in the drying box, make dry impregnated timber, wherein: baking temperature is from 50 ℃ of gradient increased temperatures to 100 ℃ progressively, per 10 ℃ is a heating gradient, and promptly baking temperature is 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, and be 3 days the drying time of the baking temperature of each gradient.
4, the heat treatment of timber
Dry impregnated timber is placed vacuum high-temperature heat treatment box (the permanent fine horse instrument and equipment in Dongguan Co., Ltd), decompression vacuum pumping, relative pressure in the heat treatment box is reached and remain-0.09MPa, heat temperature raising to 160 ℃ is heat-treated then, wherein, heat temperature raising speed is 30 ℃/h, and heat treatment time is 10h.
5, cooling discharging
Close vavuum pump, the timber after pressurized heat is handled is cooled to room temperature (about 22 ℃) back discharging.
Embodiment 2
1, preparation maceration extract stoste
1), preparation maceration extract host
A) prepare raw material according to following weight portion proportioning
Melamine 470g
Methyl alcohol 170g
Formaldehyde 540g
Urea 50g
Wherein: the mass percent concentration of formaldehyde is 37%～40%; The mass percent concentration of methyl alcohol is 99.5%;
B) melamine and formaldehyde are added in the reactor, the back adding mass percent concentration that stirs is 20% sodium hydroxide solution, and the pH value of regulating melamine and formaldehyde mixed solution is 9.0;
C) heating makes the temperature rising of reactor and remains 75 ℃, reacts 50min under this temperature, makes reactant liquor;
D) reacting liquid temperature in the reactor is reduced and remain that to add mass percent concentration after 65 ℃ be 40% sodium hydroxide solution, the pH value of conditioned reaction liquid reaches 12;
E) in reactor, add whole methyl alcohol, be cooled to 60 ℃ behind the reaction 70min, obtain cooling fluid;
F) adding mass percent concentration in cooling fluid is 10% hydrochloric acid, after the pH value of regulating cooling fluid is 8.5, adds whole urea, and stirring is dissolved urea, obtains mixed liquor;
G) adding mass percent concentration in mixed liquor is after pH value that 10% hydrochloric acid is regulated mixed liquor is 7, at 50 ℃ of following stirring reaction 90min, adding mass percent concentration then and be 20% sodium hydroxide solution in reactor, to regulate pH value be 10 back cooling discharges, make modified cyanurotriamide resin solution, i.e. maceration extract host.
Adopt GB/T 14074-2006 " wood adhesive and the resin method of inspection thereof " to detect the main liquid of dipping that is obtained, the performance indications of product are as follows:
The appearance colorless transparency liquid
PH value 10
Viscosity (MPa*s, 23 ± 0.5 ℃) 14～16
Solids content (%) 50.6
Water Combination (doubly) 6
Storage period (my god) 〉=60
2), in maceration extract host, add entry and auxiliary agent dextrin, sodium rice silica, sodium rice titanium dioxide, stir and promptly get maceration extract stoste, wherein, the weight portion proportioning of maceration extract host, dextrin, nano silicon, nano titanium oxide and water is 10: 5: 10: 10: 50.
2, impregnation of timber is handled
1) add water in maceration extract stoste and regulate its solids content, stir evenly, making solids content is 20%, obtains maceration extract;
2) tertia Eucalyptus material is put into impregnating autoclave, impregnating autoclave is carried out decompression vacuum pumping to be handled, make the relative pressure in the impregnating autoclave be-0.07MPa, vacuumize handle 1.5h after, open charging valve, be in 20% the maceration extract suction impregnating autoclave with solids content, after in maceration extract is full of impregnating autoclave, pressurize with high-pressure pump after soaking timber 0.2h, making the relative pressure in the reactor is 0.7MPa, and timber makes impregnated timber behind the pressurized treatments 2.5h with this understanding.
3, the drying of timber
Impregnated timber is taken out, gas is done to wood surface maceration extract drying, place then and carry out the gradient increased temperature drying in the drying box, make dry impregnated timber, wherein: baking temperature is from 50 ℃ of gradient increased temperatures to 100 ℃ progressively, per 10 ℃ is a heating gradient, and promptly baking temperature is 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, and be 2.5 days the drying time of the baking temperature of each gradient.
4, the heat treatment of timber
Dry impregnated timber is placed vacuum high-temperature heat treatment box (the permanent fine horse instrument and equipment in Dongguan Co., Ltd), decompression vacuum pumping, relative pressure in the heat treatment box is reached and remain-0.07MPa, heat temperature raising to 240 ℃ is heat-treated then, wherein, heat temperature raising speed is 50 ℃/h, and heat treatment time is 2h.
5, cooling discharging
Close vavuum pump, the timber after pressurized heat is handled is cooled to room temperature (about 22 ℃) back discharging.
Embodiment 3
1, preparation maceration extract stoste
1), preparation maceration extract host
A) prepare raw material according to following weight portion proportioning
Melamine 400g
Methyl alcohol 240g
Formaldehyde 500g
Urea 120g
Wherein: the mass percent concentration of formaldehyde is 37%～40%; The mass percent concentration of methyl alcohol is 99.5%;
B) melamine and formaldehyde are added in the reactor, the back adding mass percent concentration that stirs is 20% sodium hydroxide solution, and the pH value of regulating melamine and formaldehyde mixed solution is 9.5;
C) heating makes the temperature rising of reactor and remains 82 ℃, reacts 30min under this temperature, makes reactant liquor;
D) reacting liquid temperature in the reactor is reduced and remain that to add mass percent concentration after 75 ℃ be 40% sodium hydroxide solution, the pH value of conditioned reaction liquid reaches 12.5;
E) in reactor, add 50g urea and whole methyl alcohol, be cooled to 70 ℃ of reaction 60min after, obtain cooling fluid;
F) adding mass percent concentration in cooling fluid is 10% hydrochloric acid, after the pH value of regulating cooling fluid is 9.5, adds remaining urea, stirs, and urea is dissolved, and obtains mixed liquor;
G) adding mass percent concentration in mixed liquor is after pH value that 10% hydrochloric acid is regulated mixed liquor is 7, at 65 ℃ of following stirring reaction 90min, adding mass percent concentration then and be 20% sodium hydroxide solution in reactor, to regulate pH value be 11 back cooling discharges, make modified cyanurotriamide resin solution, i.e. maceration extract host.
Adopt GB/T 14074-2006 " wood adhesive and the resin method of inspection thereof " to detect the main liquid of dipping that is obtained, the performance indications of product are as follows:
The appearance colorless transparency liquid
PH value 11.0
Viscosity (MPa*s, 23 ± 0.5 ℃) 13～15
Solids content (%) 50.1
Water Combination (doubly) 6
Storage period (my god) 〉=60
2), in maceration extract host, add entry and auxiliary agent dextrin, sodium rice silica, sodium rice titanium dioxide, stir and promptly get maceration extract stoste, wherein, the weight portion proportioning of maceration extract host, dextrin, nano silicon, nano titanium oxide and water is 25: 7.5: 1: 1: 67.
2, impregnation of timber is handled
1) add water in maceration extract stoste and regulate its solids content, stir evenly, making its solids content is 22.5%, obtains maceration extract;
2) tertia Eucalyptus material is put into impregnating autoclave, impregnating autoclave is carried out decompression vacuum pumping to be handled, make the relative pressure in the impregnating autoclave be-0.08MPa, vacuumize handle 0.5h after, open charging valve, be in 22.5% the maceration extract suction impregnating autoclave with solids content, after in maceration extract is full of impregnating autoclave, pressurize with high-pressure pump after soaking timber 0.5h, making the relative pressure in the reactor is 2.5MPa, and timber makes impregnated timber behind the pressurized treatments 1.5h with this understanding.
3, the drying of timber
Impregnated timber is taken out, gas is done to wood surface maceration extract drying, place then and carry out the gradient increased temperature drying in the drying box, make dry impregnated timber, wherein: baking temperature is from 50 ℃ of gradient increased temperatures to 100 ℃ progressively, per 10 ℃ is a heating gradient, and promptly baking temperature is 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, and be 2 days the drying time of the baking temperature of each gradient.
4, the heat treatment of timber
Dry impregnated timber is placed vacuum high-temperature heat treatment box (the permanent fine horse instrument and equipment in Dongguan Co., Ltd), decompression vacuum pumping, relative pressure in the heat treatment box is reached and remain-0.096MPa, heat temperature raising to 200 ℃ is heat-treated then, wherein, heat temperature raising speed is 40 ℃/h, and heat treatment time is 4h.
5, cooling discharging
Close vavuum pump, the timber after pressurized heat is handled is cooled to room temperature (about 25 ℃) back discharging.
Embodiment 4
The relative pressure of decompression vacuum pumping treatment step is-0.08MPa except carrying out tertia Eucalyptus material for the first time in the impregnation of timber processing procedure, vacuumizes to handle 1h; The relative pressure of pressurized treatments step is 1.6MPa, and the pressurized treatments time is 2h; Remove the pressure of impregnating autoclave then, making the relative pressure in the impregnating autoclave is 0MPa, at relative pressure is under the condition of 0MPa, soak after the timber 0.5h, discharge maceration extract, timber is carried out the decompression vacuum pumping processing second time, the relative pressure of decompression vacuum pumping processing for the second time is-0.08MPa, vacuumize and handle outside the 0.75h, all the other are identical with embodiment 3.
Reference examples 1
Except not preparing maceration extract stoste, not carrying out the timber pickling processing, all the other are identical with embodiment 1, be that timber only carries out drying, heat treatment and cooling processing successively, and the treatment conditions of dry treatment step, heat treatment step and cooling processing step are identical with embodiment 1 respectively.
Reference examples 2
Except not preparing maceration extract stoste, not carrying out the timber pickling processing, all the other are identical with embodiment 2, be that timber only carries out drying, heat treatment and cooling processing successively, and the treatment conditions of dry treatment step, heat treatment step and cooling processing step are identical with embodiment 2 respectively.
Reference examples 3
Except not preparing maceration extract stoste, not carrying out the timber pickling processing, all the other are identical with embodiment 3, be that timber only carries out drying, heat treatment and cooling processing successively, and the treatment conditions of dry treatment step, heat treatment step and cooling processing step are identical with embodiment 3 respectively.
Reference examples 4
Except not preparing maceration extract stoste, not carrying out the timber pickling processing, all the other are identical with embodiment 4, be that timber only carries out drying, heat treatment and cooling processing successively, and the treatment conditions of dry treatment step, heat treatment step and cooling processing step are identical with embodiment 4 respectively.
Reference examples 5
Not make the tertia Eucalyptus material (material) of any processing, example 5 in contrast.
The 1 timber mechanics performance test of test example
Measure bending resistance elastic modelling quantity (MOE) that embodiment 1-4 and reference examples 1-5 prepare timber, measure the bending strength (MOR) that embodiment 1-4 and reference examples 1-5 prepare timber according to standard GB 1936.2-2009 " Method for determination of the modulus of elasticity in static bending of wood " according to the method for GB/T 1936.1-2009 " Method of testing in bending strength of wood ", testing result sees Table 1.
Table 1 mechanical property testing result
| Bending resistance elastic modelling quantity/MPa | Bending strength/MPa | |
| Embodiment 1 | 17770 | 161.7 |
| Embodiment 2 | 16290 | 131.5 |
| Embodiment 3 | 17160 | 155.5 |
| Embodiment 4 | 17060 | 150.6 |
| Reference examples 1 | 16520 | 147.0 |
| Reference examples 2 | 15360 | 119.2 |
| Reference examples 3 | 15680 | 139.4 |
| Reference examples 4 | 15620 | 138.2 |
| Reference examples 5 | 16920 | 155.4 |
Testing result shows:
1, the bending resistance elastic modelling quantity of timber, bending strength are: material＞heat-treated wood, and under identical heat-treat condition, bending resistance elastic modelling quantity, the bending strength of the timber that the bending resistance elastic modelling quantity of dipping heat-treated wood of the present invention, bending strength are all directly heat-treated greater than not carrying out impregnation process, the timber of promptly only heat-treating is compared the material that does not pass through any processing, its mechanical property obviously descends, without the heat-treated wood of impregnation process, its bending resistance elastic modelling quantity is than the material 2.4-9.2% that descended; Bending strength is than the material 5.4-23.3% that descended; And the mechanical property height of the mechanical property of after-baking timber than the timber of only heat-treating flooded in the present invention.
2, dipping heat-treated wood of the present invention, its bending resistance elastic modelling quantity, bending strength be without the height of the heat-treated wood of impregnation process, quite or slightly raising arranged than the mechanical property of material, and therefore, the mechanical property of the improved wood of the inventive method preparation is good.
The test of test example 2 wood dimensional stabilities
One, wood shrinkage test
Measure the contract with dry rate of the improved wood of embodiment 1-4 and reference examples 1-5 preparation according to standard GB/T 1932-2009 " Method for determination of the shrinkage of wood ".The contract with dry rate computing formula is as follows:
β
max＝(L
max-L
0)/L
0×100
In the formula: β
Max---sample radially or tangential absolutely dry shrinkage, %;
L
Max--when-sample moisture content is higher than fibre saturated point (being moist wood), radially or tangential size, mm;
L
0--when-sample is absolutely dry, radially or tangential size, mm.
The testing result of absolutely dry shrinkage is as shown in table 2:
The testing result of the absolutely dry shrinkage of table 2
Result of the test shows:
1, timber radially, tangential absolutely dry shrinkage is: material＞heat-treated wood, material＞dipping heat-treated wood, and under identical heat-treat condition, dipping heat-treated wood of the present invention radially, tangential absolutely dry shrinkage less than do not carry out that impregnation process directly heat-treats radially, tangential absolutely dry shrinkage, promptly only heat-treat the anti-shrinkage performance that can improve timber, and the inventive method promptly flood after again the timber of heat treatment preparation can further improve the anti-shrinkage performance of timber, effectively improve Wood Dimensional Stability.
2, the absolutely dry shrinkage of the heat of immersion processing improved wood of the inventive method preparation is low, and anti-drying shrinkage ability increases, and radially absolutely dry shrinkage is 6.4-6.8%; Tangential absolutely dry shrinkage is 8.2-8.5%, the improved wood of the inventive method preparation radially, tangential contract with dry rate respectively less than material radially, tangential contract with dry rate.
Two, timber bulking test
Measure embodiment 1-4 and reference examples 1-5 according to standard GB/T 1934.2-2009 " Method for determination of the swelling of wood " and prepare timber from absolutely dry bulking factor when suction is stablized.The computing formula of bulking factor is as follows:
α
max＝(L
max-L
0)/L
0×100
In the formula: α
Max--when-sample absorbs water to dimensionally stable, radially or tangential line bulking factor, %;
L
Max--when-sample absorbs water to dimensionally stable, radially or tangential size, mm;
L
0--when-sample is absolutely dry, radially or tangential size, mm.
The testing result of bulking factor is as shown in table 3:
The testing result of table 3 bulking factor
Result of the test shows:
1, timber from absolutely dry to suction when stablizing, wood radial, tangential bulking factor are: material＞heat-treated wood, material＞dipping heat-treated wood, and under identical heat-treat condition, dipping heat-treated wood of the present invention radially, tangential bulking factor less than do not carry out timber that impregnation process directly heat-treats radially, tangential bulking factor, promptly only heat-treat the bloated performance of the moisture-resistant that can improve timber, and the timber of the heat treatment preparation moisture-resistant that can further the improve timber performance that expands again behind the inventive method dipping is effectively improved Wood Dimensional Stability.
2, the bulking factor of the improved wood of the inventive method preparation is low, and the moisture-resistant ability that expands increases, and radially bulking factor is 6.3-6.7%; Tangential bulking factor is 8.3-8.8%, the improved wood of the inventive method preparation radially, tangential bulking factor be far smaller than respectively material radially, tangential bulking factor.
Claims (8)
1. a Wooden modifying processing method comprises following step in sequence: 1) modified cyanurotriamide Lauxite, water and auxiliary agent are mixed, make timber pickling liquid; 2) timber is carried out the vacuum pressed impregnation process, make timber absorption maceration extract; 3) timber after the impregnation process is heat-treated under vacuum state, wherein the Lauxite of modified cyanurotriamide described in the step 1) is prepared from according to following steps:
A) prepare raw material according to following weight portion proportioning:
B) melamine and formaldehyde are added in the reactor, the pH value that the back adding NaOH that stirs is regulated melamine and formaldehyde mixed solution, heat temperature raising reacts, make reactant liquor, wherein, pH value after the adjusting is 9.0～9.5, and reaction temperature is 75 ℃～85 ℃, and the reaction time is 30～50min;
C) make reactor internal reaction liquid temp remain 65 ℃～75 ℃, add pH value 〉=12 of sodium hydroxide solution conditioned reaction liquid then;
D) add methyl alcohol and first urea in reactor and carry out modified-reaction, reduce the temperature to 60 ℃ of reactor～70 ℃ behind reaction 50～70min, obtain cooling fluid, wherein the addition of first urea is 0～89% of a urea total amount;
E) add hydrochloric acid, regulate pH value to 8.5～9.5 of cooling fluid, add the urea of surplus then, stir, make the urea dissolving, obtain mixed liquor;
F) add pH value to 7～8 that hydrochloric acid is regulated mixed liquor, keeping mixed liquor then is that to add sodium hydroxide solution adjusting pH value after reacting 30～90min under 50 ℃～65 ℃ the condition in reactor be 10～11 in temperature, cooling discharge.
2. Wooden modifying processing method as claimed in claim 1 is characterized in that the auxiliary agent described in the step 1) is dextrin, nano silicon and nano titanium oxide.
3. Wooden modifying processing method as claimed in claim 2, the weight portion proportioning that it is characterized in that described modified cyanurotriamide Lauxite, water, dextrin, nano silicon and nano titanium oxide is 10-40: 50-83: 5-10: 1-10: 1-10.
4. modification processing method as claimed in claim 1 or 2 is characterized in that step 2) comprise the steps:
A) timber in the impregnating autoclave is carried out decompression vacuum pumping and handles, wherein for the first time the relative pressure handled of decompression vacuum pumping be-0.07MPa～-0.09MPa, vacuumizing the processing time is 0.5h～1.5h;
B) add maceration extract in impregnating autoclave, carry out impregnating by pressure and handle, wherein the relative pressure of impregnating by pressure processing is 0.7～2.5MPa, and the processing time is 1.5h～2.5h.
5. Wooden modifying processing method as claimed in claim 4 is characterized in that step 2) comprise the steps:
C) timber is carried out second time decompression vacuum pumping and handles, wherein, for the second time the relative pressure handled of decompression vacuum pumping be-0.07MPa～-0.09MPa, vacuumizing the processing time is 0.5h～1.0h.
6. Wooden modifying processing method as claimed in claim 1 or 2 is characterized in that step 3) comprises the steps:
A) timber after the impregnation process is carried out drying, make dry impregnated timber, wherein, baking temperature is 50 ℃-100 ℃, and be 10 days～20 days drying time;
B) dry impregnated timber being carried out vacuum heat, wherein heat treated relative pressure is-0.07MPa～-0.096MPa, heat treatment temperature is 160-240 ℃, heat treatment time is 2-10h.
7. Wooden modifying processing method as claimed in claim 6, it is characterized in that steps A) described in drying be to adopt the gradient increased temperature mode to carry out described drying, baking temperature is from 50 ℃ of gradient increased temperatures to 100 ℃, wherein, per 10 ℃ is a heating gradient, 2 days～3 days drying time of the baking temperature of each gradient.
8. improved wood is characterized in that being prepared from according to method as described in arbitrary as claim 1-7.
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