CN115922861B - Composition for wood impregnation, wood prepreg, modified wood, and method for producing same - Google Patents
Composition for wood impregnation, wood prepreg, modified wood, and method for producing same Download PDFInfo
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- CN115922861B CN115922861B CN202310058805.0A CN202310058805A CN115922861B CN 115922861 B CN115922861 B CN 115922861B CN 202310058805 A CN202310058805 A CN 202310058805A CN 115922861 B CN115922861 B CN 115922861B
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- wood
- impregnation
- curing
- composition
- furfuryl alcohol
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims abstract description 182
- -1 maleamic acid compound Chemical class 0.000 claims abstract description 10
- 238000001029 thermal curing Methods 0.000 claims abstract description 9
- 238000001723 curing Methods 0.000 claims description 51
- FSQQTNAZHBEJLS-UPHRSURJSA-N maleamic acid Chemical compound NC(=O)\C=C/C(O)=O FSQQTNAZHBEJLS-UPHRSURJSA-N 0.000 claims description 49
- 150000001875 compounds Chemical class 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 23
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
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- 238000002360 preparation method Methods 0.000 description 2
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Abstract
The present invention relates to a composition for wood impregnation, a wood prepreg, a modified wood, and a method for producing the same. The composition for wood impregnation of the present invention comprises furfuryl alcohol and a maleamic acid compound, wherein the mass of the maleamic acid compound is 0.9 times or more the mass of the furfuryl alcohol. The method for producing the modified wood of the present invention comprises: a) Impregnating wood with the wood impregnating composition of the present invention to obtain a wood prepreg, b) subjecting the wood prepreg to thermal curing.
Description
Technical Field
The invention relates to the field of wood modification, in particular to a composition for wood impregnation, a wood prepreg, modified wood and a manufacturing method thereof.
Background
China is the second largest wood consuming country in the world, and the available area in the existing available forest accounts for only 13% of the total forest area. In addition, compared with materials such as metal, ceramic and the like, the wood is easy to crack during drying, is easy to be eroded by organisms such as mould, termite and the like, the utilization efficiency is seriously reduced, and further unbalance of wood supply and demand is indirectly caused. Under the condition that the market gap of the wood is increasingly enlarged, the poor-quality wood is modified to improve the utilization efficiency of the poor-quality wood, so that the poor-quality wood becomes an effective way for relieving the contradiction between wood supply and demand and protecting the ecological environment in China.
At present, the modification method for wood is mainly divided into four types of heat treatment modification, chemical modification, surface modification and impregnation modification. The heat treatment process degrades amorphous hemicellulose and cellulose, so that the hygroscopicity of the wood is reduced, and the corrosion resistance and durability are greatly improved, but the bonding force of substances in the wood cell wall is reduced, and the whole cell wall becomes loose, so that the mechanical properties such as density, hardness, bending modulus, impact toughness and the like are reduced to different degrees, and further application of the wood in the engineering field is limited. The chemical modification can change the internal structure of the wood, so that the overall performance of the wood is improved, the life cycle of the wood can be greatly prolonged, but a large amount of toxic reagents are used in the chemical modification process, the environment is polluted to a certain extent, and the use of the wood in specific places is limited. Although the surface modification technology can improve the overall performance of the wood and endow the wood with brand-new functions, the technology can not change the internal structure of the wood, the mechanical properties such as bending strength, elastic modulus and the like are not obviously improved, and the application of the wood in the engineering field can be further expanded by combining the wood with other three technologies when the wood is used.
The impregnation modification is a modification method for filling wood by impregnating small molecules and then matching with a curing agent to enable the small molecules to undergo a curing reaction in the wood, so that the internal cavity of the wood is filled, the wood density is improved, and the overall performance of the wood is improved. However, current impregnating solutions are typically urea-formaldehyde resins and phenolic resins, which inevitably lead to pollution by formaldehyde during production and processing.
Accordingly, the prior art is concerned with methods of impregnating wood with furfuryl alcohol resins. For example, patent document 1 proposes a method for improving the performance of wood by a light furfuryl alcohol modified co-densification treatment, specifically, the method comprises 1) subjecting the wood subjected to an oven drying treatment to a vacuum treatment, introducing a furfuryl alcohol modified solution, and carrying out impregnation under vacuum conditions; 2) Heating the impregnating solution obtained in the step 1) to obtain pre-polymerized furfuryl alcohol resin, coating the pre-polymerized furfuryl alcohol resin on the surface of the impregnated modified wood, and standing at room temperature and normal pressure; 3) Low temperature and low pressure modified timber and is dried to absolute dryness. By the method, the advantages of furfuryl alcohol modification and densification treatment can be comprehensively utilized, the tensile strength, the bending strength and the impact toughness of the fast-growing wood are improved, and the water resistance and the moisture resistance of the wood are improved.
Patent document 2 proposes a furfuryl-based wood modifying liquid comprising the following components in mass percent: 10 to 60 percent of furfuryl alcohol, 1.2 to 5.8 percent of catalyst, 1 to 5 percent of stabilizer, 1 to 1.2 percent of urea, 2 to 5.6 percent of maltodextrin, 1.5 to 2.8 percent of toughening agent, 5 to 15 percent of organic solvent and 4.6 to 78.3 percent of water, and the catalyst is compounded by adopting maleic anhydride and triethanolamine, wherein the weight ratio of the maleic anhydride to the triethanolamine is 1:0.1 to 0.5. Through the use of the wood modifying liquid, the anti-loss property, the dimensional stability, the anti-corrosion property and the mechanical property of the wood are improved.
However, the dimensional stability of the modified wood obtained by each of the above techniques using furfuryl alcohol is still insufficient in a wet environment.
Patent literature:
patent document 1: CN 113696291A
Patent document 2: CN 111941570A
Disclosure of Invention
Problems to be solved by the invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a composition for impregnating wood, which is easily available and inexpensive in raw materials, is environmentally friendly, and when the composition is used for impregnating and hot-pressing wood, the obtained modified wood has good toughness and is excellent in dimensional stability under a humid environment.
The technical problem to be solved by the invention is to provide a wood prepreg and modified wood obtained by using the composition for wood impregnation.
The technical problem to be solved by the present invention is also to provide a method for producing a modified wood, which can easily obtain a modified wood having good toughness and also excellent dimensional stability in a wet environment.
Solution for solving the problem
According to the intensive studies of the present inventors, it was found that the above technical problems can be solved by the implementation of the following technical scheme:
[1] a composition for wood impregnation, wherein the composition comprises furfuryl alcohol and a maleamic acid-based compound, and the mass of the maleamic acid-based compound is 0.9 times or more the mass of the furfuryl alcohol.
[2] The composition for wood impregnation according to [1], wherein the composition comprises an amine group-containing compound in an amount of 0.5 to 15% by mass relative to the total amount of the furfuryl alcohol and the maleamic acid-based compound.
[3] The composition for wood impregnation according to [1] or [2], wherein the maleamic acid-based compound is derived from the reaction of maleic anhydride and ammonia.
[4] The composition for wood impregnation according to any of [1] to [3], wherein the mass of the maleamic acid-based compound is 10 times or less the mass of the furfuryl alcohol.
[5] A wood prepreg obtained by impregnating wood with the composition for wood impregnation according to any one of [1] to [4].
[6] A modified wood, wherein it is a cured product of the wood prepreg according to [5].
[7] A method of making a modified wood, wherein the method comprises:
a) Impregnating wood with the composition for wood impregnation according to any one of [1] to [4] to obtain a wood prepreg,
b) Subjecting the wood prepreg to thermal curing.
[8] The production method according to [7], wherein the heat curing is performed by a method comprising atmospheric pressure pre-curing and pressure curing.
[9] The production method according to [8], wherein the atmospheric pre-curing temperature is 20 to 100℃and the atmospheric pre-curing time is 6 to 24 hours.
[10] The production method according to [8] or [9], wherein the press-curing temperature is 100 to 250 ℃, the press-curing pressure is 0.5 to 5MPa, the dwell time of the press-curing is 5 minutes to 6 hours, and the compression ratio of the wood before and after the press-curing is 10 to 70%.
ADVANTAGEOUS EFFECTS OF INVENTION
Through implementation of the technical scheme, the invention can obtain the following technical effects:
the composition for wood impregnation of the present invention comprises furfuryl alcohol and maleamic acid-based compound having a mass 0.9 times or more the mass of furfuryl alcohol, and thus, when the composition is used for impregnating and thermosetting wood, the obtained modified wood has a good rebound resistance and a greatly improved volume wet expansion ratio. In addition, furfuryl alcohol can be sourced from biological sources, and maleamic acid is prepared by ammonifying maleic anhydride, so that raw materials are easy to obtain, the process is simple, and pollution caused by toxic substances such as formaldehyde, phenol and the like is avoided, so that the composition for wood impregnation is environment-friendly.
In addition, in the method for producing a modified wood of the present invention, by using the above-mentioned composition for wood impregnation of the present invention and subjecting the impregnated wood to heat curing (particularly, staged curing including atmospheric pre-curing and press curing), a modified wood having good rebound resistance and a greatly improved volume wet expansion ratio can be easily produced.
Detailed Description
The following describes the present invention in detail. The following description of technical features is based on the representative embodiments and specific examples of the present invention, but the present invention is not limited to these embodiments and specific examples. It should be noted that:
in the present specification, the numerical range indicated by the term "numerical value a to numerical value B" means a range including the end point numerical value A, B.
In the present specification, the numerical ranges indicated by the use of "above" and "below" refer to ranges including the end point values.
In this specification, the numerical ranges indicated by the use of "greater than" and "less than" refer to ranges that do not include the end values.
In the present specification, "%" means weight percent unless otherwise specified.
In the present specification, the meaning of "can" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
In this specification, "optional" or "optionally" means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
In the present specification, "alkyl" or "alkylene" means a linear, branched or cyclic unsubstituted "alkyl" or "alkylene"; "hydroxyalkyl" means a straight, branched, or cyclic "alkyl" or "alkylene" substituted with any number of hydroxyl groups.
Reference throughout this specification to "some specific/preferred embodiments," "other specific/preferred embodiments," "an embodiment," and so forth, means that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the elements may be combined in any suitable manner in the various embodiments.
< composition for Wood impregnation >
The composition for wood impregnation of the present invention comprises furfuryl alcohol and a maleamic acid compound, wherein the mass of the maleamic acid compound is 0.9 times or more the mass of the furfuryl alcohol.
In the present invention, when wood impregnated with the composition for wood impregnation of the present invention is thermally cured, furfuryl alcohol is polycondensed, and the maleamic acid-based compound itself undergoes a cyclization reaction forming an imide structure in addition to functioning as an acid catalyst for the polycondensation of furfuryl alcohol. Further, when the mass of the maleamic acid based compound is 0.9 times or more the mass of furfuryl alcohol, the obtained modified wood material can be made to have a good rebound resistance and a greatly improved volume wet expansion ratio.
In the present invention, from the viewpoint of better achieving the technical effect of the present invention, in some preferred embodiments, the mass of the maleamic acid-based compound is preferably more than 1 times, more preferably 1.1 times or more, still more preferably 1.15 times or more the mass of furfuryl alcohol.
In the present invention, the upper limit of the mass ratio of the maleamic acid compound to furfuryl alcohol is not particularly limited. However, from the viewpoint of better achieving the technical effect of the present invention and more fully exerting the effect of furfuryl alcohol, in some preferred embodiments, the mass of the maleamic acid-based compound is preferably 10 times or less, more preferably 2.4 times or less, still more preferably 1.2 times or less the mass of furfuryl alcohol.
The composition of the composition for wood impregnation of the present invention is described in detail as follows.
(furfuryl alcohol)
In the present invention, there is no particular limitation on the source of furfuryl alcohol, which may be homemade or commercially available.
Furfuryl alcohol is usually prepared by catalytic hydrogenation of furfural, which can be prepared from rice hulls, wheat hulls, rape stalks, corn stover, corn cobs, bagasse, sunflower stover, cotton seed hulls, and other raw materials.
(maleamic acid-based Compound)
In the present invention, the term "maleamic acid-based compound" is a compound having a maleamic acid structure. In some preferred embodiments, the maleamic acid-based compound is preferably a compound having a structure as shown in the following formula (a) from the viewpoint of being more easily available and better achieving the technical effects of the present invention:
wherein R is 1 And R is 2 Each independently represents hydrogen, an alkyl group having 1 to 22 carbon atoms, or an aryl group having 6 to 22 carbon atoms.
In some preferred embodiments, R 1 And R is 2 Preferably each independently represents hydrogen, an alkyl group having 1 to 12 carbon atoms, or an aryl group having 6 to 14 carbon atoms, more preferably each independently represents hydrogen or an alkyl group having 1 to 5 carbon atoms, and particularly preferably each is hydrogen.
In the present invention, the source of the maleamic acid is not particularly limited and may be homemade or commercially available. In some more preferred embodiments, the maleamic acid compounds of this invention are derived from maleic anhydride and are capable of producing the above-described-NR from a more readily available standpoint 1 R 2 Corresponding amine compounds. In some particularly preferred embodiments, the maleamic acid-based compounds of the present invention are derived from the reaction of maleic anhydride with ammonia.
(other Components)
In the present invention, it is understood that the composition for impregnating wood is in a liquid form, such as a solution or dispersion, etc., as it is used for impregnating wood. The kind of the solvent or dispersion medium contained in the composition for wood impregnation is not particularly limited, and examples of the solvent or dispersion medium include, but are not limited to: water; organic solvents, for example, alcohols such as methanol, ethanol, and the like, ketones such as acetone, methyl ethyl ketone, cyclohexanone, and the like. These solvents may be used singly or in combination of two or more. From the viewpoint of environmental protection, the solvent or dispersion medium contains at least water.
In addition, according to actual needs, the composition for wood impregnation of the present invention optionally contains other components, for example, persulfates, peroxides, acid catalysts, alkaline buffers, inorganic fillers, amine-containing compounds, and the like, in addition to the furfuryl alcohol and maleamic acid-based compounds described above. These other components may be used singly or in combination of two or more.
Examples of persulfates include, but are not limited to, potassium persulfate or ammonium persulfate, and the like. These persulfates may be used singly or in combination of two or more.
Examples of peroxides include, but are not limited to, benzoyl peroxide, phenylacetyl hydroperoxide, isobutyl peroxide, isopentyl peroxide, methylethyl peroxide, and the like. These peroxides may be used singly or in combination of two or more.
Examples of acidic catalysts include, but are not limited to, maleic anhydride, citric acid, oxalic acid, tartaric acid, and the like. These acidic catalysts may be used singly or in combination of two or more.
Examples of alkaline buffers include, but are not limited to, sodium tetraborate, sodium citrate, sodium bicarbonate, sodium carbonate, sodium hydroxide, and the like. These alkaline buffers may be used singly or in combination of two or more.
Examples of inorganic fillers include, but are not limited to, silica, titania, calcium carbonate, barium sulfate, montmorillonite, mica, attapulgite, calcium silicate, and the like. These inorganic fillers may be used singly or in combination of two or more.
Examples of amine-containing compounds include, but are not limited to: amino acids such as glycine, alanine, valine, leucine, isoleucine, lysine, histidine, arginine and the like; polyethylenimine, polypropylenimine, polybutylenimine, polypentenimine, polyhexene, polynonene, polyoctene, and the like; primary amines such as methylamine, ethylamine, propylamine, and the like; secondary amines such as methylethylamine, methylpropylamine, methylbutylamine, and the like; etc. These amine group-containing compounds may be used singly or in combination of two or more. However, in some preferred embodiments, the amine-containing compound does not comprise urea, i.e., the composition of the present invention does not comprise urea.
In some specific embodiments, the composition of the present invention preferably further comprises a persulfate or peroxide from the standpoint of more facilitating the polycondensation of furfuryl alcohol. In this case, the content of the persulfate or peroxide is preferably 0.5 to 5% by mass, more preferably 0.8 to 3% by mass, relative to the total amount of the furfuryl alcohol and the maleamic acid-based compound.
In some specific embodiments, the composition of the present invention preferably further comprises an amine group-containing compound from the viewpoint of better achieving the technical effects of the present invention. In this case, the content of the amine group-containing compound is preferably 0.5 to 15% by mass, more preferably 0.8 to 12% by mass, still more preferably 1 to 9% by mass, relative to the total amount of the furfuryl alcohol and the maleamic acid-based compound.
In some particularly preferred embodiments, the wood impregnating composition does not contain an inorganic filler.
In other particularly preferred embodiments, the wood impregnating composition does not include an acid other than maleamic acid, such as the acidic catalysts described above.
(preparation of the composition)
The compositions of the present invention may be prepared by various methods known in the art, for example, by mixing the ingredients using various mixing devices such as agitators, paint mixers, mills, and the like. The mixing may be performed in one step (e.g., by adding all of the ingredients to the mixing apparatus) or in stages (e.g., by adding the ingredients to the mixing apparatus in any combination, in any amount, and/or in any order, etc.).
< Wood prepreg and modified Wood >
The wood prepreg of the present invention is obtained by impregnating wood with the above-mentioned composition for wood impregnation of the present invention.
In the present invention, the term "impregnation" means that at least the inside of the wood is impregnated with the above-mentioned composition for wood impregnation of the present invention, and in some cases, the surface of the wood is also coated with the above-mentioned composition for wood impregnation of the present invention.
In the present invention, the type of wood used is not particularly limited, and is also selected according to actual needs. The wood may be derived from, but is not limited to: aspen, birch, southern us pine, red european pine, masson pine, cedar, oldham, and the like.
The modified wood of the present invention is a cured product of the above wood prepreg of the present invention.
In the present invention, the curing method of the wood prepreg is not particularly limited, and various methods generally used in the art may be used. In some particularly preferred embodiments, in order to better achieve the desired technical effects of the present invention, the modified wood of the present invention is obtained by the manufacturing method of the present invention described later.
< method for producing modified Wood >
The method for producing the modified wood of the present invention comprises: a) Impregnating wood with the above-described wood impregnating composition of the present invention to obtain a wood prepreg; b) Subjecting the wood prepreg to thermal curing.
The steps of the manufacturing method of the present invention will be described in detail below.
(step a)
In step a), wood is impregnated with the above-described wood impregnating composition of the present invention to obtain a wood prepreg. At the time of impregnation, at least a part of the wood may be contacted with the above-mentioned composition for wood impregnation of the present invention.
The impregnation conditions to be used are not particularly limited, and may be adjusted according to the kind and size of wood, the composition and the amount of the composition, and the like.
The impregnation pressure may be normal pressure or pressurized. Preferably, the impregnation is performed under pressure from the viewpoint of further improving the production efficiency. The pressurizing pressure may be appropriately adjusted according to the actual situation, and for example, the pressurizing pressure may be 0.2 to 0.9MPa, or 0.3 to 0.8MPa.
The impregnation temperature may be, for example, 10 to 50 ℃, and it is preferable to perform the impregnation at an ambient temperature from the viewpoint of reducing the production cost.
The immersion atmosphere may be an air atmosphere, an air atmosphere in which the partial pressure of oxygen is adjusted, or an inert gas atmosphere such as nitrogen or argon, or the like.
The impregnation time may be, for example, 0.5 to 10 hours, or 1 to 8 hours, etc.
(step b)
In step b), the wood prepreg obtained in step b) is subjected to heat curing. In the present invention, the term "heat curing" means that the temperature of the curing (at least one curing stage when the curing is divided into a plurality of stages) is higher than the room temperature (25 ℃).
The curing conditions for the heat curing are not particularly limited and may be appropriately adjusted according to actual needs.
The heating temperature for the thermal curing may be, for example, 55 to 220 ℃, and also, for example, 60 to 200 ℃.
The curing time for the heat curing may be, for example, 0.5 to 48 hours, and further, for example, 1 to 36 hours.
The atmosphere for thermal curing may be an air atmosphere, an air atmosphere in which the partial pressure of oxygen is adjusted, or an inert gas atmosphere such as nitrogen or argon, or the like.
The thermal curing may be carried out in one step or in the form of a plurality of stages.
In the case of performing the heat curing in the form of being divided into a plurality of stages, each stage may be performed continuously (i.e., without a time interval between adjacent two stages), or intermittently (i.e., with a certain time interval between adjacent two stages).
In the case of performing the heat curing in the form of being divided into a plurality of stages, the curing conditions may be the same for each stage (but it is not intended to cover the case where the curing conditions are the same and continuously performed for each stage), or may be different.
In some preferred embodiments, the heat curing is preferably performed in a form divided into a plurality of stages from the viewpoint of more facilitating the preparation of modified wood having good toughness and also excellent in dimensional stability in a wet environment.
In some more preferred embodiments, from the standpoint of more easily obtaining the modified wood desired in the present invention, the heat curing is preferably performed by a method comprising atmospheric pre-curing and press-curing, i.e., at least atmospheric pre-curing and press-curing are included in the multiple stages into which the heat curing process can be divided.
In the present invention, the conditions for the atmospheric pressure pre-curing are not particularly limited, and may be adjusted according to the kind and size of wood, the composition and the amount of the composition, and the like. Here, the term "normal pressure" means atmospheric pressure.
The atmospheric pre-cure temperature may be, for example, 20 to 100 ℃, e.g., ambient temperature such as room temperature (25 ℃). The atmospheric pre-curing temperature is preferably 65 to 90 deg.c from the viewpoint of further improving the production efficiency.
The time for the atmospheric pressure pre-curing may be, for example, 6 to 24 hours, and is preferably 8 to 18 hours from the viewpoint of further improving the production efficiency.
In the present invention, the conditions for press curing are not particularly limited, and may be adjusted according to the kind and size of wood, the composition and amount of the composition, the specific conditions for atmospheric pressure pre-curing, and the like.
The temperature of the press curing may be, for example, 100 to 250 ℃, preferably 110 to 200 ℃, more preferably 120 to 180 ℃ from the viewpoint of further improving the production efficiency.
The pressure of the press curing may be, for example, 0.5 to 5MPa, and is preferably 0.8 to 4MPa from the viewpoint of more facilitating the production of a modified wood having good toughness and also excellent in dimensional stability under a humid environment.
The dwell time of the press curing may be, for example, 5 minutes to 6 hours, preferably 10 minutes to 3 hours from the viewpoint of more facilitating the production of a modified wood having good toughness and also excellent dimensional stability in a wet environment.
According to practical needs, the thermal curing process may further include other atmospheric curing processes besides the atmospheric pre-curing and the pressure curing, and the conditions of these atmospheric curing may be the same as those of the atmospheric pre-curing, which will not be described herein. In addition, the press curing may be performed a plurality of times.
In some particularly preferred embodiments, the thermal curing is performed by a two-stage cure consisting of the above atmospheric pre-cure and the above pressure cure.
In addition, the compression degree of the wood in the pressing process is not particularly limited, and may be compressed or may be kept unchanged. The compression ratio of the wood before and after press curing is preferably 10 to 70%, more preferably 20 to 70%, from the viewpoint of more facilitating the production of a modified wood having good toughness and also excellent in dimensional stability under a wet environment. Here, the compression ratio= (dimension in the compression (pressing) direction of the wood before press curing-dimension in the compression (pressing) direction of the wood after press curing)/(dimension in the compression (pressing) direction of the wood before press curing) ×100%.
(other steps)
In addition to the above steps a) and b), the production method of the present invention optionally includes other steps, for example, a step of drying raw wood (for example, drying at a specific temperature), a step of purifying wood to remove air, impurities, etc. in the wood, a step of loosening the cellular structure of the wood, a treatment step provided between the respective stages when the formation into a plurality of stages is performed for heat curing, a step of cleaning the resulting modified wood, and the like.
(specific examples)
In some specific embodiments, the method of producing modified wood of the present invention is carried out by the following.
(1) An impregnating composition was prepared.
(2) And (3) carrying out vacuum treatment on the dried wood for 5-60 min, and loosening the cell structure of the wood to obtain the wood to be modified.
(3) The wood to be modified is impregnated with the impregnating composition and contacted, and the pressure is maintained for 2 to 5 hours under the condition of being pressurized to 0.2 to 0.9 MPa.
(4) After the impregnation is finished, taking out the wood prepreg, wiping to dry the residual liquid on the surface, pre-curing for 6-24 hours at the normal pressure at the temperature of 60-100 ℃, placing for 18-36 hours at the room temperature to further remove water, and further performing pressure curing under the conditions of the hot pressing temperature of 100-200 ℃ and the pressure of 1-3 MPa and the pressure maintaining for 20-120 minutes, and simultaneously controlling the specific compression rate to obtain the modified wood.
< example >
The present invention is described in detail below by way of examples, however, the scope of the present application is not limited to these examples. Hereinafter, "parts" means "parts by mass" and "%" means "% by mass" unless otherwise specified.
Example 1
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. To the furfuryl alcohol-maleamic acid solution was added 0.3 part of lysine to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 34.67%.
Example 2
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. To the furfuryl alcohol-maleamic acid solution was added 0.9 part of lysine to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 35.90%.
Example 3
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. 1.5 parts of lysine was added to the furfuryl alcohol-maleamic acid solution to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 39.59%.
Example 4
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. 1.5 parts of lysine was added to the furfuryl alcohol-maleamic acid solution to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 145 ℃, controlling the compression rate to 50%, and maintaining the pressure to 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 30.55%.
Example 5
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. 1.5 parts of lysine was added to the furfuryl alcohol-maleamic acid solution to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 160 ℃, controlling the compression rate to 50%, and maintaining the pressure to 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 36.70%.
Example 6
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. To the furfuryl alcohol-maleamic acid solution was added 0.3 part of polyethylenimine to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 39.84%.
Example 7
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. To the furfuryl alcohol-maleamic acid solution was added 0.9 part of polyethyleneimine to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 26.92%.
Example 8
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. To the furfuryl alcohol-maleamic acid solution was added 3 parts of polyethyleneimine to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 36.03%.
Example 9
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. To the furfuryl alcohol-maleamic acid solution was added 0.3 part of potassium persulfate to obtain an impregnating solution as a composition for impregnation. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 39.84%.
Example 10
According to the mass parts, 13.8 parts of furfuryl alcohol, 16.2 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. In the impregnating solution, the mass of maleamic acid is 1.17 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above furfuryl alcohol-maleic acid solution was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen gas, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 59.00%.
Comparative example 1
According to the parts by mass, 30 parts of furfuryl alcohol and 70 parts of water are uniformly mixed under the stirring condition to obtain a furfuryl alcohol solution with the mass concentration of 30% as a composition for impregnation.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above furfuryl alcohol solution was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen gas, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 110%.
Comparative example 2
According to the parts by mass, 30 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition, so as to obtain the maleamic acid solution with the mass concentration of 30%.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above furfuryl alcohol-maleic acid solution was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen gas, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 62.69%.
Comparative example 3
According to the mass parts, 17.6 parts of furfuryl alcohol, 12.4 parts of maleamic acid and 70 parts of water are uniformly mixed under the stirring condition to obtain the furfuryl alcohol-maleamic acid solution with the mass concentration of 30%. 1.5 parts of lysine was added to the furfuryl alcohol-maleamic acid solution to obtain an impregnating solution as a composition for impregnation. In the impregnation liquid, the mass of maleamic acid is 0.7 times of that of furfuryl alcohol.
The cedar wood blocks with the dimensions of 50mm×50mm×28mm were dried at 100 ℃, placed in a vacuum impregnation tank, and subjected to vacuum treatment for 30min to remove air in wood cells, and the wood cell structure was loosened for impregnation. Subsequently, 30 parts of the above impregnation liquid was sucked into a vacuum impregnation tank by negative pressure, pressurized to 0.6MPa by nitrogen, and maintained at the pressure for 3 hours. Taking out the wood block after the impregnation, wiping the solution on the surface of the wood block, wrapping the wood block by aluminum foil, pre-fixing the wood block in an oven at 80 ℃ for 12 hours, and further standing the wood block at room temperature for 24 hours to further remove water. Then placing the wood into a double-plate hot press for pressing, controlling the hot pressing temperature to 130 ℃, controlling the compression rate to be 50%, and maintaining the pressure to be 1-3 MPa for 60 minutes to obtain the modified wood.
The dimensional stability of the modified wood was tested according to standard GB/T1934.2-2009 with a thickness expansion of 68.47%.
Claims (10)
1. A composition for wood impregnation, characterized in that the composition comprises furfuryl alcohol and a maleamic acid compound, the mass of the maleamic acid compound is more than 0.9 times of the mass of the furfuryl alcohol,
the maleamic acid compound has a structure represented by the following formula (a):
wherein R is 1 And R is 2 Each independently represents hydrogen, an alkyl group having 1 to 22 carbon atoms, or an aryl group having 6 to 22 carbon atoms.
2. The composition for wood impregnation according to claim 1, wherein the composition comprises an amine group-containing compound, and the amine group-containing compound is contained in an amount of 0.5 to 15 mass% relative to the total amount of the furfuryl alcohol and the maleamic acid-based compound.
3. The composition for wood impregnation according to claim 1 or 2, wherein the maleamic acid-based compound is derived from the reaction of maleic anhydride and ammonia.
4. The composition for wood impregnation according to claim 1 or 2, wherein the mass of the maleamic acid-based compound is 10 times or less the mass of the furfuryl alcohol.
5. A wood prepreg, characterized in that it is obtained by impregnating wood with the composition for wood impregnation according to any one of claims 1 to 4.
6. A modified wood characterized in that it is a cured product of the wood prepreg according to claim 5.
7. A method of making a modified wood, the method comprising:
a) Impregnating wood with the composition for wood impregnation according to any of claims 1 to 4 to obtain a wood prepreg,
b) Subjecting the wood prepreg to thermal curing.
8. The method of manufacturing according to claim 7, wherein the heat curing is performed by a method including atmospheric pressure pre-curing and pressure curing.
9. The method according to claim 8, wherein the atmospheric pre-curing is performed at a temperature of 20 to 100 ℃ for a time of 6 to 24 hours.
10. The production method according to claim 8 or 9, wherein the press-curing temperature is 100 to 250 ℃, the press-curing pressure is 0.5 to 5MPa, the dwell time of the press-curing is 5 minutes to 6 hours, and the compression ratio of the wood before and after the press-curing is 10 to 70%.
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