CN101954662A - Method for modifying wood by filling grafted cell walls with organic monomers and polymerization-filling cell cavities - Google Patents
Method for modifying wood by filling grafted cell walls with organic monomers and polymerization-filling cell cavities Download PDFInfo
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- CN101954662A CN101954662A CN 201010281955 CN201010281955A CN101954662A CN 101954662 A CN101954662 A CN 101954662A CN 201010281955 CN201010281955 CN 201010281955 CN 201010281955 A CN201010281955 A CN 201010281955A CN 101954662 A CN101954662 A CN 101954662A
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Abstract
The invention discloses a method for modifying wood by filling grafted cell walls with organic monomers and polymerization-filling cell cavities, which relates to a wood modification method. The invention solves the problem of difficulty in simultaneously enhancing mechanical properties and durability of wood in the existing wood modification method. The method comprises the following steps: 1, preparing organic acid anhydride solution; 2, soaking the wood with the organic acid anhydride solution; 3, filling grafted wood cell walls with organic acid anhydride by heating; 4, preparing the organic polymerizable monomer solution; 5, soaking the wood with the organic polymerizable monomer solution; and 6, carrying out polymerization-filling on the wood cell cavities with the monomers by heating. Since organic function micromolecules firstly enter the wood cell walls, the method realizes filling and bonding and eliminates a great deal of hydroxyl groups in the cell walls, thereby enhancing wood durability; and the wood cell cavities are soaked by the organic polymerizable monomers to initiate the polymerization and realize the filling of the cell cavities, so that the wood has higher mechanical properties and durability.
Description
Technical field
The present invention relates to a kind of method of modifying of timber.
Background technology
Timber is the living beings polymer composite of the natural reproducible that a kind of mankind depend on for existence since ancient times.Its unique chemical composition comprises the cellulose and amorphous hemicellulose that wraps up and the lignin etc. that have great amount of hydroxy group on every side, has constituted wood cell wall matrix, and then has formed the natural cellular shape structure with high ratio of strength to weight.These characteristics make it be better than other materials in a lot of fields.But according to different purposes, timber, especially fast growing wood such as poplar, China fir etc. also present some unfavorable characteristics.For example, quick growing species of trees mechanical property is relatively poor, is difficult to use as structure material; Most durabilities of wood are low, and wood substrates is easy to rotten degraded, size and changes defectives such as the contraction that is easy to expand with ambient humidity, make it to be difficult to as the effective material that is utilized for a long time etc.And cause timber to have the reason of low durability, say to a certain extent, owing to topmost functional groups in the wood components---hydroxyl is to the sorption of moisture.Based on this understanding, people have attempted many processing methods, permeate the quantity with free hydroxyl in the minimizing wood cell wall such as processing cell membrane, timber densification processing, high temperature carbonization heat treatment as little molecular chemistry reagent, and therefore obtained certain effect of improving with organic or inorganic; But these methods often can only be improved the durability of timber, but are difficult to improve effectively the especially mechanical strength of fast growing wood of timber.
In the recent period, researchers have explored and have utilized vinyl unsaturated monomer in-situ polymerization in timber to form high polymer, make wood plastic composite, to give the timber excellent mechanical property, and delay simultaneously or stop moisture and microorganism, and then improve the method for durability such as wood durability, dimensional stability to wood cell wall infiltration and invasion.But regrettably, because most of unsaturated monomer polarity are lower, and be the simple function group monomer, be difficult to enter wood cell wall then with it hydroxyl realize chemical bonding, and the high polymer that polymerization forms in the wood cell chamber is difficult realizes the grafting binding with wood cell wall, cause the chemically composited weak effect of two-phase, great amount of hydroxy group in the timber is still isolated to be existed, so when the kind method effectively improves the timber mechanics performance, but often improve not ideal enough to endurance qualities such as wood preservation, dimensional stabilitys.
Summary of the invention
The objective of the invention is to be difficult to improve simultaneously the mechanical property of timber and the problem of durability, a kind of method of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber is provided in order to solve existing method for modifying wood.
The present invention utilizes the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows: one, the configuration of organic acid anhydride solution: organic acid anhydride is dissolved in acetone or the oxolane, drip 3～5 pyrimidines then, make the organic acid anhydride mass fraction and be 10～30% organic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the organic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～130 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: organic polymerisable monomer is mixed with initator, make organic polymerisable monomer solution, the mass concentration of initator is 0.5%～1% in organic polymerisable monomer solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through organic acid anhydride that step 3 is obtained immerses in organic polymerisable monomer solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through organic acid anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃～110 ℃ through the timber of handling through organic acid anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber; Organic acid anhydride described in the step 1 is the mixture of two or three in maleic anhydride, succinyl oxide and the phthalic anhydride; Organic polymerisable monomer described in the step 4 is a methyl methacrylate, EMA, n-BMA, isobutyl methacrylate, the just own ester of methacrylic acid, benzyl methacrylate, decyl-octyl methacrylate, lauryl methacrylate, the methacrylic acid hard acid ester, methacrylic acid-α-hydroxyl ethyl ester, methacrylic acid-α-hydroxypropyl acrylate, dimethylaminoethyl acrylate methyl ammonia ethyl ester, methacrylic acid diethylamino ethyl ester, methacrylic acid-3-chloro-2-hydroxypropyl acrylate, methacrylic acid-2,3-dibromo propyl ester, cyclohexyl methacrylate, ethylene glycol dimethacrylate, the diethylene glycol dimethylacrylate, triethylene glycol dimethylacrylate, TEG dimethylacrylate, polyethylene glycol dimethacrylate, one propane diols dimethylacrylate, DPG dimethylacrylate, tripropylene glycol dimethylacrylate, 1, the 3-butanediol dimethylacrylate, 1, the 4-butanediol dimethylacrylate, bisphenol a dimethacrylate, 2, two [the methacryl propoxyl group phenol] propane of 2-, the third three methyl alcohol trimethyl acrylic esters, GMA, styrene, acrylonitrile, methacrylonitrile, vinylacetate, to divinylbenzene, to chlorostyrene, Methacrylamide, N hydroxymethyl acrylamide, isobutylvinyl ether, DEF, diethyl maleate, the methyl-prop ketenes, allyl chloride, vinylpyridine, naphthalene ethene, poly-phthalic acid-1, a kind of or wherein several mixture in 2-propylene diester and poly-phthalic acid-oxygen di-ethyl ester; Initator described in the step 4 is azodiisobutyronitrile or benzoyl peroxide.
The present invention utilizes the little molecule of organic functions to be introduced into wood cell wall, realizes inflation and bonding, eliminates the great amount of hydroxy group in the cell membrane, and then improves the durability of timber; Then by organic polymerisable monomer immersing wood lumen, and initiated polymerization realizes that lumen fills, and then gives higher mechanical property of timber and durability, thereby realizes the improvement to the timber combination property.
The little molecule of organic acid anhydride has higher activity from the molecular structure, under the effect of little amount of catalyst very easily with wood cell wall on activity hydroxy generation nucleophilic substitution; And the little molecule of cyclic anhydride has higher polarity parameter, infiltrates through the wood cell pars intramuralis easily down the auxiliary of polar solvent, so the class organic monomer can be realized inflation and bonding to wood cell wall, and then effectively improves the durability of timber.In addition, when the hydroxyl generation single substitution reaction on little molecule of organic acid anhydrides and the wood cell wall, can attach the generation carboxylic group, give timber certain acidity, can play certain acidic catalyst effect; Introduce organic polymerisable monomer when second step, when especially having the polymerisable monomer of functional group such as epoxy radicals, this carboxyl can participate in the reaction of organic polymerisable monomer, be beneficial to the polymer of monomer polymerization formation and the grafting of wood substrates, thereby improve the two-phase interface compatibility of timber and polymer, can give timber potential more excellent durability giving timber more in the strong mechanical performance.
By the low-quality fast growing wood of the inventive method modification, can be widely used in the ornament materials of construction material, furniture, woodcarving material, sports equipment, weaving facility, musical instrument, house decoraton plate, floor, ceiling, gun stock and various transport facilitys etc.
Description of drawings
Fig. 1 is the stereoscan photograph that utilizes the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber in the specific embodiment 13; Fig. 2 is the stereoscan photograph without the timber of any processing; Fig. 3 adopts maleic anhydride to handle the stereoscan photograph of back timber in the specific embodiment 19; Fig. 4 is the stereoscan photograph that utilizes the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber in the specific embodiment 20; Fig. 5 is the N distribution diagram of element corresponding with Fig. 4.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: organic acid anhydride is dissolved in acetone or the oxolane, drip 3～5 pyrimidines then, make the organic acid anhydride mass fraction and be 10～30% organic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the organic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～130 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: organic polymerisable monomer is mixed with initator, make organic polymerisable monomer solution, the mass concentration of initator is 0.5%～1% in organic polymerisable monomer solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through organic acid anhydride that step 3 is obtained immerses in organic polymerisable monomer solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through organic acid anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃～110 ℃ through the timber of handling through organic acid anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
The seeds of used timber source is any seeds, the particularly quick growing species of trees (birch, poplar and China fir) in the present embodiment.
Respectively maleic anhydride, succinyl oxide or phthalic anhydride are dissolved in acetone or the oxolane as the inflation agent in the present embodiment step 1, utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber then, the wood performance such as the table 1 of process modification:
Table 1
By table 1 data as can be known, when the different organic acids acid anhydride is done the inflation agent, all can realize the inflation to wood cell wall, inflation effect order from high in the end is followed successively by: maleic anhydride＞succinic anhydride＞phthalic anhydride.
The specific embodiment two: what present embodiment and the specific embodiment one were different is that the organic acid anhydride described in the step 1 is the mixture of two or three in maleic anhydride, succinyl oxide and the phthalic anhydride.Other is identical with the specific embodiment one.
When organic acid anhydride is mixture in the present embodiment between each composition for arbitrarily than.
The specific embodiment three: what present embodiment was different with one of the specific embodiment one or two is that the organic polymerisable monomer described in the step 4 is a methyl methacrylate, EMA, n-BMA, isobutyl methacrylate, the just own ester of methacrylic acid, benzyl methacrylate, decyl-octyl methacrylate, lauryl methacrylate, the methacrylic acid hard acid ester, methacrylic acid-α-hydroxyl ethyl ester, methacrylic acid-α-hydroxypropyl acrylate, dimethylaminoethyl acrylate methyl ammonia ethyl ester, methacrylic acid diethylamino ethyl ester, methacrylic acid-3-chloro-2-hydroxypropyl acrylate, methacrylic acid-2,3-dibromo propyl ester, cyclohexyl methacrylate, ethylene glycol dimethacrylate, the diethylene glycol dimethylacrylate, triethylene glycol dimethylacrylate, TEG dimethylacrylate, polyethylene glycol dimethacrylate, one propane diols dimethylacrylate, DPG dimethylacrylate, tripropylene glycol dimethylacrylate, 1, the 3-butanediol dimethylacrylate, 1, the 4-butanediol dimethylacrylate, bisphenol a dimethacrylate, 2, two [the methacryl propoxyl group phenol] propane of 2-, the third three methyl alcohol trimethyl acrylic esters, GMA, styrene, acrylonitrile, methacrylonitrile, vinylacetate, to divinylbenzene, to chlorostyrene, Methacrylamide, N hydroxymethyl acrylamide, isobutylvinyl ether, DEF, diethyl maleate, the methyl-prop ketenes, allyl chloride, vinylpyridine, naphthalene ethene, poly-phthalic acid-1, a kind of or wherein several mixture in 2-propylene diester and poly-phthalic acid-oxygen di-ethyl ester.Other is identical with one of the specific embodiment one or two.
When the organic polymerisable monomer described in the present embodiment is mixture between each composition for arbitrarily than.
The specific embodiment four: what present embodiment was different with one of specific embodiment one to three is that the initator described in the step 4 is azodiisobutyronitrile or benzoyl peroxide.Other is identical with one of specific embodiment one to three.
The specific embodiment five: present embodiment is different with one of specific embodiment one to four is that the mass fraction of organic acid anhydride in the step 1 organic acid anhydride solution is 15～25%.Other is identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different with one of specific embodiment one to five is that the mass fraction of organic acid anhydride in the step 1 organic acid anhydride solution is 20%.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different with one of specific embodiment one to six is will coat timber with aluminium-foil paper in the step 3 to heat under 120 ℃ of conditions.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: present embodiment is different with one of specific embodiment one to seven is that the mass concentration of initator in the organic polymerisable monomer solution of step 4 is 0.8%.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different with one of specific embodiment one to eight is will coat the timber of process organic acid anhydride processing 90 ℃～100 ℃ heating with aluminium-foil paper through what step 5 was handled in the step 6.Other is identical with one of specific embodiment one to eight.
The specific embodiment ten: what present embodiment was different with one of specific embodiment one to nine is will coat the timber of process organic acid anhydride processing 95 ℃ of heating with aluminium-foil paper through what step 5 was handled in the step 6.Other is identical with one of specific embodiment one to nine.
The specific embodiment 11: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: maleic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the maleic anhydride mass fraction and be 25～30% maleic anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the maleic anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～120 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: styrene (St) is mixed with azodiisobutyronitrile (AIBN), make styrene (St) solution, the mass concentration of azodiisobutyronitrile is 0.5%～1% in styrene (St) solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through maleic anhydride that step 3 is obtained immerses in styrene (St) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through maleic anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through maleic anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
The specific embodiment 12: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: maleic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the maleic anhydride mass fraction and be 25～30% maleic anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the maleic anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～120 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: (MMA) mixes with azodiisobutyronitrile with methyl methacrylate, make methyl methacrylate (MMA) solution, the mass concentration of azodiisobutyronitrile is 0.5%～1% in methyl methacrylate (MMA) solution; Five, organic polymerisable monomer solution impregnating timber: the timber that the process that step 3 is obtained has maleic anhydride to handle immerses in methyl methacrylate (MMA) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through maleic anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through maleic anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
The specific embodiment 13: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: maleic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the maleic anhydride mass fraction and be 25～30% maleic anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the maleic anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～120 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: GMA (GMA) is mixed with azodiisobutyronitrile (AIBN), make GMA (GMA) solution, the mass concentration of azodiisobutyronitrile (AIBN) is 0.5%～1% in GMA (GMA) solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through maleic anhydride that step 3 is obtained immerses in GMA (GMA) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through maleic anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through maleic anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
Show clearly that by Fig. 1 through maleic anhydride inflation cell membrane, then behind GMA (GMA) the tytosis chamber, the original loose structure of timber is aggregated the thing complete filling, has reached the imagination of expection.
The specific embodiment 14: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: maleic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the maleic anhydride mass fraction and be 25～30% maleic anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the maleic anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～130 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: organic polymerisable monomer is mixed with azodiisobutyronitrile (AIBN), make organic polymerisable monomer solution, the mass concentration of azodiisobutyronitrile (AIBN) is 0.5%～1% in organic polymerisable monomer solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through maleic anhydride that step 3 is obtained immerses in organic polymerisable monomer solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through maleic anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through maleic anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then, under 110 ℃ of conditions, further heat 8～10h again, and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber; Organic polymerisable monomer is made up of according to 0.1: 1: 5 mol ratio maleic anhydride (MAn), GMA (GMA) and styrene (St) in the step 4.
The specific embodiment 15: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: succinyl oxide is dissolved in the acetone, drip 3～5 pyrimidines then, make the succinyl oxide mass fraction and be 25～30% succinic anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the succinic anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 115 ℃～120 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: styrene (St) is mixed with azodiisobutyronitrile (AIBN), make styrene (St) solution, the mass concentration of azodiisobutyronitrile (AIBN) is 0.5%～1% in styrene (St) solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through succinyl oxide that step 3 is obtained immerses in styrene (St) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through succinyl oxide and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through succinyl oxide with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
The specific embodiment 16: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: succinyl oxide is dissolved in the acetone, drip 3～5 pyrimidines then, make the succinyl oxide mass fraction and be 15～20% succinic anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the succinic anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 115 ℃～120 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: GMA (GMA) is mixed with azodiisobutyronitrile (AIBN), make GMA (GMA) solution, the mass concentration of azodiisobutyronitrile (AIBN) is 0.5%～1% in GMA (GMA) solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through succinyl oxide that step 3 is obtained immerses in GMA (GMA) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through succinyl oxide and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through succinyl oxide with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then, under 110 ℃ of conditions, further heat 8～10h again, and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
The specific embodiment 17: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: phthalic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the phthalic anhydride mass fraction and be 10～15% phthalic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the phthalic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 120 ℃～130 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: styrene (St) is mixed with azodiisobutyronitrile (AIBN), make styrene (St) solution, the mass concentration of azodiisobutyronitrile (AIBN) is 0.5%～1% in styrene (St) solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through phthalic anhydride that step 3 is obtained immerses in styrene (St) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through phthalic anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through phthalic anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
The specific embodiment 18: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: phthalic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the phthalic anhydride mass fraction and be 10～15% phthalic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the phthalic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 120 ℃～130 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: GMA (GMA) is mixed with azodiisobutyronitrile (AIBN), make GMA (GMA) solution, the mass concentration of azodiisobutyronitrile (AIBN) is 0.5%～1% in GMA (GMA) solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through phthalic anhydride that step 3 is obtained immerses in GMA (GMA) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through phthalic anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through phthalic anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then, under 110 ℃ of conditions, further heat 8～10h again, and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
The specific embodiment 19: adopt the method for maleic anhydride processing timber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: maleic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the organic acid anhydride mass fraction and be 10～15% organic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the organic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper.
Can clearly observe the natural cellular shape loose structure of timber by Fig. 2; As shown in Figure 3, after maleic anhydride was handled, timber had still kept loose structure, does not find obvious filler in the lumen, can judge tentatively that maleic anhydride may infiltrate through (as shown by arrows) in the cell membrane.
It is as follows to adopt succinyl oxide to handle the method for timber in the present embodiment: one, the configuration of organic acid anhydride solution: succinyl oxide is dissolved in the acetone, drips 3～5 pyrimidines then, make the organic acid anhydride mass fraction and be 10～15% organic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the organic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper.
Adopt the method for phthalic anhydride processing timber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: phthalic anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the organic acid anhydride mass fraction and be 10～15% organic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the organic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper.
Through the preservation of timber against decay performance and dimensional stability such as the table 2 that the specific embodiment 11 is handled to present embodiment, the mechanical property such as the table 3 of the timber that the process specific embodiment 11 to present embodiment is handled:
Table 2
Table 3
Show by table 2 and table 3, after cell membrane inflation and lumen filling two step modifications, handle material and have more excellent durability and mechanical property than unseasoned timber far away.
The specific embodiment 20: utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows in the present embodiment: one, the configuration of organic acid anhydride solution: organic acid anhydride is dissolved in the acetone, drip 3～5 pyrimidines then, make the organic acid anhydride mass fraction and be 25～30% organic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the organic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～120 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: styrene (St) is mixed with azodiisobutyronitrile (AIBN), make styrene (St) solution, the mass concentration of azodiisobutyronitrile is 0.5%～1% in styrene (St) solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through maleic anhydride that step 3 is obtained immerses in styrene (St) solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through organic acid anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃ through the timber of handling through organic acid anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber; Organic acid anhydride described in the step 1 is made up of according to 1: 1 mol ratio DAAM (reagent of marking) and maleic anhydride.
Fig. 4 and Fig. 5 fit like a glove, indirect proof maleic anhydride infiltrate through in the wood cell wall.
Claims (10)
1. utilize the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber, it is characterized in that utilizing the method for the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber as follows: one, the configuration of organic acid anhydride solution: organic acid anhydride is dissolved in acetone or the oxolane, drip 3～5 pyrimidines then, make the organic acid anhydride mass fraction and be 10～30% organic acid anhydride solution; Two, organic acid anhydride solution impregnating: timber is immersed in the organic acid anhydride solution to timber, under the condition of vacuum, vacuumize 20min for-0.08MPa, the 20min that pressurizes under the pressure of 0.8MPa again recovers normal pressure, coats timber and displays 12～24h at normal temperatures and pressures with aluminium-foil paper; Three, heating realizes organic acid anhydride inflation grafting wood cell wall: will coat timber with aluminium-foil paper and heat 2～4h under 110 ℃～130 ℃ conditions, and remove aluminium-foil paper then, and be evacuated to constant weight at normal temperatures, and obtain the timber of handling through organic acid anhydride; Four, the configuration of organic polymerisable monomer solution: organic polymerisable monomer is mixed with initator, make organic polymerisable monomer solution, the mass concentration of initator is 0.5%～1% in organic polymerisable monomer solution; Five, organic polymerisable monomer solution impregnating timber: the timber of handling through organic acid anhydride that step 3 is obtained immerses in organic polymerisable monomer solution, under the condition of vacuum, vacuumize 12～24h for-0.08MPa, 12～24h again pressurizes under the pressure of 0.8MPa, recover normal pressure, coat the timber of handling through organic acid anhydride and display 12～24h at normal temperatures and pressures with aluminium-foil paper; Six, heating realizes the polymerization filling of monomer to the wood cell chamber: will heat 8～10h at 80 ℃～110 ℃ through the timber of handling through organic acid anhydride with the aluminium-foil paper coating that step 5 is handled, remove aluminium-foil paper then and be evacuated to constant weight at normal temperatures, promptly finish and utilize the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber.
2. according to the described method of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber of claim 1, it is characterized in that the organic acid anhydride described in the step 1 is the mixture of two or three in maleic anhydride, succinyl oxide and the phthalic anhydride.
3. according to claim 1 or the 2 described methods of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber, it is characterized in that the organic polymerisable monomer described in the step 4 is a methyl methacrylate, EMA, n-BMA, isobutyl methacrylate, the just own ester of methacrylic acid, benzyl methacrylate, decyl-octyl methacrylate, lauryl methacrylate, the methacrylic acid hard acid ester, methacrylic acid-α-hydroxyl ethyl ester, methacrylic acid-α-hydroxypropyl acrylate, dimethylaminoethyl acrylate methyl ammonia ethyl ester, methacrylic acid diethylamino ethyl ester, methacrylic acid-3-chloro-2-hydroxypropyl acrylate, methacrylic acid-2,3-dibromo propyl ester, cyclohexyl methacrylate, ethylene glycol dimethacrylate, the diethylene glycol dimethylacrylate, the triethylene glycol dimethylacrylate, the TEG dimethylacrylate, polyethylene glycol dimethacrylate, a propane diols dimethylacrylate, the DPG dimethylacrylate, the tripropylene glycol dimethylacrylate, 1, the 3-butanediol dimethylacrylate, 1, the 4-butanediol dimethylacrylate, bisphenol a dimethacrylate, 2, two [the methacryl propoxyl group phenol] propane of 2-, the third three methyl alcohol trimethyl acrylic esters, GMA, styrene, acrylonitrile, methacrylonitrile, vinylacetate is to divinylbenzene, to chlorostyrene, Methacrylamide, N hydroxymethyl acrylamide, isobutylvinyl ether, DEF, diethyl maleate, methyl-prop ketenes, allyl chloride, vinylpyridine, naphthalene ethene, poly-phthalic acid-1, a kind of or wherein several mixture in 2-propylene diester and poly-phthalic acid-oxygen di-ethyl ester.
4. according to the described method of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber of claim 3, it is characterized in that the initator described in the step 4 is azodiisobutyronitrile or benzoyl peroxide.
5. according to claim 1, the 2 or 4 described methods of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber, the mass fraction that it is characterized in that organic acid anhydride in the step 1 organic acid anhydride solution is 15～25%.
6. according to claim 1, the 2 or 4 described methods of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber, the mass fraction that it is characterized in that organic acid anhydride in the step 1 organic acid anhydride solution is 20%.
7. according to the described method of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber of claim 6, it is characterized in that will coat timber with aluminium-foil paper in the step 3 heats under 120 ℃ of conditions.
8. according to claim 1,2, the 4 or 7 described methods of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber, it is characterized in that the mass concentration of initator in the organic polymerisable monomer solution of step 4 is 0.8%.
9. the described according to Claim 8 method of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber is characterized in that will coating the timber of process organic acid anhydride processing 90 ℃～100 ℃ heating with aluminium-foil paper through what step 5 was handled in the step 6.
10. the described according to Claim 8 method of utilizing the combined modified timber of organic monomer inflation grafting cell membrane and polymerization tytosis chamber is characterized in that will coating the timber of process organic acid anhydride processing 95 ℃ of heating with aluminium-foil paper through what step 5 was handled in the step 6.
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