CN102873724A - Nanometer hydroxide wood composite material and preparation method thereof - Google Patents
Nanometer hydroxide wood composite material and preparation method thereof Download PDFInfo
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- CN102873724A CN102873724A CN2012103878413A CN201210387841A CN102873724A CN 102873724 A CN102873724 A CN 102873724A CN 2012103878413 A CN2012103878413 A CN 2012103878413A CN 201210387841 A CN201210387841 A CN 201210387841A CN 102873724 A CN102873724 A CN 102873724A
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Abstract
The invention discloses a nanometer hydroxide wood composite material. The nanometer hydroxide wood composite material is a high-quality composite wood material which consists of fast-growing wood serving as a base body and inorganic nanometer hydroxide serving as a reinforcing body. The inorganic nanometer hydroxide is uniformly filled in nanometer cavities among microfibers of the fast-growing wood, and is nanometer aluminum hydroxide, nanometer aluminum oxyhydroxide, nanometer magnesium hydroxide or nanometer magaldrate. The nanometer wood composite material is prepared from the fast-growing wood serving as the base body for the first time by a (microwave) hydrothermal method, surface activity and dispersion conditions of nanometer particles in a matrix and influence of a boundary structure on the mechanical property and the flame retardant property of the composite material are researched, so that filled wood is strengthened and has multiple functions of flame retardance, smoke suppression and the like, and the novel material with the excellent mechanical property and the good flame retardant property is obtained.
Description
Technical field
The present invention relates to a kind of nanometer hydroxide Wood composite material and preparation method thereof.
Background technology
The china natural resources environment is faced with very stern challenge at present, and non-renewable resources are day by day exhausted, and environment can't bear the heavy load, and for guaranteeing sustainable economic development, should take full advantage of renewable, free of contamination biomass resource and biological material.Timber is the engineering material of present unique recyclable regenerative, utilize the bio-based materials of the friendly and reusable edible of abundant timber resources development environment, for energy-saving and emission-reduction, develop a circular economy, Resources for construction economizing type and friendly environment society be significant.Along with China came into effect wildwood protected project in 1998, the imbalance between supply and demand of high-quality timber sharply strengthens, and China's importation of timber amount surpasses 40 % of consumption figure for years, and timber safety is extremely urgent.And China has abundant fast-growing woods timber resources, and is accelerating the fast-growing woods Industrial Construction at present with the effective supply of increase timber, but fast-growing woods timber is because the loose poor mechanical property that causes of (1) material; (2) shortcoming of easy firing is severely limited the range of application of fast-growing woods timber, has affected the application prospect of fast-growing woods timber, has greatly limited the sustainable development of timber industry and forest products industry.Therefore fast-growing woods timber is carried out modification improves its mechanical property and fire resistance, make low material high performance, accelerate to realize low-carbon green economy for China, alleviate the resource and environment two "bottlenecks" pressure of China's sustainable economic development, have important theory value and application prospect.
Researcher has carried out large quantity research at present, timber is carried out the functionality improvements such as physics, chemistry and mechanics to realize the high performance of low-quality timber.For the shortcoming of wood dimensional stability and poor mechanical property, the study hotspot of Chinese scholars is with inorganic nano material SiO
2(B.Mahltig, C.Swaboda, A.Roessler, H.Bottcher. Functionalising wood by nanosol application. J. Mater. Chem. 2008. 18:3180-3192.), TiO
2(Miyafuji. H, Saka. S. Fire-resisting properties in several TiO
2Wood-inorganic composites and their top chemistry. Wood Science and Technology 1997. 31:449-455). and CaCO
3(Yuan Guangming, Liu Yuan, Hu Yunchu, Wu Zhiping. China fir/nano calcium carbonate composite material preparation and property is analyzed. Sino-South African Forestry University of Science and Technology's journal 2009. 29 (4): 83-87.) etc. be distributed to the composite that obtains a kind of strong mechanical performance in the wood substrates as strengthening body.Flameproof protection to timber mainly is to use fire proofing such as (NH
4)
3PO
4(C. S. Chuang, K.C. Tsai, M. K. Wang, C. Ou, C. H. Ko, I. L. Shiau. Effects of intumescent formulation for acrylic-based coating on flame-retardancy of painted red lauan (Parashorea spp.) thin plywood .Wood Sci Technol 2008. 18 (4): 593 – 607.), boric acid and borax carry out surperficial coating processing to timber, and use phosphate, carbonate and boric acid carry out two kinds of methods of impregnation process to timber.Yet the solution that these processing methods can only be local is some problems wherein, so fast-growing woods timber real practical also is badly in need of a kind of method that can two problems of a step solution fast-growing woods timber.
Summary of the invention
The object of the present invention is to provide the nanometer hydroxide Wood composite material of the strong and good flame resistance of a kind of mechanical property.
Nanometer hydroxide Wood composite material of the present invention, it is take fast-growing woods timber as matrix, take the composite wood material of inorganic nano hydroxide as a kind of high-quality of enhancing body formation, in the lar nanometric cavities of described inorganic nano hydroxide uniform filling between fast-growing woods timber microfibre, described inorganic nano hydroxide is nano-aluminum hydroxide, nano-hydroxy aluminium oxide, nano-sized magnesium hydroxide or nano-sized magnesium hydroxide aluminium etc.
The preparation method of nanometer hydroxide Wood composite material of the present invention comprises the steps:
(1) to contain concentration be 0.2-1.0 molL in preparation
-1Aluminium ion and/or the solution A of magnesium ion, and at room temperature it is evenly mixed with the solution B that contains ethylenediamine or urea, add ammoniacal liquor and regulate pH=5-6, get precursor solution; Or directly configuration concentration is 0.2-1.0 molL
-1AlO
2 -Solution is as precursor solution;
(2) with step (1) gained precursor solution vacuum impregnation in the fast-growing woods wood substrates, vacuum 0.1 MPa, the processing time is 2-24hr;
(3) with the timber behind the vacuum impregnation under 100-160 oC, constant temperature 3-20hr in hydrothermal reaction kettle, or microwave hydrothermal is processed 20-60 min in the teflon reactor;
(4) be cooled to room temperature, take out step (3) gained timber, deionized water washing, vacuum drying and get final product.
In the described step (1), the mol ratio of aluminium ion and/or magnesium ion and urea or ethylenediamine is preferably 1:1-3.
Fast-growing woods timber described in the step (2) preferably adopts ultrasonic wave or Microwave Pretreatment 0.5-3 hr.
Vacuum drying described in the step (4) is at 60-80 ° of C, and dry 24-48 hr is good under the vacuum 0.1-0.3 atm.
Layered hydroxide such as Al (OH)
3Its decomposition temperature lower (just beginning to decompose under 200 ° of C) is fit to be applied in (the unstable temperature on the timber calorifics is 260 ° of C) in the wooden material as fire proofing very much.Behind the layered hydroxide fine, surface energy increases, thereby the reactivity of particle surface is strengthened, be conducive to the dispersion of particle in wooden material, improve the interface binding power between fire proofing and wooden material, therefore not only can make fire retardant give full play to its fire retardation, and can improve the mechanical property of moulding processability and the goods of matrix material, and play the humidification of rigid particles.
Therefore adopt layered hydroxide as strengthening the standby timber inorganic nano composite material of system, and characterize the composition of composite in XRD, use thermal property and the mechanical property of TG-DSC and omnipotent mechanical test machine test wooden material, the research composite is on the rule that affects of timber heat endurance and mechanical property.
X-ray diffraction analysis (XRD): with obtaining timber/nanometer Al (OH)
3The composite test specimen places vacuum drying chamber vacuum drying 24 hr to over dry, the timber test specimen is positioned over uses cooled with liquid nitrogen in the mortar, is milled to Powderedly, crosses 180 mesh sieve samples and makes XRD analysis;
The composite thermal property is measured: powdered samples is filled in the platinum-rhodium crucible, weigh in the balance heavy after, put on the body of heater high accuracy sample mount, add porose crucible cover, then begin the experiment that heats up, the pyrolysis oven heating rate is 10 ° of C/min.Sample is risen to 800 ° of C from room temperature (20 ° of C), record differential scanning curve (DSC) curve.
The composite materials property test: adopt the WDW100 microcomputer to control omnipotent mechanical test machine, sample dimensions is 20 mm * 20 mm * 30 mm, sample is placed on the center of testing machine sphere movable bearing support, with the even speed loading, and loading velocity 2 mmmin
-1, sample is destroyed, till namely the pointer of testing machine is return significantly.
The present invention proposes take fast-growing woods timber first as matrix, prepare nanometer hydroxide Wood composite material by (microwave) hydro-thermal method, surface-active, dispersion situation and the interfacial structure of nano particle are on the impact of mechanical property and the fire resistance of composite in the research matrix, make timber after the filling have enhancing, fire-retardant and press down the multi-functional such as cigarette, thus the new material of the mechanical property that obtains to integrate excellent and good fire resistance.The present invention can not only improve the reasonable utilization of China's fast-growing woods timber resources and utilize level, and can promote China and build up early the new industrial system of biological material, petroleum replacing base synthetic material progressively is for china natural resources and ecological environment provide reliable safety guarantee.This not only expands the new technology and method of material subject in the application in timber and biological material field, for China's timber industry industrial upgrading and Forestry Sustainable fast development provide crucial technical guarantee, the 21 century of commanding elevation particularly seize biological material research and innovation and re-invent industry in to(for) China is significant.
Description of drawings
Fig. 1 is the optical microscopy map of nano-aluminum hydroxide Wood composite material;
Fig. 2 is fast-growing woods timber material, Al (OH)
3Composite wood material and Mg (OH)
2The DSC figure of composite wood material;
Fig. 3 a is fast-growing woods timber material, Al (OH)
3The radial crush resistance energy resolution chart of composite wood material;
Fig. 3 b is fast-growing woods timber material, Al (OH)
3The tangential compressive property resolution chart of composite wood material;
Fig. 3 c is fast-growing woods timber material, Mg (OH)
2The axial compression resistance performance test figure of composite wood material;
Fig. 4 is fast-growing woods timber material, Al (OH)
3Composite wood material and Mg (OH)
2The XRD figure of composite wood material.
The specific embodiment
Embodiment 1
Fast-growing woods willow 69 poplars that extensively plant in employing Northern Anhui area (
Populus deltoids cv. I-69/55).With log debarking, saw is made as the thick sheet material in the 5cm left and right sides, and after the ventilation placement was air-dry, sheet material was processed into 20 mm (radially) * 20 mm (tangential) * 30 mm (vertically), and volume is 12cm
3Quality is 3.0 g, uses ultrasonic wave with the active group of timber preliminary treatment 1 hr with increase timber.Prepare 100 mL, 1.0 molL
-1Al (NO
3) 9H
2O and 3.0 molL
-1CO (NH
2)
2Mixed solution, add concentrated ammonia liquor and regulate pH=6 and use vacuum decompression system (vacuum is 0.1 MPa) with the precursor liquid vacuum impregnation after 24 hours, approximately 6-8 mL precursor liquid is injected in the wood substrates.Pour the wooden unit behind the dipping into hydrothermal reaction kettle, 120 ° of C heat 12 hr, are cooled to take out after the washing of test specimen deionized water that vacuum is 0.1atm under 70 ° of C after the room temperature, and vacuum drying 48 hr namely get Al (OH)
3Mass fraction is 15% the fire-retardant Al of inorganic nano (OH) approximately
3Wood composite material.Gained Al (OH) in this example
3Timber microstructure analysis such as Fig. 1 of Wood composite material, thermal property is tested such as Fig. 2, mechanical experimental results such as Fig. 3 a and Fig. 3 b.
Fast-growing woods willow 69 poplars that extensively plant in employing Northern Anhui area (
Populus deltoids cv. I-69/55).With log debarking, saw is made as the thick sheet material in the 5 cm left and right sides, after the ventilation placement was air-dry, sheet material was processed into 20 mm (radially) * 20 mm (tangential) * 30 mm (vertically), used microwave with the active group of timber preliminary treatment 3hr with increase timber.Prepare 100 mL, 1.0 molL
-1NaAlO
2Solution uses the vacuum decompression system with the precursor liquid vacuum impregnation after 24 hours, and approximately to be injected into volume be 12 cm to 6-8 mL precursor liquid
3Quality is in the wood substrates of 3.0g.Pour the wooden unit behind the dipping into hydrothermal reaction kettle, 60 ° of C heat 12 hr, or with the direct 60-100 ° of C heating 6-12 hr in baking oven of wooden unit, be cooled to and take out after the washing of test specimen deionized water that vacuum is 0.1 atm under 70 ° of C after the room temperature, vacuum drying 48 hr namely get Al (OH)
3Mass fraction is 13% inorganic fire-retarded Al (OH) approximately
3Wood composite material.Gained Al (OH) in this example
3XRD test result such as Fig. 4 of Wood composite material.
Fast-growing woods willow 69 poplars that extensively plant in employing Northern Anhui area (
Populus deltoids cv. I-69/55).With log debarking, saw is made as the thick sheet material in the 5cm left and right sides, and after the ventilation placement was air-dry, sheet material was processed into 20 mm (radially) * 20 mm (tangential) * 30 mm (vertically), uses microwave with the active group of timber preliminary treatment 3hr with increase timber.Prepare 100 mL 0.2molL
-1Mg (NO
3)
29H
2O and 0.2 molL
-1CO (NH
2)
2Mixed solution, mix and add concentrated ammonia liquor and regulate pH=5 and use the vacuum decompression system that the precursor liquid vacuum impregnation was injected in the wood substrates in 24 hours.Pour the wooden unit behind the dipping into hydrothermal reaction kettle, 160 ° of C heat 10 hr, are cooled to take out after the washing of test specimen deionized water that vacuum is 0.1 atm under 70 ° of C after the room temperature, and vacuum drying 48 hr namely get inorganic fire-retarded Mg (OH)
2Wood composite material.Gained Mg (OH) in this example
2The thermal property of Wood composite material is tested such as Fig. 2, mechanical experimental results such as Fig. 3 c.
Embodiment 4
Fast-growing woods willow 69 poplars that extensively plant in employing Northern Anhui area (
Populus deltoids cv. I-69/55).With log debarking, saw is made as the thick sheet material in the 5 cm left and right sides, after the ventilation placement was air-dry, sheet material was processed into 20 mm (radially) * 20 mm (tangential) * 30 mm (vertically), used microwave with the active group of timber preliminary treatment 3 hr with increase timber.Prepare 100 mL, 0.5 molL
-1MgCl
29H
2O and 0.5 molL
-1The mixed solution of ethylenediamine mixes and adds concentrated ammonia liquor and regulates pH=5, uses the vacuum decompression system with precursor liquid vacuum impregnation 24 hours, is injected in the wood substrates.Pour in 140 ° of C teflon reactors the wooden unit behind the dipping into microwave hydrothermal and process 40-60 min, be cooled to and take out after the washing of test specimen deionized water that vacuum is 0.1 atm under 70 ° of C after the room temperature, vacuum drying 48 hr namely get inorganic fire-retarded Mg (OH)
2Wood composite material.
Fig. 1 is Al (OH)
3The fibrous structure chart of Wood composite material (cross section), Al (OH)
3Content is 15 wt. %.As seen from Figure 1: improved wood is keeping the timber microstructure of log, Al (OH)
3Be distributed in whole wood transverse section, be filled in conduit inner with wood-fibred on every side, and the wood cell around the conduit is darker with respect to other site color, this be since when filling because conduit diameter is larger, easier the entering by conduit of precursor solution causes the solids content of conduit peripheral cell more in its peripheral cell.
From Fig. 2, can see that the timber material finishes two continuous larger exothermic peaks in 245-500 ° of C scope, this heat release behavior is because hemicellulose, cellulose and the pyrolysis of lignin and the general performance of pentosan and organic extract etc. in the timber.First exothermic peak between 200-400 ° of C, corresponding to the pyrolysis of hemicellulose, cellulose and lignin in the timber with become the charcoal process; Second process between 400-500 ° of C, the oxidation Decomposition of the carbon residue that forms corresponding to last process.At Al (OH)
3Can see among the DSC figure of composite that two discontinuous exothermic peaks are arranged, first exothermic peak is between 220-300 ° of C, and this is because Al (OH)
3Thermal decomposition generates Al
2O
3Exothermic peak; Second exothermic peak is between 380-480 ° of C, and this is because Al (OH)
3The steam that thermal decomposition generates waters down and has diluted imflammable gas, helps to make burning to interrupt, and has played the effect that suppresses burning, simultaneously Al (OH)
3Thermal decomposition generates Al
2O
3Generate protective layer and be covered in sample surfaces, isolation burning things which may cause a fire disaster and oxygen make first exothermic peak of wooden material 380 ° of C that lag behind, and the thermal discharge of second exothermic peak greatly reduce.At Mg (OH)
2Also can see among the DSC figure of composite in 220-400 ° of C and two discontinuous exothermic peaks of 450-510 ° of C, this is because Mg (OH)
2Heat decomposition temperature is relatively high, and its thermal decomposition causes first exothermic peak thermal discharge of timber to reduce, and makes 60 ° of C of temperature delay of second exothermic peak.So fire proofing Al (OH)
3And Mg (OH)
2Oxide and steam that thermal decomposition produces work in gas phase and solid phase reaction district respectively, suppress the burning behavior of timber in gas phase and solid phase, play good flame retardant effect.
Fig. 3 a, 3b, 3c are the compressive property resolution chart of material and hydroxide Wood composite material of the present invention, are respectively (a) radially; (b) tangential; (c) axial.Such as Fig. 3 a, radially (a) proportional limit is reduced to 1.03 by 1.07, and pressure-proof elasticity modulus brings up to 3.87 by 2.21; Such as Fig. 3 b, tangential (b) proportional limit brings up to 1.71 by 1.27, and pressure-proof elasticity modulus brings up to 4.08 by 3.50; Such as Fig. 3 c, axially (c) proportional limit is reduced to 8.48 by 9.91, and pressure-proof elasticity modulus brings up to 17.60 by 11.53; The mechanical property of composite and material is compared, composite is except radial and axial proportional limit reduces a little, and elastic modelling quantity and tangential proportional limit all have more significantly raising, explanation can use hydroxide as the wooden material filler, can improve simultaneously the mechanical property of timber under the prerequisite that improves timber heat endurance and fire resistance.
Fig. 4 is timber material and embodiment 2 gained Al (OH)
3The XRD figure of composite wood material.As we can see from the figure: material and improved wood cellulosic characteristic peak all occurred at 16 ° and 22.5 °, but the cellulose diffraction maximum of improved wood is sharp-pointed than material, the degree of crystallinity that wood-cellulose after the modification is described becomes large, and this can improve the mechanical property of composite to a certain extent.From the sample powder timber inside Al (OH) that composite inner is taken out
3Content is 15 %, locates to see weak Al (OH) at 18.82,20.41 and 37.3 °
3Characteristic peak, this be since Wood composite material in Al (OH)
3Content less (15 %), Al (OH) during XRD characterizes
3Diffraction maximum is not obvious.And the diffraction maximum at the places such as 32.3 and 33.38 may be because generated in-situ Al (OH)
3Produce with organo-functional group bondings such as timber carboxyls.And the Al (OH) that reaction generates in the solution
3Be attached to the Wood composite material surface, in the XRD collection of illustrative plates that surface sampling is tested, locate to occur characteristic peak, respectively corresponding A l (OH) at 18.82,20.41 and 40.56 ° etc.
3(001), (020) and (201) etc., be monoclinic system.
Claims (5)
1. nanometer hydroxide Wood composite material, it is take fast-growing woods timber as matrix, take inorganic nano hydroxide as strengthening the composite wood material of a kind of high-quality that body was consisted of, in the lar nanometric cavities of described inorganic nano hydroxide uniform filling between fast-growing woods timber microfibre, described inorganic nano hydroxide is nano-aluminum hydroxide, nano-hydroxy aluminium oxide, nano-sized magnesium hydroxide or nano-sized magnesium hydroxide aluminium.
2. the preparation method of the described nanometer hydroxide of claim 1 Wood composite material is characterized in that: comprise the steps:
(1) compound concentration is 0.2-1.0 molL
-1Aluminium ion and/or the solution A of magnesium ion, and at room temperature it is evenly mixed with the solution B that contains ethylenediamine or urea, add ammoniacal liquor and regulate pH=5-6, get precursor solution; Or directly configuration concentration is 0.2-1.0 molL
-1AlO
2 -Solution is as precursor solution;
(2) with step (1) gained precursor solution vacuum impregnation in the fast-growing woods wood substrates, vacuum 0.1 MPa, the processing time is 2-24hr;
(3) with the timber behind the vacuum impregnation under 100-160 oC, constant temperature 3-20hr in hydrothermal reaction kettle, or microwave hydrothermal is processed 20-60 min in the teflon reactor;
(4) be cooled to room temperature, take out step (3) gained timber, deionized water washing, vacuum drying and get final product.
3. the preparation method of nanometer hydroxide Wood composite material as claimed in claim 2, it is characterized in that: in the described step (1), the mol ratio of aluminium ion and/or magnesium ion and urea or ethylenediamine is 1:1-3.
4. the preparation method of nanometer hydroxide Wood composite material as claimed in claim 2, it is characterized in that: fast-growing woods timber described in the step (2) adopts ultrasonic wave or Microwave Pretreatment 0.5-3hr.
5. the preparation method of nanometer hydroxide Wood composite material as claimed in claim 2, it is characterized in that: vacuum drying described in the step (4) is at 60-80 ° of C, dry 24-48 hr under the vacuum 0.1-0.3 atm.
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| 姚晓林，刘盛全: "纳米氢氧化物木材复合材料的制备及其性能的研究", 《第四届全国生物质材料科学与技术学术研讨会论文集》 * |
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