CN101745967B - Method for preparing poplar fiber /Al2O3 nano composite material - Google Patents

Method for preparing poplar fiber /Al2O3 nano composite material Download PDF

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CN101745967B
CN101745967B CN2009102338740A CN200910233874A CN101745967B CN 101745967 B CN101745967 B CN 101745967B CN 2009102338740 A CN2009102338740 A CN 2009102338740A CN 200910233874 A CN200910233874 A CN 200910233874A CN 101745967 B CN101745967 B CN 101745967B
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silicon
fiber
composite material
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nano composite
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CN101745967A (en
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徐莉
周晓燕
姜维娜
杨星
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Nanjing Forestry University
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Nanjing Forestry University
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Abstract

The invention relates to a method for preparing a poplar fiber/Al2O3 nano composite material. The poplar fiber/Al2O3 nano composite material is prepared by a sol-gel technique, and the heat release rate, the total heat release amount, the ignition time and the like are researched by utilizing a cone calorimeter. Experimental results show that after the nano composite material is modified by inorganic nano Al2O3, heat release peak values generated at 45s and 175s are obviously weakened, the heat release speed is obviously reduced, the average heat release speed is reduced by 38 percent, the heat release speed peak value drops by 25 percent, the total heat release is reduced by 38 percent, and the ignition time is prolonged by one time. The fire resistance of the poplar fiber/Al2O3 nano composite material is obviously improved.

Description

Aspen fibers by using silicon/Al 2O 3Nano composite material preparation method
Technical field
That the present invention relates to is a kind of aspen fibers by using silicon/Al 2O 3Nano composite material preparation method belongs to aspen fibers by using silicon/Al 2O 3The nano composite material technical field.
Background technology
String is a kind of hydrophilic material, and the composite wooden material of being made by string without water-proofing treatment has very big hygroscopicity and water imbibition, the poor dimensional stability of goods.Promptly deform, reduce intensity after the sheet material suction, increase conduct heat, electric conductivity, apt to rot, influence the scope of application and the service life of material.In addition, timber is a kind of combustible material, also has this critical defect with its composite wooden material of making, has also therefore limited the scope of application of composite wooden material.So far, the numerous scientific research personnel of timber industry circle to composite wooden material modification done number of research projects, in the hope of improving dimensional stability, anti-corrosive properties and the anti-flammability of material, increase the added value of composite wooden material.
At present, the waterproof of composite wooden material, main method anticorrosion and flame treatment are realized by applying waterproofing agent, anticorrisive agent and fire retardant.This method characteristics are that macroscopic view is mixed, filled or coating, exist the defective of easy loss, and this is the main problem that influences its result of use.
With the sol-gel technology preparing nano composite material history of existing more than ten years, existing both at home and abroad a lot of about utilizing sol-gel process to prepare the research of timber/inorganic nano composite material.The S.Saka of Japan, K.Ogiso, timber/inorganic nano composite material that H.Miyafuji and domestic employing sol-gel processes such as Wang Xicheng, Li Jian prepare has good flame retardancy.But the modification of wood-fibred sol-gel yet there are no report.
Summary of the invention
That the present invention proposes is a kind of aspen fibers by using silicon/Al 2O 3Nano composite material preparation method, and utilize taper calorimeter method (CONE) to aspen fibers by using silicon/inorganic nano Al 2O 3The fire resistance of composite has been carried out analytical test.
Technical solution of the present invention: aspen fibers by using silicon/Al 2O 3Nano composite material preparation method comprises following processing step:
One, aspen fibers by using silicon preparation: after the peeling of raw material poplar, chipping, wood chip is put into autoclaving pot boiling 40min (keep-up pressure and be 1.5MPa)).Chip raw material behind the poach is put into the ZSP-300 high concentration plate mill and is processed into fiber.After treating air dry, carry out secondary and pulverize.Placing 101-A-2B type electric drying oven with forced convection to be dried to moisture content then is 8% with standby.
Two, Al 2O 3Colloidal sol preparation: 1mol/L ammoniacal liquor is added drop-wise to the 0.96mol/L aluminum nitrate) in the solution, make final solution system pH＞9.20, filter with Bush's funnel again and obtain precipitating, and spend deionised water repeatedly, until the pH of system value near 7.0.Maintain the temperature at 50 ℃ at last, gradation adding concentration is the 0.94mol/L salpeter solution in precipitation, is stirred to system pH=3.5-4.1, can obtain transparent Al 2O 3Colloidal sol.
Three, urea-formaldehyde resin adhesive preparation: solid content 52%, viscosity 20mPas, pH value 7.0-7.5; The raw material that uses in the urea-formaldehyde resin adhesive preparation process: 37% formaldehyde, 700 grams; 98% urea, 300 grams; 99% melamine, 18 grams; 10% NaOH is an amount of; 20% ammonium chloride is an amount of.
Concrete preparation technology comprises:
(1) formaldehyde metering back is added reaction pot, transfer pH to 7.5-8.5 with sodium hydroxide solution.Add urea (264g) and all melamine for the first time;
(2) in 40-50min, be warmed up to 90 ± 1 ℃, insulation 30min;
(3) transfer pH to 4.8-5.0 with ammonium chloride solution, reaction to terminal;
(4) being neutralized to pH with NaOH immediately after reaction to terminal is 7.0-7.5, adds urea (36g) for the second time, and logical water quench;
(5) be cooled to 40 ℃, blowing.
Four, aspen fibers by using silicon modification: aspen fibers by using silicon successively is dried to constant weight with acetone, each extracting of running water 24 hours and in 100 ℃ in apparatus,Soxhlet's.Put into process tank and vacuumize, keep vacuum 0.096MPa20min, add inorganic nano Al then 2O 3Colloidal sol submergence fiber, after continuing to keep vacuum 10min, process tank leads to atmosphere, makes the abundant permeable fiber of colloidal sol.Fiber is poured in the beaker after sucking colloidal sol, leave standstill aging, and ultrasonic processing 10min.Suction filtration is removed colloidal sol, and fiber is dried to constant weight for 100 ℃, promptly obtains inorganic Al 2O 3The aspen fibers by using silicon of nano modification.
Five, Composite Preparation:
It is 0.8g/cm that modifying aspen fibers by using silicon is set density 3, the plate face is of a size of 20cm * 20cm * 6mm.The Composite Preparation step is as follows: dry (100 ℃ of temperature, moisture content 2-3%); Applying glue (resin added be bone dry fiber heavy 12%, 24g); Mat formation; Hot pressing (175 ℃ of hot pressing temperatures, hot pressing time 30sec/mm, hot pressing pressure 3.5Mpa); Cooling.
Six, the taper calorimeter is analyzed: intercept test specimen from the composite of preparation, be of a size of 10cm * 10cm * 6mm, adopt Britain Fire Testing Technology taper calorimeter that it is carried out the CONE experiment; It is 50kWm that heat radiation power is adopted in experiment -2In order to reduce external influence, sample all faces except that heating surface are coated with aluminium-foil paper, put into stainless steel sample fixed mount, and cut off the heat that outwards transmits from the sample back side with heat insulation foam, by the CONE test, the parameter that records has: HRR HRR, total heat burst size THR, burning time TTA.
Advantage of the present invention: with the wood-fibred is research object, and sol-gel technique is used to prepare aspen fibers by using silicon-Al 2O 3Inorganic nano composite material.The work of this respect does not appear in the newspapers both at home and abroad.Aspen fibers by using silicon-Al that this patent proposes 2O 3Nano composite material is that the structure to material designs and controls from cell/nanometer level, for the poor dimensional stability that fundamentally solves Wood Fiber Composites, problem such as apt to rot, inflammable provide new approaches.
Description of drawings
Accompanying drawing 1 is to be untreated and to handle the HRR schematic diagram of medium density fibre board (MDF).
Accompanying drawing 2 is to be untreated and to handle the THR schematic diagram of medium density fibre board (MDF).
The specific embodiment
From the composite of preparation, intercept test specimen, be of a size of 10cm * 10cm * 6mm, adopt Britain FireTesting Technology taper calorimeter that it is carried out the CONE experiment; For making experimental temperature near actual fire temperature, it is 50kW.m that heat radiation power is adopted in this experiment -2In order to reduce external influence, sample all faces except that heating surface are coated with aluminium-foil paper, put into stainless steel sample fixed mount, and cut off the heat that outwards transmits from the sample back side with heat insulation foam.
HRR HRR.Blank fiberboard and aspen fibers by using silicon/Al 2O 3The HRR-t curve of inorganic nano composite material is seen Fig. 1.Blank fiberboard and aspen fibers by using silicon/inorganic nano Al 2O 3The hot release characteristic value of composite sees Table 2.
Table 2 is untreated and handles the hot release characteristic value of medium density fibre board (MDF)
Figure GSB00000394759200041
The HRR of general timber has two exothermic peaks, the combustion process when the of short duration flaming combustion process when first exothermic peak is lighted corresponding to sample, second exothermic peak higher flame occurs corresponding to the second time.Second exothermic peak all is higher than first exothermic peak, and the area (thermal discharge) that is covered below this peak is also big than first exothermic peak, thereby mainly is the combustibility that second exothermic peak has reflected material.
From Fig. 1 as seen, compare aspen fibers by using silicon/Al with blank fiberboard 2O 3Inorganic nano composite material obviously weakens in two heat release peaks of 45s and 175s appearance, and HRR obviously reduces; As shown in Table 1, the evenly heat rate of release has descended 38%, and the HRR peak value has descended 25%.The inorganic nano aluminium oxide of introducing in this explanation wood-fibred cell can delay the transmission of heat effectively, make the cell wall constituent carbonization of can only dewatering, thereby the speed that generates flammable volatility product during the medium density fiber sheet material pyrolysis of compacting obviously reduces, the speed that the while heat is delivered to plate surface slows down, and flame retardant effect is obvious.
Total heat burst size THR
Blank fiberboard and aspen fibers by using silicon/Al 2O 3The THR-t curve of inorganic nano composite material is seen Fig. 2.Blank fiberboard and aspen fibers by using silicon/Al 2O 3Total release heat of inorganic nano composite material sees Table 3.As can be seen from Fig. 2, aspen fibers by using silicon/Al 2O 3Inorganic nano composite material is compared with blank fiberboard, and total heat that discharges descends obviously, and according to table 3 as can be known, total release heat has descended 38%.This trend is consistent with the Changing Pattern of HRR HRR.In addition, as shown in Figure 1, blank fiberboard two heat release peaks, aspen fibers by using silicon/Al occur at 55s and 235s 2O 3Two heat of inorganic nano composite material discharge the peak and appear at 45s and 175s; As can be seen from Fig. 2, lighted the second exothermic peak peak value from sample and this time period occurred, the total heat burst size increase sharply and when exothermic peak occurs the increasing degree maximum, this time period is flaming combustion; After second exothermic peak, the increase of total heat burst size is obviously slowed down, and illustrates that the heat that the sheet material burning discharges is mainly provided by flaming combustion, therefore suppresses the key that flaming combustion is a fire-retarding of wood.
Table 3 is untreated and handles the total release heat of medium density fibre board (MDF)
Figure GSB00000394759200061
Burning time TTI
TTI represents that material lighted the needed constant ignition time s of unit from being heated to.TTI is bigger, and illustrative material is difficult for lighting more, and anti-flammability is good more.
This experiment empty fiberboard burning time is 13s, aspen fibers by using silicon/inorganic nano Al 2O 3The composite burning time is 26s, compares with blank fiberboard, has increased by one times.As seen, the inorganic nano Al in the wood-fibred 2O 3Played significant flame retardant effect.
3 conclusions
With sol-gel technology preparing aspen fibers by using silicon/Al 2O 3Nano composite material, the method novelty has extensive use and is worth.Experimental results such as the HRR in the analysis-by-synthesis CONE experiment, total heat burst size, burning time are compared aspen fibers by using silicon/Al with blank fibrous plate 2O 3Inorganic nano composite material has good flame retardancy.

Claims (1)

1. aspen fibers by using silicon/Al 2O 3Nano composite material preparation method, its feature comprises following processing step:
One, aspen fibers by using silicon preparation: after the peeling of raw material poplar, chipping, wood chip is put into autoclaving pot boiling 40min, keep-uping pressure is 1.5MPa; Chip raw material behind the poach is put into high concentration plate mill and is processed into fiber, treat air dry after, carry out secondary and pulverize, placing electric drying oven with forced convection to be dried to moisture content then is 8% with standby;
Two, Al 2O 3Colloidal sol preparation: 1mol/L ammoniacal liquor is added drop-wise in the 0.96mol/L aluminum nitrate solution, make final pH＞9.20, obtain precipitation with Bush's funnel suction filtration, and spend the deionised water precipitation repeatedly, until system pH near 7.0,50 ℃ of last constant temperature, gradation adds the 0.94mol/L salpeter solution to system pH=3.5～4.1 in precipitation, can obtain transparent Al 2O 3Colloidal sol;
Three, urea-formaldehyde resin adhesive preparation: solid content 52%, viscosity 20mPas, pH value 7.0-7.5, the raw material that uses in the urea-formaldehyde resin adhesive preparation process: 37% formaldehyde, 700 grams; 98% urea, 300 grams; 99% melamine, 18 grams; 10% NaOH is an amount of; 20% ammonium chloride is an amount of;
Concrete preparation technology comprises:
(1) formaldehyde metering back is added reaction pot, transfer pH to 7.5-8.5, add urea 264g and all melamine for the first time with sodium hydroxide solution;
(2) in 40-50min, be warmed up to 90 ± 1 ℃, insulation 30min;
(3) transfer pH to 4.8-5.0 with ammonium chloride solution, reaction to terminal;
(4) being neutralized to pH with NaOH immediately after reaction to terminal is 7.0-7.5, adds urea 36g for the second time, and logical water quench;
(5) be cooled to 40 ℃, blowing;
Four, aspen fibers by using silicon modification: aspen fibers by using silicon successively is dried to constant weight with acetone, each extracting of running water 24 hours and in 100 ℃ in apparatus,Soxhlet's; Put into process tank and vacuumize, keep vacuum 0.096MPa20min, add Al then 2O 3Colloidal sol submergence fiber, after continuing to keep vacuum 10min, process tank leads to atmosphere, makes the abundant permeable fiber of colloidal sol; Fiber is poured in the beaker after sucking colloidal sol, leave standstill aging, and ultrasonic processing 10min; Suction filtration is removed colloidal sol, and fiber is dried to constant weight for 100 ℃, promptly obtains inorganic Al 2O 3The aspen fibers by using silicon of nano modification;
Five, Composite Preparation:
It is 0.8g/cm that modifying aspen fibers by using silicon is set density 3, the plate face is of a size of 20cm * 20cm * 6mm, and the Composite Preparation step is as follows: 100 ℃ of baking temperatures, moisture content 2-3%; Applying glue, resin added be bone dry fiber heavy 12%, 24g; Mat formation; Hot pressing, 175 ℃ of hot pressing temperatures, hot pressing time 30sec/mm, hot pressing pressure 3.5Mpa; Cooling.
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CN102175718A (en) * 2011-02-23 2011-09-07 中南林业科技大学 Method for measuring combustion performance of powder or liquid sample by utilizing cone calorimeter
CN106633977A (en) * 2016-11-23 2017-05-10 浙江农林大学 Nanometer matter/biomass fibrous composite and preparation method for nanometer matter/biomass fibrous composite
CN107962657A (en) * 2017-11-13 2018-04-27 常州凯途纺织品有限公司 A kind of preparation method of core-board

Citations (4)

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Publication number Priority date Publication date Assignee Title
DE19647368A1 (en) * 1996-11-15 1998-05-20 Inst Neue Mat Gemein Gmbh Composites
CN1586843A (en) * 2004-09-14 2005-03-02 广西大学 Method for producing nano artificial board
WO2006066488A1 (en) * 2004-12-21 2006-06-29 Anson Nanotechnology Group Co., Ltd. Manufacturing methods and applications of antimicrobial plant fibers having silver particles
KR20080072437A (en) * 2007-02-02 2008-08-06 주식회사 제이에스마루 Wood flooring and method of manufacturing the same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19647368A1 (en) * 1996-11-15 1998-05-20 Inst Neue Mat Gemein Gmbh Composites
CN1586843A (en) * 2004-09-14 2005-03-02 广西大学 Method for producing nano artificial board
WO2006066488A1 (en) * 2004-12-21 2006-06-29 Anson Nanotechnology Group Co., Ltd. Manufacturing methods and applications of antimicrobial plant fibers having silver particles
KR20080072437A (en) * 2007-02-02 2008-08-06 주식회사 제이에스마루 Wood flooring and method of manufacturing the same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
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袁光明等.几种用于木材纳无机纳米复合材料的纳米粒子分散与改性研究.《武汉理工大学学报(交通科学与工程版)》.2008,第32卷(第1期),142-145. *

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