CN103112066A - Wood flour modifier, wood flour modified thereby, and preparation method of wood flour - Google Patents
Wood flour modifier, wood flour modified thereby, and preparation method of wood flour Download PDFInfo
- Publication number
- CN103112066A CN103112066A CN2013100299907A CN201310029990A CN103112066A CN 103112066 A CN103112066 A CN 103112066A CN 2013100299907 A CN2013100299907 A CN 2013100299907A CN 201310029990 A CN201310029990 A CN 201310029990A CN 103112066 A CN103112066 A CN 103112066A
- Authority
- CN
- China
- Prior art keywords
- wood powder
- modifier
- sodium
- wood
- ddac
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention provides a wood flour modifier; the wood flour modifier is prepared from na-montmorillonite, didecyl dimethyl ammonium chloride, polyethylene glycol and de-ionized water which are mixed and then dispersed by a ball mill; and the cation exchange capacity of the na-montmorillonite and the didecyl dimethyl ammonium chloride is 1:(0.5-1). The modifier provided by the invention is simple in process, is obtained in one step and is easy to operate. The invention further provides a method for modifying wood flour by using the modifier; the modifier provided by the invention can improve wood plastic composite material interfacial compatibility, the wood flour is converted from ordinary packing into reinforcing material and becomes the wood flour especially for wood plastic composite material.
Description
Technical field
The present invention relates to wood powder, the preparation method of a kind of wood powder modifier and modification thereof, belong to wood processing field.
Background technology
Wood plastic composite (Wood-plastic composite, WPC) is composited by timber and plastics, due to the double dominant that combines timber and plastics, so have good combination property.Yet there is a large amount of polar functional groups in wood surface, in the recombination process of wood plastic composite, between the plastic material of hydrophilic wood materials and hydrophobicity, exists higher interface energy poor, and bi-material is difficult to reach sufficient surface and mutually merges.In addition, the hydrogen bond action between wood surface also makes the lumber fibre can not Uniform Dispersion in thermoplastic, thereby has affected the performance of wood plastic composite.Therefore, improving the compatibility at wood plastic composite interface, is one of effective way that improves the wood plastic composite performance.
The method that tradition is improved the wood plastic composite interface compatibility mainly contains three kinds: (1) carries out pretreatment to wooden raw material, reduces the polarity of wood material or removes the interface in conjunction with disadvantageous extract; (2) plastic raw materials is carried out pretreatment, improve the polarity of plastics.(3) add the 3rd component, i.e. coupling agent.Simply effective because of it, be to adopt at present maximum a kind of method of modifying.
Imvite is a kind of laminar silicic acid salt compounds of 2:1 type, has high specific area and the reactable of interlayer, and is widely distributed in China.It is also in recent years study hotspot that nano imvite is used for wood plastic composite, use imvite to add the physical and mechanical property that can increase substantially wood plastic composite in wood plastic composite to, but usually nano imvite to the modification of wood plastic composite mainly for remain wherein macromolecule rather than wood powder.Usually just the simple mixed refining process by nano imvite and wood powder and plastics prepares composite, or carries out compound making with wood powder by nano imvite again after to modifying plastics.In this process, wood powder still just plays the effect of a filler.In addition, as (Journal of Reinforced Plastics and Composites29 such as Hemmasi, 964-971) studies show that, when adding to imvite in wood plastic composite, after imvite too high levels (higher than 6%), can stick in a large number wood powder surface and plastics compound tense and can form weak interface layer, affect interface compatibility, reduce on the contrary the performance of composite.In addition, when adding imvite to wood plastic composite, general also need to be in the situation that carry out compound use with coupling agent etc., the performance of composite just can obviously increase.
Summary of the invention
The purpose of this invention is to provide a kind of wood powder modifier.
Another purpose of the present invention is to provide the method for wood powder modifier modification wood powder.
Still a further object of the present invention is to provide a kind of wood powder of modification.
In order to realize the object of the invention, the invention provides a kind of wood powder modifier, described wood powder modifier is after being mixed by sodium-based montmorillonite, DDAC, polyethylene glycol and deionized water, to be prepared from through the ball milling dispersion treatment; Described sodium-based montmorillonite and DDAC cation exchange capacity (CEC) are 1:0.5-1; Be preferably 1:0.7.
The weight ratio of described sodium-based montmorillonite and dispersant polyethylene glycol is 1:0.1-0.4, is preferably 1:0.2.
The preparation of described wood powder modifier comprises the following steps:
1) sodium-based montmorillonite, DDAC, polyethylene glycol and deionized water are mixed;
2) adopt ball mill with 1) in mixed liquor carry out low speed ball milling dispersion treatment;
3) with 2) mixed liquor after processing carries out high speed ball milling dispersion treatment, obtains wood powder modifier.
Described 1) in, sodium-based montmorillonite and DDAC cation exchange capacity (CEC) are 1:0.5-1; Preferred 1:0.7.
Described 1) in, the weight ratio of sodium-based montmorillonite and dispersant polyethylene glycol is 1:0.1-0.4; Be preferably 1:0.2.
Described 2) in, the rotating speed of low speed ball milling dispersion treatment is 80-150r/min, preferred 100r/min, and the time is 5-15min, preferred 10min; The diameter of the large ball in described ball mill is 9-11mm; The small ball's diameter is 4-6mm; Large ball is 1:6-20 with the ratio of the number of bead, is preferably 1:15;
Described 3) rotating speed of high speed ball milling dispersion treatment is 200-300r/min, and the time is 1-3h.
The present invention also provides the method for above-mentioned wood powder modifier modification wood powder, comprises the steps:
Step 2, first wood powder is carried out application of vacuum, then import the wood powder modifier after dilution in step 1, make wood powder modifier soak wood powder fully; Again wood powder is carried out pressurized treatments, be dried to constant weight, obtain the wood powder after modification.
Described step 2 comprises the steps:
1) open vavuum pump and vacuumize processing, when the relative vacuum degree reach-during 0.05--0.1MPa, keeping closing vavuum pump after 20-60min under this relative vacuum degree state, import simultaneously modifier; Described relative vacuum degree is preferably-0.07--0.096MPa.
2) open pressurizing valve and carry out pressurized treatments, when relative pressure reaches 0.5-1.5MPa, wood powder is carried out pressurized treatments, keeping closing pressurizing valve, pressure relief after 60min under this relative pressure state.
The wood powder of described said method modification.
Beneficial effect of the present invention is as follows:
1, in the present invention, sodium-based montmorillonite and DDAC (DDAC) carry out cation exchange, use the sodium ion in the long chain quaternary instead of sodium base montmorillonite in DDAC.Adopt DDAC that sodium-based montmorillonite is carried out organically-modified, improve the interlamellar spacing of wood powder modifier, change the hydrophilic environment of interlayer, improve simultaneously the dispersion stabilization of wood powder modifier by electrostatic interaction.
But find also have the effect of surfactant due to DDAC through great many of experiments, after DDAC was excessive, remaining DDAC can cause organo montmorillonite generation backward reaction to regenerate sodium-based montmorillonite.And along with the cation exchange capacity (CEC) of DDAC increases, the settling volume of modifier also increases thereupon gradually.When the cation exchange capacity (CEC) of sodium-based montmorillonite and DDAC is 1:0.7, the modifier of preparation is through after the placement of 24 hours, settling volume percentage is about 5%, and when the cation exchange capacity (CEC) of sodium-based montmorillonite and DDAC was 1:1, settling volume percentage was about 7%.Therefore, the best cation exchange capacity (CEC) of determining sodium-based montmorillonite and DDAC is 1:0.7.Prepared modifier suspension is better under this proportioning, and performance is more stable.
2, polyethylene glycol itself is a kind of polymer of long-chain, contains some hydroxyls, can increase the suspension stability of modifier, extends the sedimentation time.
After placing through 24 hours, settling volume percentage is compared and is not added the polyethylene glycol group and can reduce by 1～2%.When sodium-based montmorillonite and polyethylene glycol weight ratio are 1:0.2, and select the polyethylene glycol of molecular weight 1000, settling volume percentage was about 3% in 24 hours; When polyethylene glycol and sodium-based montmorillonite weight ratio less than 0.2 the time, settling volume percentage was about 5% in 24 hours, and along with polyethylene glycol and sodium-based montmorillonite weight ratio increase, settling volume percentage is almost unchanged, consider economic factor, determine that polyethylene glycol and sodium-based montmorillonite optimum weight ratio are 0.2.
In addition, when molecular weight polyethylene glycol hour, the modifier less stable, along with molecular weight polyethylene glycol increases gradually, modifier stability is better, but after molecular weight surpassed 4000, settling volume percentage can reduce again in 24 hours, thus the present invention to select best molecular weight polyethylene glycol be 1000.
3, in the present invention, the preparation process of modifier has adopted ball grinding technique, greatly reduced the degree of aggregation of sodium-based montmorillonite particle, promoted sodium-based montmorillonite evenly to mix and catalytic chance with polyethylene glycol, DDAC, the chance that the active ingredient that has improved modifier enters and reacts with wood powder.
Adopt the modifier average grain diameter of ball milling dispersion technology preparation less, the organo montmorillonite of particle diameter in gained modifier≤10 μ m occupies 52.42% of machine imvite gross weight.Adopt that high speed ball milling dispersion treatment is because the low speed ball-milling treatment can first make sodium-based montmorillonite and modifier after first low speed, dispersant and deionized water mix, if directly adopt high speed ball milling dispersion treatment, there is most of sodium-based montmorillonite to adhere to ball milling cover inwall under the high speed centrifugation effect and abundant reaction can not occur, can make the weight of remaining sodium-based montmorillonite increase 1-2%.
The area that when the bead number can improve ball milling with diameter, sodium-based montmorillonite contacts with ball, the organo montmorillonite particle diameter of preparation is less, if the bead number is less, the particle diameter that prepares organo montmorillonite can be slightly bigger than normal, and what the organo montmorillonite of≤10 μ m only occupied machine imvite gross weight is about 45%.Hence one can see that, and bead number, diameter play vital effect to the modifier particle size.
Wood powder modifier capability and performance of the present invention is stable, and granularity is little, is uniformly dispersed, and occurs without reunion, deposited phenomenon; And make simple, only need sodium-based montmorillonite, after mixing, DDAC and dispersant polyethylene glycol carry out dispersion treatment, for conventional method, need not be first sodium-based montmorillonite be carried out carrying out compound with macromolecule dispersing agent again after organically-modified, technique is simple, easy operating.
4, adopt the modifier of average grain diameter≤10 μ m in modified wood powder method of the present invention, make when impregnating wood powder and need to by the macromolecule intermediate medium, can not complete in a step.
5, the wood powder moisture pick-up properties after the modification of the present invention's preparation obviously descends, modifier enters into the wood powder lumen by conduit, pit etc., part can enter into the wood powder cell membrane, with the effect of cell membrane inner base material generation intercalation, after modification, obviously reduce on wood powder surface carbon content relatively, and oxygen, silicon, aluminium content rise.
6, the invention solves in wood plastic composite when adding organo montmorillonite, too much organo montmorillonite can stick to the wood powder surface and form the phenomenon of weak interface layer, but most of organo montmorillonite Uniform Dispersion enters wood powder inside.
After modification of the present invention wood powder, service efficiency improves greatly, is converted into " reinforcing material " from simple " filler ", becomes the wood powder that is exclusively used in wood plastic composite.
Description of drawings
Fig. 1 is the XRD contrast figure of embodiment 1, embodiment 3 and reference examples 1 gained wood powder.
Fig. 2 (a) is the SEM picture of the wood powder of reference examples 1.
Fig. 2 (b) is the SEM picture of the wood powder of embodiment 1.
Fig. 3 (a) is the picture of the wood powder of embodiment 1.
Fig. 3 (b) is the distribution map of Si element in embodiment 1.
Fig. 3 (c) is the distribution map of Al element in embodiment 1.
Fig. 4 (a) is the hydroscopicity comparison diagram of embodiment 1 and Comparative Examples 1.
Fig. 4 (b) is the hydroscopicity comparison diagram of embodiment 2 and Comparative Examples 2.
Fig. 4 (c) is the hydroscopicity comparison diagram of embodiment 3 and Comparative Examples 1.
Fig. 5 (a) is the water absorption rate comparison diagram of embodiment 1, embodiment 3 and Comparative Examples 1.
Fig. 5 (b) is the water absorption rate comparison diagram of embodiment 2 and Comparative Examples 2.
The specific embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
In the present invention, except specified otherwise, described concentration is mass percent concentration.
Wood powder is selected Chinese white poplar wood powder (Populus tomentasa Carr.), 10-60 order, Gaocheng, Hebei wood powder factory of Xingda; Sodium-based montmorillonite (Na-MMT), 200 orders, cation exchange capacity (CEC) is 90mmol/100g, interlamellar spacing is 1.459nm, Zhejiang Feng Hong clay chemical industry Co., Ltd; DDAC (DDAC), the rich biochemical technology of mass percent concentration 70%, three (Shanghai) Co., Ltd.; Polyethylene glycol (PEG), molecular weight 1000, Liaoning Province Fushun Jiahua Chemicals Co., Ltd; PLA (poly-left-handed, as easily to give birth to the AI-1001 type), number-average molecular weight 80000, density 1.25g/cm
3, melt index 10-20g/min, Shenzhen brilliance great achievement Industrial Co., Ltd..
(1) preparation modifier
The polyethylene glycol (PEG-1000) of sodium-based montmorillonite (Na-MMT), DDAC (DDAC), molecular weight 1000 and deionized water are added in ball mill (spring dragon laboratory apparatus Co., Ltd) carry out the ball milling dispersion treatment, it is 75 of the beads of 5mm that diameter is wherein arranged in ball mill, diameter is 5, the large ball of 10mm, at first after carrying out dispersion treatment 10min under the grinding rate of 100r/min, again the grinding rotary speed of ball mill is brought up to 260r/min, ball milling 2h, the granularity of sodium-based montmorillonite particle is reduced, namely get modifier.Wherein, the ratio of the cation exchange capacity (CEC) of sodium-based montmorillonite and DDAC (DDAC) is 1:0.7; The weight portion proportioning of sodium-based montmorillonite and cetomacrogol 1000 (PEG-1000) is 1:0.2.The organo montmorillonite of particle diameter in gained modifier≤10 μ m occupies 52.42% of machine imvite gross weight.
(2) preparation of the wood powder after modification
Add deionized water in modifier, dilute, stir, obtain the diluting modification agent, the mass percent concentration that makes organo montmorillonite in the diluting modification agent is 0.5%.Wood powder is placed in beaker, carries out vacuum pressure impregnating and process in immersion can.Connect vacuum equipment and pressurized equipment, guarantee to start and close pressurizing valve when vavuum pump vacuumizes; Close vavuum pump when opening pressurizing valve.Open vavuum pump and vacuumize processing, relative vacuum degree in the vacuum pressed tank is reached-0.096MPa, keep closing vavuum pump after 30min, import simultaneously preparation organo montmorillonite mass percent concentration be 0.5% modifier, and make modifier soak wood powder fully; Open pressurizing valve, pass into compressed nitrogen in immersion can, make it relative pressure and reach 0.6MPa, wood powder is carried out pressurized treatments, after keeping 60min under this pressure state, close pressurizing valve, pressure relief obtains the wood powder in beaker afterwards with the sieves filtration, put into dish, be dried to constant weight in 80 ℃ of air dry ovens, the gained wood powder is of a size of 60 orders.
(3) preparation of wood powder/lactic acid composite material
The wood powder of modification is mixed 4min with PLA according to mass ratio 1:1, rotating speed 2900rpm in high-speed mixer.Afterwards, mixture is extruded by the double screw extruder melt blending, the temperature setting area of extruder is respectively 150/160/180/180/150 ℃, rotating speed 180rpm.Compound after extruding is pulverized into about the particle about 5mm, dry 2h in 105 ℃ of air dry ovens.Use hot press to prepare wood powder/lactic acid composite material.Composite is preset density 1.28g/cm
3, size 270 * 270 * 3mm.In mould, in mould, paving one deck poly tetrafluoroethylene is as release materials with 280g hybrid particles uniform spreading.Hot pressing 6min in hot press, pressure 4MPa, 180 ℃ of temperature, the 6min that at room temperature once colds pressing afterwards fixes, pressure 4MPa.Cold pressing complete after, namely obtain wood powder/lactic acid composite material.
Embodiment 2
In experimentation except using Chinese white poplar wood powder (Populus tomentasa Carr.), the 60-80 order, beyond the wood powder factory of Xingda of Gaocheng, Hebei, all the other are all identical with embodiment 1.
Embodiment 3
Be 1% except the mass percent concentration that uses organic imvite modified dose in experimentation, all the other are all identical with embodiment 1.
Embodiment 4
(1) preparation modifier
The polyethylene glycol (PEG-4000) of sodium-based montmorillonite (Na-MMT), DDAC (DDAC), molecular weight 4000 and deionized water are added in ball mill (spring dragon laboratory apparatus Co., Ltd) carry out the ball milling dispersion treatment, it is 36 of the beads of 4mm that diameter is wherein arranged in ball mill, diameter is 6, the large ball of 9mm, at first after carrying out dispersion treatment 15min under the grinding rate of 150r/min, again the grinding rotary speed of ball mill is brought up to 300r/min, ball milling 3h, the granularity of sodium-based montmorillonite particle is reduced, namely get modifier.Wherein, the ratio of the cation exchange capacity (CEC) of sodium-based montmorillonite and DDAC (DDAC) is 1:1; The weight portion proportioning of sodium-based montmorillonite and Macrogol 4000 (PEG-4000) is 1:0.4; The organo montmorillonite of particle diameter in gained modifier≤10 μ m occupies 54.76% of machine imvite gross weight.
(2) preparation of the wood powder after modification
Add deionized water in modifier, dilute, stir, obtain the diluting modification agent, the mass percent concentration that makes organo montmorillonite in the diluting modification agent is 0.1%.Wood powder is placed in beaker, carries out vacuum pressure impregnating and process in immersion can.Connect vacuum equipment and pressurized equipment, namely start and close pressurizing valve when vavuum pump vacuumizes; Close vavuum pump when opening pressurizing valve.Open vavuum pump and vacuumize processing, relative vacuum degree in the vacuum pressed tank is reached-0.07MPa, keep closing vavuum pump after 60min, the mass percent concentration that imports simultaneously preparation is 0.1% organo montmorillonite suspension, and makes organo montmorillonite suspension soak wood powder fully; Open pressurizing valve, pass into compressed nitrogen in immersion can, make it relative pressure and reach 0.5MPa, wood powder is carried out pressurized treatments, after keeping 120min under this pressure state, open vent valve, pressure relief obtains the wood powder in beaker afterwards with the sieves filtration, put into dish, be dried to constant weight in 105 ℃ of air dry ovens, the gained wood powder is of a size of 10 orders.
(3) preparation of wood powder/lactic acid composite material
Identical with embodiment 1.
In experimentation, except following steps, all the other are all identical with embodiment 1.
(1) preparation modifier
with sodium-based montmorillonite (Na-MMT), DDAC (DDAC), the polyethylene glycol of molecular weight 400 (PEG-400) and deionized water add in ball mill (spring dragon laboratory apparatus Co., Ltd) carries out the ball milling dispersion treatment, it is 160 of the beads of 6mm that diameter is wherein arranged in ball mill, diameter is 8, the large ball of 11mm, at first after carrying out dispersion treatment 5min under the grinding rate of 80r/min, again the grinding rotary speed of ball mill is brought up to 200r/min, ball milling 1h, the granularity of sodium-based montmorillonite particle is reduced, namely get modifier, wherein, the ratio of the cation exchange capacity (CEC) (CEC) of sodium-based montmorillonite and DDAC (DDAC) is 1:0.5, the weight portion proportioning of sodium-based montmorillonite and PEG400 (PEG-400) is 1:0.1, the organo montmorillonite of particle diameter in gained modifier≤10 μ m occupies 58.83% of machine imvite gross weight.
(2) preparation of the wood powder after modification
Add deionized water in modifier, dilute, stir, obtain the diluting modification agent, the mass percent concentration that makes organo montmorillonite in the diluting modification agent is 1%.Wood powder is placed in beaker, carries out vacuum pressure impregnating and process in immersion can.Connect vacuum equipment and pressurized equipment, namely start and close pressurizing valve when vavuum pump vacuumizes; Close vavuum pump when opening pressurizing valve.Open vavuum pump and vacuumize processing, relative vacuum degree in the vacuum pressed tank is reached-0.096MPa, keep closing vavuum pump after 20min, the mass percent concentration that imports simultaneously preparation is 1% organo montmorillonite suspension, and makes organo montmorillonite suspension soak wood powder fully; Open pressurizing valve, pass into compressed nitrogen in immersion can, make it relative pressure and reach 1.5MPa, wood powder is carried out pressurized treatments, after keeping 30min under this pressure state, open vent valve, pressure relief obtains the wood powder in beaker afterwards with the sieves filtration, put into dish, be dried to constant weight in 60 ℃ of air dry ovens, the gained wood powder is of a size of 100 orders.
(3) preparation of wood powder/lactic acid composite material
Identical with embodiment 1.
Reference examples 1
In experimentation, except directly impregnating wood powder with deionized water, all the other are identical with embodiment 1.
Reference examples 2
In experimentation, except directly impregnating wood powder with deionized water, all the other are identical with embodiment 2.
Interpretation of result:
1, X-ray diffraction analysis
Adopt XRD-6000 type X-ray diffractometer (XRD) that Japanese Shimadzu produces to carry out XRD to the wood powder of embodiment 1, embodiment 3 and reference examples 1 and characterize, as shown in Figure 1.
1) wood powder and the unmodified wood powder of reference examples 1 after embodiment 1, embodiment 3 modifications is 17 ° at 2 θ, 22.5 ° and the diffraction maximum of 35 ° of (101) that the wood powder fiber occurs, (002) and (040), and the position of diffraction maximum does not change, modification is described after the cellulosic crystalline texture of wood powder do not have destroyed.
2) wood powder after embodiment 1 and embodiment 3 modifications is through ° having located to occur a new diffraction maximum in 2 θ=3.60 after modification, and this is the characteristic peak of organo montmorillonite, and the interlamellar spacing of corresponding organo montmorillonite is 2.451nm.Because the interlamellar spacing of sodium-based montmorillonite itself is 1.459nm, therefore, has illustrated that the present invention can successfully change sodium-based montmorillonite into organo montmorillonite, and successfully entered wood powder inside under vacuum pressed is processed.
2, in modifier, organo montmorillonite distributes in wood powder
After embodiment 1 is processed through vacuum metallizing with the wood powder of reference examples 1, adopt the S-3000N type SEM (SEM) that Titachi company produces that specimen surface is observed,
In analysis modifier, active ingredient is in the distribution of wood powder lumen, and observed result is as shown in Fig. 2 (a), Fig. 2 (b).
By Fig. 2 (a), Fig. 2 (b) as can be known: wood powder is through after modification, occurred the particle of some organo montmorillonites in the wood powder lumen, illustrated that the organo montmorillonite of modification can be under the condition of impregnating deposits to wood powder inside by passages such as timber conduit, cross trachields.
3, the distribution of each element in wood powder
After the wood powder of embodiment 1, embodiment 3 and reference examples 1 is processed through vacuum metallizing, the 7021-H X-ray energy spectrometer (EDXA) that employing Horiba company produces is analyzed specimen surface under face is swept pattern, analyze Si and the distribution of Al element in wood powder and the content of each element of modifier organo montmorillonite, observed result is as shown in Fig. 3 (a), Fig. 3 (b), Fig. 3 (c).
Fig. 3 (a) is the picture of the wood powder of embodiment 1, and Fig. 3 (b) is the distribution map of Si element in embodiment 1, and Fig. 3 (c) is the distribution map of Al element in embodiment 1.
By Fig. 3 (a), Fig. 3 (b), Fig. 3 (c) as can be known: the content of Si and Al element can be detected in the cell membrane of wood powder, illustrate that organo montmorillonite has entered into the wood powder cell membrane inner.Each element percentage composition of reference examples 1, embodiment 1 and embodiment 3 is as shown in table 1.
Each constituent content value in table 1 wood powder
As shown in Table 1: wood powder is through after modification, and the relative amount of C element descends, and the relative amount of O, Si and Al rises, and has illustrated that organo montmorillonite has entered into wood powder; And the content of Na and Cl is zero, and illustrating does not have after modification Na and Cl to remain in the wood powder surface.
4, wood powder hygroscopicity test
Unmodified wood powder to the wood powder after the modification of embodiment 1-3 and reference examples 1-2 carries out the test of wood powder hygroscopicity.
At first wood powder is dried to constant weight under 105 ℃, takes approximately the 2g wood powder and put into tinfoil,
Tinfoil is put into the drier that deionized water is housed carry out hygroscopicity mensuration, environment temperature is 23 ± 2 ℃, and relative humidity is near 100%.Wood powder taken out and weigh through certain hour, and calculating rate of body weight gain.Result is as shown in Fig. 4 (a), Fig. 4 (b), Fig. 4 (c).
By Fig. 4 (a), Fig. 4 (b), Fig. 4 (c) as can be known: wood powder is through after modification, and moisture absorption speed descends, and finally hygroscopicity obviously descends, and embodiment 1 and the whole hydroscopicity of embodiment 3 are 20.70% and 20.21%, and the whole hydroscopicity of reference examples 1 is 22.02%; Equally, the whole hydroscopicity of embodiment 2 is 20.21%, and the whole hydroscopicity of reference examples 2 is 23.80%, and through after modification, the hygroscopicity of wood powder has reduction in various degree.
5, the suction hygroscopicity of wood powder/lactic acid composite material test
To the hygroscopicity test that absorbs water of unmodified wood powder/lactic acid composite material of the wood powder/lactic acid composite material after the modification of embodiment 1-3 and reference examples 1-2.
According to national standard " wood-plastic decorative board " (GB/T24137-2009) in, to water imbibition and the thickness swelling rate of the absorptive assay method standard testing of wood plastic composite wood plastic composite.
The water absorption rate result is as shown in Fig. 5 (a), Fig. 5 (b).
By Fig. 5 (a), Fig. 5 (b) result as can be known: the rate of water absorption of the wood powder/lactic acid composite material after modification is compared unmodified wood powder/lactic acid composite material with whole moisture content obvious decline.Wherein, the whole moisture content of embodiment 1 and embodiment 3 is 9.75% and 10.53%, and reference examples 1 is 11.05%; The whole moisture content of embodiment 2 is 10.03%, and reference examples 2 is 11.26%.
The thickness swelling rate result is as shown in table 2.
Table 2 thickness swelling rate result
As shown in Table 2: the thickness swelling rate of the wood powder/lactic acid composite material after modification also reduces obviously, and the thickness swelling rate of embodiment 1-3 can be reduced to 4.66-5.85%, and the dimensionally stable property improvement of composite is obvious.
6, the bending resistance of wood powder/lactic acid composite material experiment
According to national standard " wood-plastic decorative board " (GB/T24137-2009) in, to MOR and the elastic modelling quantity of the assay method standard testing wood plastic composite of wood plastic composite anti-bending strength.Result is as shown in table 3.
Table 3 anti-bending strength measurement result
As shown in Table 3: modifier enters the intensity that has improved wood powder after wood powder inside, has played the effect of " reinforcing material ", and the wood plastic composite MOR of preparation is obvious except the raising of embodiment 3, substantially at 55MPa.Elastic modelling quantity increases obviously, can reach 6.02GPa.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements, all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a wood powder modifier, is characterized in that, after being mixed by sodium-based montmorillonite, DDAC, polyethylene glycol and deionized water, is prepared from through the ball milling dispersion treatment; Described sodium-based montmorillonite and DDAC cation exchange capacity (CEC) are 1:0.5-1.
2. wood powder modifier according to claim 1, is characterized in that, described sodium-based montmorillonite and DDAC cation exchange capacity (CEC) are 1:0.7.
3. wood powder modifier according to claim 1, is characterized in that, the weight ratio of described sodium-based montmorillonite and dispersant polyethylene glycol is 1:0.1-0.4, is preferably 1:0.2.
4. the method for the arbitrary described wood powder modifier modification wood powder of claim 1-3, is characterized in that, comprises the steps:
Step 1, with deionized water dilution wood powder modifier, the mass percent concentration that makes the organo montmorillonite in wood powder modifier is 0.1-1%;
Step 2, first wood powder is carried out application of vacuum, then import the wood powder modifier after dilution in step 1, make wood powder modifier soak wood powder fully; Again wood powder is carried out pressurized treatments, be dried to constant weight, obtain the wood powder after modification.
5. method according to claim 4, is characterized in that, in described step 1, the preparation of wood powder modifier comprises the following steps:
1) sodium-based montmorillonite, DDAC, polyethylene glycol and deionized water are mixed;
2) adopt ball mill with 1) in mixed liquor carry out low speed ball milling dispersion treatment;
3) with 2) mixed liquor after processing carries out high speed ball milling dispersion treatment, obtains wood powder modifier.
6. method according to claim 5, is characterized in that, described 1), sodium-based montmorillonite and DDAC cation exchange capacity (CEC) are 1:0.5-1; Preferred 1:0.7.
7. method according to claim 5, is characterized in that, described 1), the weight ratio of sodium-based montmorillonite and dispersant polyethylene glycol is 1:0.1-0.4; Be preferably 1:0.2.
8. method according to claim 5, is characterized in that, described 2), the rotating speed of low speed ball milling dispersion treatment is 80-150r/min, preferred 100r/min, and the time is 5-15min, preferred 10min; The diameter of the large ball in described ball mill is 9-11mm; The small ball's diameter is 4-6mm; Large ball is 1:6-20 with the ratio of the number of bead, is preferably 1:15;
Described 3) rotating speed of high speed ball milling dispersion treatment is 200-300r/min, and the time is 1-3h.
9. method according to claim 4, is characterized in that, described step 2 comprises the steps:
1) open vavuum pump and vacuumize processing, when the relative vacuum degree reach-during 0.05--0.1MPa, keeping closing vavuum pump after 20-60min under this relative vacuum degree state, import simultaneously modifier; Described relative vacuum degree is preferably-0.07--0.096MPa;
2) open pressurizing valve and carry out pressurized treatments, when relative pressure reaches 0.5-1.5MPa, wood powder is carried out pressurized treatments, keeping closing pressurizing valve, pressure relief after 60min under this relative pressure state.
10. the wood powder that in claim 4-9, arbitrary described method prepares.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100299907A CN103112066A (en) | 2013-01-25 | 2013-01-25 | Wood flour modifier, wood flour modified thereby, and preparation method of wood flour |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100299907A CN103112066A (en) | 2013-01-25 | 2013-01-25 | Wood flour modifier, wood flour modified thereby, and preparation method of wood flour |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103112066A true CN103112066A (en) | 2013-05-22 |
Family
ID=48410486
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013100299907A Pending CN103112066A (en) | 2013-01-25 | 2013-01-25 | Wood flour modifier, wood flour modified thereby, and preparation method of wood flour |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103112066A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104277377A (en) * | 2014-10-31 | 2015-01-14 | 安徽省三乐门窗幕墙工程有限公司 | Heat-preservation plastic door and window filler and preparation method thereof |
| CN104292704A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Strengthening filler for plastic doors and windows and preparation method of strengthening filler |
| CN104292705A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Special calcium carbonate filler for PVC doors and windows, and preparation method thereof |
| CN104292706A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Flame retardant PVC plastic door and window filler and preparation method thereof |
| CN104292707A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Oxidation resisting calcium carbonate filler and preparation method thereof |
| CN104356543A (en) * | 2014-10-31 | 2015-02-18 | 安徽省三乐门窗幕墙工程有限公司 | Filler for plastic door window and preparation method of filler |
| CN106380607A (en) * | 2016-08-29 | 2017-02-08 | 桂林舒康建材有限公司 | Preparation method of modified wood powder |
| CN111410828A (en) * | 2020-05-15 | 2020-07-14 | 运城学院 | Preparation method of plant wood powder/montmorillonite filled high-performance fully biodegradable polylactic acid composite material |
| CN112048936A (en) * | 2020-09-17 | 2020-12-08 | 齐鲁工业大学 | Method for preparing coating by using biomass, coating and sizing material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012040910A1 (en) * | 2010-09-28 | 2012-04-05 | 北京林业大学 | Wood modifier, preparation method thereof and method for modifying wood using the same |
-
2013
- 2013-01-25 CN CN2013100299907A patent/CN103112066A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012040910A1 (en) * | 2010-09-28 | 2012-04-05 | 北京林业大学 | Wood modifier, preparation method thereof and method for modifying wood using the same |
Non-Patent Citations (1)
| Title |
|---|
| 姜卸宏等: "MMT/PVA/木材复合材料的物理力学性能", 《林产化学与工业》, vol. 31, no. 1, 28 February 2011 (2011-02-28), pages 41 - 46 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104277377A (en) * | 2014-10-31 | 2015-01-14 | 安徽省三乐门窗幕墙工程有限公司 | Heat-preservation plastic door and window filler and preparation method thereof |
| CN104292704A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Strengthening filler for plastic doors and windows and preparation method of strengthening filler |
| CN104292705A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Special calcium carbonate filler for PVC doors and windows, and preparation method thereof |
| CN104292706A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Flame retardant PVC plastic door and window filler and preparation method thereof |
| CN104292707A (en) * | 2014-10-31 | 2015-01-21 | 安徽省三乐门窗幕墙工程有限公司 | Oxidation resisting calcium carbonate filler and preparation method thereof |
| CN104356543A (en) * | 2014-10-31 | 2015-02-18 | 安徽省三乐门窗幕墙工程有限公司 | Filler for plastic door window and preparation method of filler |
| CN106380607A (en) * | 2016-08-29 | 2017-02-08 | 桂林舒康建材有限公司 | Preparation method of modified wood powder |
| CN111410828A (en) * | 2020-05-15 | 2020-07-14 | 运城学院 | Preparation method of plant wood powder/montmorillonite filled high-performance fully biodegradable polylactic acid composite material |
| CN112048936A (en) * | 2020-09-17 | 2020-12-08 | 齐鲁工业大学 | Method for preparing coating by using biomass, coating and sizing material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103112066A (en) | Wood flour modifier, wood flour modified thereby, and preparation method of wood flour | |
| US20150151449A1 (en) | Adhesive materials and methods of forming lignocellulosic composites using such adhesive materials | |
| CN107542249B (en) | A kind of cork-rubber composite floor board | |
| CN1974151A (en) | Nanometer intercalated timber/montmorillonite composite material and its production process | |
| Ayrilmis et al. | Effect of wood-derived charcoal content on properties of wood plastic composites | |
| CN110587749B (en) | Complexing wood shavings, complexing shaving board and manufacturing method thereof | |
| CN111360965A (en) | Floor containing graphene coating and preparation method thereof | |
| CN108822440A (en) | A kind of flame-retardant wood-plastic plate and preparation method thereof | |
| WO2012040910A1 (en) | Wood modifier, preparation method thereof and method for modifying wood using the same | |
| CN111070824A (en) | Halogen-free flame-retardant wood-plastic co-extrusion composite material and preparation method thereof | |
| Khan et al. | Synthesis and characterization of carbon fibers and their application in wood composites | |
| CN107236204A (en) | A kind of preparation technology of PVC wood plastic composite decorating board | |
| CN109760172A (en) | A kind of preparation method of hydrophobic wood | |
| CN103073904B (en) | Preparation method of special wood powder for wood-plastic composite | |
| CN106674699A (en) | Polyethylene wood-plastic micro-foaming board and preparation method thereof | |
| Lima et al. | Influence of the Addition of Al2O3 Nanoparticles and the Duration of Pressing on the Physical Properties of OSB Panels | |
| CN108794820A (en) | A kind of compound flax floor of cork | |
| CN112358815A (en) | Preparation method of negative oxygen ion releasing material and application of negative oxygen ion releasing material in building material | |
| Mukbaniani et al. | COMPOSITES ON THE BASIS OF STRAW WITH SOME ORGANIC AND INORGANIC BINDERS. | |
| Liu | Improvements in the physical properties and decay resistance of bamboo materials via modification with boric acid and borax | |
| Liu et al. | Fungi resistance of organo‐montmorillonite modified lignocellulosic flour/polypropylene composites | |
| CN106625947A (en) | Composite modifying agent added with oxide graphene modified emulsion for fast growing wood | |
| CN106497119A (en) | A kind of flame-retardant wood-plastic composite material and preparation method thereof | |
| CN106239645A (en) | Use the method that anticorrosion composite urea formaldehyde resin produces full Eucalyptus solid wooden compound floor | |
| CN105906921A (en) | Halogen-free flame-retardant wood-plastic composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130522 |