CN103483838A - Preprocessing method of wood powder - Google Patents

Preprocessing method of wood powder Download PDF

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CN103483838A
CN103483838A CN201310364967.3A CN201310364967A CN103483838A CN 103483838 A CN103483838 A CN 103483838A CN 201310364967 A CN201310364967 A CN 201310364967A CN 103483838 A CN103483838 A CN 103483838A
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wood powder
silicone oil
low viscosity
powder
particularly preferably
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CN103483838B (en
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薛杨
张冬海
刘海弟
吴镇江
陈运法
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Institute of Process Engineering of CAS
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00Compositions of lignin-containing materials
    • C08L97/02Lignocellulosic material, e.g. wood, straw or bagasse
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27NMANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
    • B27N1/00Pretreatment of moulding material

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Forests & Forestry (AREA)
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  • Manufacturing & Machinery (AREA)
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  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Dry Formation Of Fiberboard And The Like (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention relates to a preprocessing method of wood powder. According to the preprocessing method, a mixture of low-viscosity silicone oil and active silicone oil is introduced into a three-phase circulating fluidized bed filled with the wood powder so as to modify the wood powder. The wood powder prepared by the preprocessing method has excellent hydrophobicity and damping resistance, and a wood plastic material prepared from the wood powder has excellent properties; compared with the prior art, the preprocessing method further has the advantages of circulation, environment friendliness, high efficiency, simple process, convenience in industrialization and the like.

Description

A kind of pretreatment process of wood powder
Technical field
The present invention relates to wood processing field, particularly, the present invention relates to a kind of pretreatment process of wood powder.
Background technology
Wood plastic composite due to its premium properties that has timber and plastics concurrently with and environmentally friendly and characteristics recoverable be widely used in every field, the wood industry of moulding has obtained developing rapidly.Because there is a large amount of hydroxyls in the lumber fibre surface, so timber has very strong polarity, and the easy moisture absorption, and most of resin is all nonpolar or polarity is less, therefore both compound tense consistencies are bad, there is obvious phase interface, thereby cause the mechanical property of wood plastic composite not good.And a large amount of hydroxyls forms intermolecular hydrogen bonding on the lumber fibre surface, make timber be not easy to disperse in the non-polar polymer matrix, in the preparation process of matrix material, lumber fibre is tending towards mutual gathering, form fibrous mass, bundle, the probability increase that causes stress concentration and produce defect, also cause the decline of material mechanical performance.Therefore, improve the bonding interface of wood plastic composite, interfacial adhesion effect and the dispersiveness of wood materials in resin matrix of resolving wood materials and resin are to improve the key issue of wood plastic composite performance, and this is also the Focal point and difficult point of studying at present.
At present, wood powder pretreatment process commonly used mainly comprises physically modified and chemical modification.Physically modified comprises thermal treatment, alkaline purification, radiotreatment, discharge process, gas explosion processing etc.; chemical process is mainly to carry out modification on the xylon surface by polar functional group is carried out to acidylate, etherificate, graft copolymerization etc.; make it generate nonpolar chemical functional group and there is mobility; make wood surface polarity similar to resin surface; to reduce the repellence between resin matrix and wooden material surface, reach the purpose that improves interfacial adhesion.From effect, chemical modification is better than physically modified, but chemical modification is often than physically modified complexity.
CN1876724A discloses agricultural stalk base wood plastic composite materials and combined technical method.Raw material comprises that plasticizing agricultural stalk powder particles material, thermoplastics, lubricant comprise that dimethyl silicone oil, stearic acid and polyester are cured, expanding material is vinylformic acid-alternate styrene-maleic anhydride copolymer, softening agent is dioctyl phthalate (DOP), and fire retardant is red iron oxide.Its preparation method is by the above-mentioned raw materials mixing and stirring, sends into forming machine and makes section bar.But the method adopts the conventional hybrid mode, auxiliary agent mixes even not with stalk powder and plastics, can affect the interfacial adhesion of Wood-plastic material, and gas-liquid-solid three-phase fluid bed wood powder and the silicone oil of making that the present invention adopts is fully mixed and modified, and can realizes the continuity of operation.
Therefore, develop a kind of capable of circulation, environment-friendly high-efficiency, technique simple, be convenient to industrialization, and the wood powder method of modifying that the modified wood powder prepared has excellent physicals and a mechanical property is the technical barrier in affiliated field.
Summary of the invention
For the deficiencies in the prior art, one of purpose of the present invention is to provide a kind of pretreatment process of wood powder, and it adopts silicone oil to carry out modification to wood powder, compared with prior art, have capable of circulation, environment-friendly high-efficiency, technique simple, be convenient to the advantage such as industrialization.
The pretreatment process of described wood powder comprises: silicone oil with low viscosity, active silicone oil and wood powder are fully mixed, obtain modified wood powder, wherein, the viscosity that described silicone oil with low viscosity is 25 ℃ is 0.5-40mPa.s.
Preferably, described being blended in fluidized-bed carried out; Preferably, described fluidized-bed is gas-liquid-solid three-phase fluid bed.
Preferably, the pretreatment process of described wood powder comprises: by after the mixture preheating of silicone oil with low viscosity and active silicone oil, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is introduced gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into warm air at the bottom of tower, obtain modified wood powder, wherein, the viscosity that described silicone oil with low viscosity is 25 ℃ is 0.5-40mPa.s.
Preferably, the combination that described wood powder is any a kind or at least 2 kinds in trees powder, sawdust powder, Wood waste powder, shell powder or farm crop powder.
In this article, described active silicone oil refers to the silicone oil with reactive behavior.
Preferably, the particle diameter of described wood powder is 10~150 orders, and more preferably 15~120 orders, be particularly preferably 20~100 orders; If the particle diameter of wood powder is greater than described size, need in advance it to be pulverized.
Preferably, described wood powder water content<3wt%, such as 2.9wt%, 2.8wt%, 2.5wt%, 2wt%, 1.8wt%, 1.5wt%, 1.2wt%, 1wt%, 0.8wt%, 0.5wt%, 0.2wt%, 0.1wt% or 0.05wt% etc.; If its water content >=3wt%, so just need to it is carried out to drying before silicone oil with low viscosity and active silicone oil mix; Preferably, described drying temperature is 50~150 ℃, more preferably 70~130 ℃, is particularly preferably 80~120 ℃; Preferably, be 0.5h at least described time of drying, and more preferably 0.8~6h, be particularly preferably 1~4h; Preferably, described drying is carried out in baking oven.
Preferably, described silicone oil with low viscosity is polydimethylsiloxane, cyclopentasiloxane, cyclohexasiloxane, ring decamethylcyclopentaandoxane or the combination that encircles any a kind or at least 2 kinds in ten diformazan basic ring six siloxanes.
Preferably, described silicone oil with low viscosity is the low viscosity volatile silicone oils; Preferably, the viscosity of 25 ℃ of described low viscosity volatile silicone oils is 1-27mPa.s; Preferably, the boiling point of described low viscosity volatile silicone oils is 200-300 ℃, particularly preferably 220-270 ℃.
The example of described silicone oil with low viscosity is as DOW CORNING
Figure BDA0000369443140000031
pMX-0245,
Figure BDA0000369443140000032
pMX-0246,
Figure BDA0000369443140000033
pMX-0345, 2945, the AK10 of the KF-96L of SHIN-ETSU HANTOTAI, KF-995, watt gram, the GE-9981 of Toshiba etc.
Preferably, described active silicone oil is amido silicon oil and/or hydroxy silicon oil; Preferably, the amino content of described amido silicon oil is 0.2-1.65wt%, particularly preferably 0.37-1.5wt%; Preferably, the hydroxy radical content of described hydroxy silicon oil is 2-16wt%, particularly preferably 2.5-7wt%.
Preferably, described activated silica oil viscosity is 38-120mPa.s, further preferred 45-100mPa.s, particularly preferably 50-75mPa.s.
The amido silicon oil specific product is as DOW CORNING
Figure BDA0000369443140000035
oFX-8040, oFX-8630,
Figure BDA0000369443140000041
oFX-8803,
Figure BDA0000369443140000042
oFX-8813,
Figure BDA0000369443140000043
oFX-8822 etc.; The hydroxy silicon oil specific product is as DOW CORNING
Figure BDA0000369443140000044
pMX-0156,
Figure BDA0000369443140000045
pMX-0930 etc.
Preferably, the volume ratio of described silicone oil with low viscosity and active silicone oil is 0.2:1-6:1, particularly preferably 0.5:1-4.5:1.
Preferably, the total amount of described silicone oil with low viscosity and active silicone oil and the mass ratio of wood powder are 0.001:1-0.01:1, particularly preferably 0.003:1-0.006:1.
Gas, liquid, solid three-phase in described gas-liquid-solid three-phase circulating fluidized bed is respectively air, silicon oil mixture and wood powder.
Preferably, in described gas-liquid-solid three-phase circulating fluidized bed, gas flow rate is 0.0100-2.1300m/s, further preferred 0.0250-1.8500m/s, particularly preferably 0.0410-1.2000m/s.
Preferably, the temperature after the mixture preheating of described silicone oil with low viscosity and active silicone oil is 80~150 ℃, more preferably 90~130 ℃, and 100-120 ℃ particularly preferably.
Preferably, the temperature of described warm air is 50~110 ℃, more preferably 55~100 ℃, and 60-95 ℃ particularly preferably.
Preferably, the described fluidization treatment time is 10-95 minute, particularly preferably 15-50 minute.
Preferably, modified wood powder is mixed with plastic powder and extrude, granulation, finally the compacting or injection moulding; Preferably, described mixing time is 4min at least, and more preferably 5~25min, be particularly preferably 5~15min; Preferably, described being blended in high-speed mixer carried out; The described employing twin screw extruder of extruding; Preferably, the temperature of screw rod is 140 ℃-220 ℃, and screw speed is 12-250r/min, and rate of feeding is 10-57r/min, and pelletizing speed is 60-160r/min.
Preferably, the pretreatment process of described wood powder comprises the following steps:
(1) wood powder is pulverized and sieved, particle diameter is 10~150 orders, then by wood powder 50~150 ℃ of dryings at least 0.5h to water content<3wt%;
(2) after the mixture of silicone oil with low viscosity and active silicone oil is preheated to 80~150 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, (1) wood powder described in is introduced gas-liquid-solid three-phase fluid bed from bottom, pass into the warm air that temperature is 50~110 ℃ at the bottom of tower, fluidisation 10-95 minute, obtain modified wood powder; Wherein, the volume ratio of silicone oil with low viscosity and active silicone oil is 0.2:1-6:1, and the weight ratio of silicon oil mixture and wood powder is 0.001:1-0.01:1, and the control gas flow rate is 0.0100-2.1300m/s.
Two of purpose of the present invention is to provide a kind of modified wood powder, by the method for the invention, prepared by described modified wood powder.
The wood powder prepared according to the method for the invention, contact angle is greater than 100 ° after tested, the 300h rate of moisture absorption is less than 2%, illustrate after its modification and possess good hydrophobicity and the anti-performance of getting damp, compared with prior art, the present invention also have capable of circulation, environment-friendly high-efficiency, technique simple, be convenient to the advantage such as industrialization.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
In following each embodiment, adopt following methods to carry out performance test to modified wood powder:
Measure the wood powder hydrophobic performance after processing with the German Kruss DSA100 of company static contact angle determinator: wood powder is suppressed on powder compressing machine in flakes, pressure is 20MPa, pressurize 5min, the thin rounded flakes of formation even thickness, measure the contact angle of water droplet on the wood powder compressing tablet.
The wood powder prepared according to the method for the invention, obtain wood plastic composite with the plastics powder after twin-screw extrusion, repressed or the injection moulding of granulation, its flexural strength is measured according to GB/T9341-2008, the Young's modulus test is measured according to GB/T17657-1999, the tensile property test is measured according to GB/T1040-92, and shock strength is measured according to GB/T1043.1-2008, and hardness test is measured according to GB9342-88.
Hygroscopic property test: the wood plastic composite test specimen is put on climatic chamber inner jar dividing plate, pressed humidity exposure time 300h and take out the title quality, according to calculating rate of moisture absorption of poor quality.
Embodiment 1
At first with pulverizing mill, wood powder is crushed to 100 orders, then wood powder is put into to 110 ℃ of dry 1h(water content<3wt% of baking oven), then be cooled to 40 ℃.By silicone oil with low viscosity
Figure BDA0000369443140000061
pMX-0244 and amido silicon oil
Figure BDA0000369443140000062
oFX-8040 mixes according to 0.2:1 (V/V), after being preheated to 100 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.001:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 60 ℃ at the bottom of tower, the control gas flow rate is 0.0100m/s, and the treatment time is 15 minutes, obtains modified wood powder.Modified wood powder is mixed to 5min with the PE powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 220 ℃, and screw speed is 25r/min, and rate of feeding is 57r/min, and pelletizing speed is 160r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 103.05 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 42.8MPa, and shock strength is 6.2kJ/m 2, flexural strength is 51.7MPa, Young's modulus 1954.45MPa, and hardness is 43.1, rate of moisture absorption is 1.5%.
Embodiment 2
At first with pulverizing mill, wood powder is crushed to 40 orders, then wood powder is put into to 80 ℃ of dry 4h(water content<3wt% of baking oven), then be cooled to 30 ℃.By silicone oil with low viscosity
Figure BDA0000369443140000063
pMX-0246 and amido silicon oil
Figure BDA0000369443140000064
oFX-8630 mixes according to 6:1 (V/V), after being preheated to 120 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.01:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 70 ℃ at the bottom of tower, the control gas flow rate is 1.2000m/s, and the treatment time is 30 minutes, obtains modified wood powder.Modified wood powder is mixed to 15min with the PP powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 200 ℃, and screw speed is 12r/min, and rate of feeding is 10r/min, and pelletizing speed is 60r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 134.73 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 53.3MPa, and shock strength is 8.4kJ/m 2, flexural strength is 74.9MPa, Young's modulus 2107.36MPa, and hardness is 33.5, rate of moisture absorption is 0.4%.
Embodiment 3
At first with pulverizing mill, wood powder is crushed to 80 orders, then wood powder is put into to 90 ℃ of dry 2h(water content<3wt% of baking oven), then be cooled to 40 ℃.By silicone oil with low viscosity pMX-0245 and hydroxy silicon oil
Figure BDA0000369443140000072
pMX-0156 mixes according to 0.2:1 (V/V), after being preheated to 110 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.003:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 80 ℃ at the bottom of tower, the control gas flow rate is 2.1300m/s, and the treatment time is 45 minutes, obtains modified wood powder.Modified wood powder is mixed to 10min with the PVC powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 140 ℃, and screw speed is 20r/min, and rate of feeding is 30r/min, and pelletizing speed is 80r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 110.92 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 62.4MPa, and shock strength is 9.7kJ/m 2, flexural strength is 73.2MPa, Young's modulus 2454.38MPa, and hardness is 51.8, rate of moisture absorption is 1.2%.
Embodiment 4
At first with pulverizing mill, wood powder is crushed to 60 orders, then wood powder is put into to 100 ℃ of dry 1.5h(water content<3wt% of baking oven), then be cooled to 30 ℃.By silicone oil with low viscosity
Figure BDA0000369443140000073
pMX-0344 and hydroxy silicon oil
Figure BDA0000369443140000074
pMX-0930 mixes according to 3:1 (V/V), after being preheated to 105 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.006:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 90 ℃ at the bottom of tower, the control gas flow rate is 0.0410m/s, and the treatment time is 25 minutes, obtains modified wood powder.Modified wood powder is mixed to 7min with the PS powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 190 ℃, and screw speed is 60r/min, and rate of feeding is 57r/min, and pelletizing speed is 110r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 113.06 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 45.1MPa, and shock strength is 5.7kJ/m 2, flexural strength is 59.3MPa, Young's modulus 2954.38MPa, and hardness is 39.2, rate of moisture absorption is 1.0%.
Embodiment 5
At first with pulverizing mill, wood powder is crushed to 90 orders, then wood powder is put into to 105 ℃ of dry 2h(water content<3wt% of baking oven), then be cooled to 40 ℃.By silicone oil with low viscosity
Figure BDA0000369443140000081
pMX-0345(217) and amido silicon oil
Figure BDA0000369443140000082
oFX-8803 is according to 1.7:1 (V/V), respectively from the bottom of tower and the tower side introduce, with wood powder, according to weight ratio 0.005:1, introduce gas-liquid-solid three-phase fluid bedly, the control gas flow rate is 1.8500m/s, the treatment time is 50 minutes, obtains modified wood powder.Modified wood powder is mixed to 13min with the PS powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 180 ℃, and screw speed is 40r/min, and rate of feeding is 35r/min, and pelletizing speed is 70r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 129.40 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 48.8MPa, and shock strength is 7.1kJ/m 2, flexural strength is 65.7MPa, Young's modulus 1762.14MPa, and hardness is 53.6, rate of moisture absorption is 0.7%.
Embodiment 6
At first with pulverizing mill, wood powder is crushed to 50 orders, then wood powder is put into to 85 ℃ of dry 3h(water content<3wt% of baking oven), then be cooled to 30 ℃.By silicone oil with low viscosity KF-96L and amido silicon oil
Figure BDA0000369443140000083
oFX-8813 mixes according to 0.5:1 (V/V), after being preheated to 115 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.004:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 95 ℃ at the bottom of tower, the control gas flow rate is 0.0250m/s, and the treatment time is 40 minutes, obtains modified wood powder.Modified wood powder is mixed to 15min with the ABS powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 210 ℃, and screw speed is 12-250r/min, rate of feeding is 10-57r/min, and pelletizing speed is 60-160r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 106.10 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 67.7MPa, and shock strength is 12.4kJ/m 2, flexural strength is 98.5MPa, Young's modulus 3325.11MPa, and hardness is 54.8, rate of moisture absorption is 1.1%.
Embodiment 7
At first with pulverizing mill, wood powder is crushed to 70 orders, then wood powder is put into to 95 ℃ of dry 2.5h(water content<3wt% of baking oven), then be cooled to 40 ℃.By silicone oil with low viscosity
Figure BDA0000369443140000091
2945(200) and amido silicon oil
Figure BDA0000369443140000092
oFX-8822 mixes according to 4.5:1 (V/V), after being preheated to 107 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.007:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 85 ℃ at the bottom of tower, the control gas flow rate is 0.1300m/s, and the treatment time is 35 minutes, obtains modified wood powder.Modified wood powder is mixed to 8min with the PET powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 210 ℃, and screw speed is 50r/min, and rate of feeding is 27r/min, and pelletizing speed is 90r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 115.56 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 53.6MPa, and shock strength is 8.2kJ/m 2, flexural strength is 65.3MPa, Young's modulus 2497.12MPa, and hardness is 45.9, rate of moisture absorption is 0.9%.
Embodiment 8
At first with pulverizing mill, wood powder is crushed to 10 orders, then wood powder is put into to 150 ℃ of dry 0.5h(water content<3wt% of baking oven), then be cooled to 40 ℃.By silicone oil with low viscosity
Figure BDA0000369443140000101
2945(200) and amido silicon oil
Figure BDA0000369443140000102
oFX-8822 mixes according to 0.5:1 (V/V), after being preheated to 80 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.007:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 50 ℃ at the bottom of tower, the control gas flow rate is 0.0200m/s, and the treatment time is 75 minutes, obtains modified wood powder.Modified wood powder is mixed to 4min with the PET powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 200 ℃, and screw speed is 15r/min, and rate of feeding is 12r/min, and pelletizing speed is 130r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 102.16 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 49.1MPa, and shock strength is 7.5kJ/m 2, flexural strength is 60.9MPa, Young's modulus 2318.63MPa, and hardness is 37.2, rate of moisture absorption is 1.6%.
Embodiment 9
At first with pulverizing mill, wood powder is crushed to 150 orders, then wood powder is put into to 50 ℃ of dry 10h(water content<3wt% of baking oven), then be cooled to 40 ℃.By silicone oil with low viscosity
Figure BDA0000369443140000103
2945(200) and amido silicon oil oFX-8822 mixes according to 5:1 (V/V), after being preheated to 150 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is according to silicon oil mixture: wood powder weight ratio 0.002:1 introduces gas-liquid-solid three-phase fluid bed from bottom, carry out fluidisation from passing into the warm air that temperature is 110 ℃ at the bottom of tower, the control gas flow rate is 2.0000m/s, and the treatment time is 25 minutes, obtains modified wood powder.Modified wood powder is mixed to 10min with the PET powder in high-speed mixer, then batch mixing is reacted and extrudes in twin screw extruder, the temperature that screw rod is set is 180 ℃, and screw speed is 180r/min, and rate of feeding is 45r/min, and pelletizing speed is 70r/min; The composite cools down granulation of extruding is by compacting or injection moulding.
In flakes, measuring the contact angle of water droplet on the wood powder compressing tablet is 100.43 ° in the modified wood powder compacting, and the tensile strength of the wood plastic composite obtained is 45.2MPa, and shock strength is 6.8kJ/m 2, flexural strength is 54.7MPa, Young's modulus 2293.05MPa, and hardness is 38.6, rate of moisture absorption is 1.9%.
Should be noted that and understand, in the situation that do not break away from the desired the spirit and scope of the present invention of accompanying claim, can make to the present invention of foregoing detailed description various modifications and improvement.Therefore, the scope of claimed technical scheme is not subject to the restriction of given any specific exemplary teachings.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.The person of ordinary skill in the field should understand, any improvement in the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., within all dropping on protection scope of the present invention and open scope.

Claims (10)

1. the pretreatment process of a wood powder, comprising: silicone oil with low viscosity, active silicone oil and wood powder are fully mixed, obtain modified wood powder, wherein, the viscosity that described silicone oil with low viscosity is 25 ℃ is 0.5-40mPa.s.
2. the method for claim 1, it is characterized in that, the pretreatment process of described wood powder comprises: by after the mixture preheating of silicone oil with low viscosity and active silicone oil, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, wood powder is introduced gas-liquid-solid three-phase fluid bed from bottom, from passing into warm air at the bottom of tower, carry out fluidisation, obtains modified wood powder, wherein, the viscosity of 25 ℃ of described silicone oil with low viscosity is 0.5-40mPa.s.
3. method as claimed in claim 1 or 2, is characterized in that, the combination that described wood powder is any a kind or at least 2 kinds in trees powder, sawdust powder, Wood waste powder, shell powder or farm crop powder;
Preferably, the particle diameter of described wood powder is 10~150 orders, and more preferably 15~120 orders, be particularly preferably 20~100 orders;
Preferably, described wood powder water content<3wt%;
Preferably, if described wood powder water content >=3wt% carries out drying to it; Preferably, described drying temperature is 50~150 ℃, more preferably 70~130 ℃, is particularly preferably 80~120 ℃; Preferably, be 0.5h at least described time of drying, and more preferably 0.8~6h, be particularly preferably 1~4h; Preferably, described drying is carried out in baking oven.
4. as the described method of claim 1-3 any one, it is characterized in that, described silicone oil with low viscosity is polydimethylsiloxane, cyclopentasiloxane, cyclohexasiloxane, ring decamethylcyclopentaandoxane or the combination that encircles any a kind or at least 2 kinds in ten diformazan basic ring six siloxanes;
Preferably, described silicone oil with low viscosity is the low viscosity volatile silicone oils; Preferably, the viscosity of 25 ℃ of described low viscosity volatile silicone oils is 1-27mPa.s; Preferably, the boiling point of described low viscosity volatile silicone oils is 200-300 ℃, particularly preferably 220-270 ℃.
5. as the described method of claim 1-4 any one, it is characterized in that, described active silicone oil is amido silicon oil and/or hydroxy silicon oil; Preferably, the amino content of described amido silicon oil is 0.2-1.65wt%, particularly preferably 0.37-1.5wt%; Preferably, the hydroxy radical content of described hydroxy silicon oil is 2-16wt%, particularly preferably 2.5-7wt%;
Preferably, described activated silica oil viscosity is 38-120mPa.s, further preferred 45-100mPa.s, particularly preferably 50-75mPa.s.
6. as the described method of claim 1-5 any one, it is characterized in that, the volume ratio of described silicone oil with low viscosity and active silicone oil is 0.2:1-6:1, particularly preferably 0.5:1-4.5:1;
Preferably, the total amount of described silicone oil with low viscosity and active silicone oil and the mass ratio of wood powder are 0.001:1-0.01:1, particularly preferably 0.003:1-0.006:1.
7. as the described method of claim 2-6 any one, it is characterized in that, in described gas-liquid-solid three-phase circulating fluidized bed, gas flow rate is 0.0100-2.1300m/s, further preferred 0.0250-1.8500m/s, particularly preferably 0.0410-1.2000m/s;
Preferably, the temperature after the mixture preheating of described silicone oil with low viscosity and active silicone oil is 80~150 ℃, more preferably 90~130 ℃, and 100-120 ℃ particularly preferably;
Preferably, the temperature of described warm air is 50~110 ℃, more preferably 55~100 ℃, and 60-95 ℃ particularly preferably;
Preferably, the described fluidization treatment time is 10-95 minute, particularly preferably 15-50 minute.
8. as the described method of claim 1-7 any one, it is characterized in that, the pretreatment process of described wood powder comprises the following steps:
(1) wood powder is pulverized and sieved, particle diameter is 10~150 orders, then by wood powder 50~150 ℃ of dryings at least 0.5h to water content<3wt%;
(2) after the mixture of silicone oil with low viscosity and active silicone oil is preheated to 80~150 ℃, respectively from the bottom of tower and the tower side introduce gas-liquid-solid three-phase fluid bed, (1) wood powder described in is introduced gas-liquid-solid three-phase fluid bed from bottom, pass into the warm air that temperature is 50~110 ℃ at the bottom of tower, fluidisation 10-95 minute, obtain modified wood powder; Wherein, the volume ratio of silicone oil with low viscosity and active silicone oil is 0.2:1-6:1, and the weight ratio of silicon oil mixture and wood powder is 0.001:1-0.01:1, and the control gas flow rate is 0.0100-2.1300m/s.
9. as the described method of claim 1-8 any one, it is characterized in that, modified wood powder is mixed with plastic powder and extrude, granulation, finally the compacting or injection moulding; Preferably, described mixing time is 4min at least, and more preferably 5~25min, be particularly preferably 5~15min; Preferably, described being blended in high-speed mixer carried out; The described employing twin screw extruder of extruding; Preferably, the temperature of screw rod is 140 ℃-220 ℃, and screw speed is 12-250r/min, and rate of feeding is 10-57r/min, and pelletizing speed is 60-160r/min.
10. a modified wood powder, is characterized in that, described modified wood powder is by the described method preparation of claim 1-9 any one.
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