CN113897071B - Preparation method of resin-impregnated wood powder filled wood-plastic composite material - Google Patents
Preparation method of resin-impregnated wood powder filled wood-plastic composite material Download PDFInfo
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- CN113897071B CN113897071B CN202111156724.1A CN202111156724A CN113897071B CN 113897071 B CN113897071 B CN 113897071B CN 202111156724 A CN202111156724 A CN 202111156724A CN 113897071 B CN113897071 B CN 113897071B
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- wood
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- plastic
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- 239000002023 wood Substances 0.000 title claims abstract description 206
- 239000000843 powder Substances 0.000 title claims abstract description 162
- 229920001587 Wood-plastic composite Polymers 0.000 title claims abstract description 30
- 239000011155 wood-plastic composite Substances 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 65
- 239000011347 resin Substances 0.000 claims abstract description 65
- 229920003023 plastic Polymers 0.000 claims abstract description 64
- 239000004033 plastic Substances 0.000 claims abstract description 64
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000002952 polymeric resin Substances 0.000 claims abstract description 7
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 14
- 239000005011 phenolic resin Substances 0.000 claims description 14
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 13
- 238000001125 extrusion Methods 0.000 claims description 13
- 229920001568 phenolic resin Polymers 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 238000007493 shaping process Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 125000005442 diisocyanate group Chemical group 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229920005672 polyolefin resin Polymers 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 12
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 235000013312 flour Nutrition 0.000 description 30
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 18
- 238000007598 dipping method Methods 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 14
- 238000005470 impregnation Methods 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 210000004027 cell Anatomy 0.000 description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 description 9
- 239000000839 emulsion Substances 0.000 description 9
- 239000006057 Non-nutritive feed additive Substances 0.000 description 8
- 239000001913 cellulose Substances 0.000 description 8
- 229920002678 cellulose Polymers 0.000 description 8
- 229920001903 high density polyethylene Polymers 0.000 description 8
- 239000004700 high-density polyethylene Substances 0.000 description 8
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 7
- 239000008116 calcium stearate Substances 0.000 description 7
- 235000013539 calcium stearate Nutrition 0.000 description 7
- 239000000945 filler Substances 0.000 description 7
- 235000021190 leftovers Nutrition 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 230000000007 visual effect Effects 0.000 description 5
- 229920002488 Hemicellulose Polymers 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000004584 weight gain Effects 0.000 description 4
- 235000019786 weight gain Nutrition 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 210000002421 cell wall Anatomy 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009408 flooring Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 239000012633 leachable Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 210000001724 microfibril Anatomy 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/0207—Pretreatment of wood before impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/15—Impregnating involving polymerisation including use of polymer-containing impregnating agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/15—Impregnating involving polymerisation including use of polymer-containing impregnating agents
- B27K3/153—Without in-situ polymerisation, condensation, or cross-linking reactions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K2200/00—Wooden materials to be treated
- B27K2200/15—Pretreated particles or fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K2240/00—Purpose of the treatment
- B27K2240/70—Hydrophobation treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Biochemistry (AREA)
- Dry Formation Of Fiberboard And The Like (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The application relates to a preparation method of a resin-impregnated wood powder filled wood-plastic composite material, and belongs to the technical field of wood-plastic materials. The preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps: a) Providing wood powder; b) Immersing wood powder in the dispersion liquid of the low molecular weight resin to obtain immersed wood powder; c) Mixing the impregnated wood powder with high polymer resin, and granulating to obtain modified wood-plastic master batch; d) Extruding the modified wood-plastic master batch by using an extruder to prepare the resin-impregnated modified wood powder filled wood-plastic composite material. According to the application, the wood powder is firstly subjected to plasticizing modification by using the low molecular weight resin to impregnate the wood powder, so that not only can the hydrophobicity of the wood powder be improved, but also the compatibility of the wood powder and the resin can be obviously improved, and the effect of uniform mixing under microcosmic condition can be achieved by treating the wood powder by a high-speed mixer, so that the mechanical property of the wood-plastic composite board in a humid environment is improved.
Description
Technical Field
The application relates to a preparation method of a resin-impregnated wood powder filled wood-plastic composite material, and belongs to the technical field of wood-plastic materials.
Background
The wood powder used for wood-plastic production is generally directly used as wood-plastic raw material for extrusion production after being dried and dehydrated. Since the compatibility of wood flour with plastics is not very good, the prior art generally requires mixing at high speed with a high speed mixer, then turning to low speed mixing, and then granulating; finally, extruding the wood-plastic master batch in an extruder with a die.
In order to enable the wood-plastic product to be more closely attached to wood, the filling proportion of wood powder is high and can reach 60% -70% at most. For example, the Chinese patent publication No. CN 103265768B discloses a method for producing wood-plastic floor. According to the method, 80-120 meshes of crushed, ground and dried wood powder with the water content less than or equal to 1% are selected, 10-15% of light calcium carbonate, 1.8-2.5% of stabilizer, 1.0-1.5% of modifier, 0.5-1.5% of coupling agent, 1.0-2.5% of lubricant, 2.5-3.5% of reinforcing agent, 1.5-2.0% of plastic processing aid, 0.5-1.0% of foaming agent and 0.8-2.0% of colorant are added into a high-low mixer to be fully mixed and reacted with waste plastic, and the required wood-plastic floor is obtained through an extruder, an extrusion die head, vacuum shaping, water cooling and automatic cutting. As described above, the wood flour is used in an amount of about 70%. Which also affects the quality of the wood-plastic panel to some extent.
Disclosure of Invention
The application aims to solve the technical problems, and provides a preparation method of a resin-impregnated wood powder filled wood-plastic composite material.
The method comprises the steps of firstly adopting resin to impregnate wood powder to modify the wood powder, then using the modified wood powder to blend with the resin to form raw materials, and finally forming the required plate or profile through an extruder, an extrusion die head, vacuum shaping and water cooling.
The technical scheme for solving the problems is as follows:
the preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps:
a) Providing wood powder;
b) Immersing the wood powder in a dispersion liquid of low molecular weight resin, taking out after immersing, and drying to obtain immersed wood powder;
c) And mixing the impregnated wood powder with a polymer resin in an amount of (1-5): 1, mixing and granulating to obtain modified wood-plastic master batch;
d) And carrying out melt extrusion on the modified wood-plastic master batch by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the resin-impregnated modified wood powder filled wood-plastic composite material.
Although the degree of mixing of wood flour with resin can be significantly improved by the masterbatch technique. But from a microscopic point of view this degree of mixing is far from sufficient. The microphotograph of the section of the plate shows that the resin cannot completely wrap the wood powder, only a small part of the wood powder is uniformly dispersed, and most of the wood powder has a agglomeration phenomenon; the problems of poor dimensional stability, reduced mechanical property and the like of the wood-plastic plate after being used for a period of time are caused, and even the phenomenon of environmental stress cracking can be caused.
In the above technical solution of the present application, the inventor proposes the solution because the inventor finds that the structure of the existing wood-plastic panel in the microscopic state is very uneven. In the prior art, wood powder and resin powder (such as PE) are uniformly mixed by a high-speed mixer, or a granulator is used for preparing wood-plastic master batches; and then extruded with a die using an extruder. This operation is often considered to be a macroscopic (visual) mixing of wood flour with resin flour, i.e. whether microscopic mixing is negligible. The inventors believe that the deterioration of the properties of wood-plastic panels is often based on the microstructure of the panel being destroyed, such as the wood flour component becoming wet or absorbing water. Because the prior art shows that wood powder is added into resin to produce wood-plastic boards, the physical properties of the boards are obviously changed along with the addition amount of the wood powder, when the addition amount of the wood powder is about 5%, the boards have little influence, and the water absorption is equivalent to that of the boards without the wood powder; when the wood powder addition amount reaches 20%, the water absorption of the plate is increased, and the compressive strength after weight increment is also reduced; when the addition amount of wood plastic exceeds 50%, the above problems are highlighted. The analysis of the problems in the prior art is simply classified as the influence of the addition amount of wood powder on the wood-plastic panel, and the fact that the excessive addition amount of wood powder can cause adverse effect on the wood-plastic panel is considered fully by the person skilled in the art when producing the wood-plastic panel is suggested. Thus, one of the technological developments in the wood-plastic panel industry is to replace wood flour with other powders, a typical technical representative being SPC flooring. SPC floors are boards formed by a large amount of filling PVC resin with stone powder such as calcium carbonate.
In analyzing the cause of the above problems, the present inventors have proposed their new theories. The inventors believe that the filling amount of wood powder naturally has a negative effect on the water absorption of the wood-plastic panel, but this negative effect is not unilaterally caused by the addition amount factor of wood powder, and it is important that the wood powder is not uniformly mixed with the resin. I.e. the applicant believes that macroscopic mixing is often still not in the microscopic state. Based on this, the applicant carried out high magnification observation under a microscope on the existing wood-plastic panel. It was found that the dispersive distribution of wood flour pellets was seen in the existing wood-plastic panels at a magnification of 10 times. The wood powder aggregate is particles formed by a large amount of wood powder which are clustered together, the particles are small, the small particles can be seen to be uniformly dispersed in the resin component under the visual angle, and under the magnification of 10 times, the wood powder and the resin component can be seen to have low mixing degree, namely, in the 10 times visual field, partial areas are not distributed with wood powder, partial areas are distributed with wood powder aggregate, the wood powder aggregate is unevenly distributed in the visual field, and linear connection is formed among partial wood powder aggregate, so that most wood powder aggregate forms an intermittent network structure. Under the magnification of 40 times, the enlarged structure of the wood powder aggregate can be seen, and the wood powder aggregate and the surrounding resin are not well fused, and a narrow cavity exists between the wood powder aggregate and the surrounding resin. At a magnification of 100 times, almost all the visual field is occupied by the aggregates of wood powder, and the internal enlarged structure of the aggregates of wood powder can be seen, and no resin is impregnated into the interior of wood powder. Based on the above, the inventors have proposed a hypothesis that if all wood powder particles are uniformly mixed with resin without agglomeration, and some degree of fusion is generated (i.e., no narrow void is generated, and at least part of the interior of the wood powder is immersed in the resin), the addition amount of the wood powder can be further increased and the physical properties of the wood-plastic panel, especially various mechanical properties under a humid environment, are not significantly reduced. Because the inventors believe that in this ideal case, the wood powder aggregates are eliminated, the network structure formed by the aggregates is more unable to be constituted, the periphery of each wood powder is covered with the resin, and the resin and the wood powder form a fusion; the inventor also believes that in this case, the wood flour in the board itself does not come into contact with moisture, i.e. the wood-plastic board does not undergo significant weight gain in wet or even in a water-soaked environment, the board dimensions do not change significantly, and the mechanical properties do not significantly decrease. However, the inventors have not been able to mix wood flour and resin powder to an ideal state by any operation when mixing wood flour and resin powder by a high-speed mixer.
Based on the above factors, the inventors have conceived a solution for modifying wood flour. That is, the wood powder is resinated, whereby the mixing degree of the wood powder and the resin is improved.
However, the prior art reports on wood flour treatment, mainly comprising pretreatment of wood flour, mainly mechanical crushing, ultrasonic crushing and chemical reagent treatment. Wherein the mechanical crushing comprises mechanical shearing and ball milling treatment, so that the size of the raw material is obviously reduced, the crystalline structure of cellulose is destroyed, and the ball milling treatment is more common and has optimal effect. After ball milling treatment, the surface area of the wood powder is increased, the crystal structure of cellulose is damaged to a certain extent, so that the three-dimensional network structure is loose, intermolecular hydrogen bonds in microfibrils and inter-microfibril crystal areas are broken, and the compatibility of the wood powder and resin powder is improved to a certain extent. The chemical reagent treatment mainly comprises soaking wood powder with sodium hydroxide or dilute sulfuric acid; the alkali liquor soaking can break the ester bonds connected between cellulose, hemicellulose and lignin in the plant cell wall. Whereas dilute sulfuric acid hydrolyzes part of the cellulose.
The inventors believe that simple pretreatment does not improve the uniformity of wood flour in the resin and improve compatibility with the resin. Further modification of wood flour is required.
The present application adopts the scheme of impregnating wood powder with low molecular weight resin to pretreat wood powder. Tests show that the resin with low molecular weight can penetrate into wood powder, and the effect is better especially under the condition of pressurized impregnation. In the above-described embodiment of the present application, wood flour is first immersed in a dispersion of a low molecular weight resin. The grain diameter of the wood powder is 100-1 mm, and the size of wood cells is 10-100 mu m; that is, one wood powder is generally composed of several tens to several hundreds of wood cells. The process of impregnating the wood powder with the low molecular weight resin dispersion is also the process of entering the wood powder with the resin; since wood flour is composed of a large number of wood cells, impregnation of resin is practically divided into two cases, the first is that resin enters into the gaps between wood cells, such as pits, and fills in; alternatively, the low molecular weight resin penetrates the cell wall and fills the cell interior; however, in either case, the wood powder is filled therein. The impregnation operation described above impregnates some of the wood cells, on the one hand, and low molecular weight resin, on the other hand, into the pores between the wood cells. That is, by the operation of step b), not only some of the free organic matters in the wood powder can be released, but also the low molecular weight resin can be filled in the wood powder. More importantly, these low molecular weight resins tend to react with hydroxyl groups that the cells have, thereby allowing the low molecular weight resins to be immobilized within the wood flour and not readily leachable in the presence of water as some of the contents of the wood cells themselves. That is, through the operation of step b), the cells are permanently swollen and the wood flour is modified. The modified wood powder is difficult to show water absorption property because the internal gaps are occupied; and the compatibility of the modified wood powder and the high polymer resin is obviously improved. For example, after wood powder impregnated with the low-molecular-weight aqueous phenolic resin emulsion is prepared into wood-plastic boards, the dimensional stability of the boards is improved, for example, after the traditional wood-plastic boards are subjected to a 24-hour water soaking test, the wood weight gain rate reaches more than 10%, and the wood weight gain rate is within 2% of that of the wood-plastic boards prepared from the wood powder impregnated with the low-molecular-weight aqueous phenolic resin emulsion. Secondly, the strength is improved, and after 5 freeze thawing cycles are carried out, the bending modulus of the traditional wood plastic plate is reduced by 40 percent; and the bending modulus of the wood-plastic plate made of wood powder impregnated with the low molecular weight aqueous phenolic resin emulsion is reduced by less than 10 percent. The applicant speculates that these losses in properties before unmodified are most likely due to hygroscopicity and poor interfacial compatibility between wood flour and resins. Therefore, after wood powder is modified, the weight gain rate and the bending modulus reduction amplitude of the wood can be effectively controlled under the same test conditions.
As a preferable mode of the above technical scheme, the wood flour is pretreated with acid or alkali before being impregnated with the low molecular weight resin, and then rinsed with water and dried.
The hydrophilic components in the wood powder can be separated out by treating with acid liquor or alkali liquor; these components are generally not free components and are difficult to remove without treatment with acid or lye. Then the wood powder is impregnated with the resin with low molecular weight, so that the impregnation effect of the resin with low molecular weight can be remarkably improved.
As a preferable mode of the technical scheme, 10-50 vol% of ethanol is added when the alkali liquor is adopted for pretreatment.
The alkali liquor soaking can break the ester bonds connected between cellulose, hemicellulose and lignin in the plant cell walls, so that the solubility of the cellulose in the ionic liquid can be improved. In addition to cellulose, hemicellulose and lignin, wood flour also contains free substances, which tend to have higher solubility in ethanol, and the addition of ethanol can further increase the dissolution rate and dissolution rate of these substances.
As a preferable mode of the technical scheme, the dispersion liquid with low molecular weight is water-soluble resin, the polymerization degree is 2-50, and the average molecular weight is not more than 6000.
In the technical scheme, the impregnating effect of the water-soluble resin on wood powder is obviously better than that of the fat-soluble resin; and the impregnation effect of the resin having a lower polymerization degree on wood flour is also better.
As a preferable mode of the above technical scheme, the solid content of the dispersion liquid of the low molecular weight resin is 20wt% to 45wt%.
In the technical scheme, the solid content is 20-45 wt% which indicates that the concentration of the resin dispersion liquid is low, and the rapid impregnation of the resin is facilitated.
Preferably, the low molecular weight dispersion is a water-soluble phenol resin or a melamine resin.
As a preferred option of the above technical scheme, step b) adopts vacuum pressurizing impregnation, placing wood powder in a vacuum impregnation tank to vacuumize, then injecting the dispersion liquid of the low molecular weight resin, taking out after impregnation, and drying to obtain impregnated wood powder.
As the optimization of the technical scheme, when vacuumizing, the vacuum degree is controlled to be-95 KPa to-10 KPa; the vacuumizing time is controlled to be 30-60 min.
Experiments show that the resin impregnation effect of wood powder can be obviously improved by the preliminary vacuum treatment.
Preferably, the above-mentioned technical solution is that, before step c), the impregnated wood flour is further post-treated with a diisocyanate. The NCO group of the diisocyanate can react with the bare OH group of the impregnated wood powder which is not coated by the low molecular weight resin, so that the hydrophobicity of the wood powder is further improved, the compatibility of the wood powder and the resin is improved, the mechanical strength and the hydrophobicity of the wood-plastic composite material are improved, and the service life of the wood plastic is prolonged.
Preferably, the polymer resin is a polyolefin resin.
As a further preferable aspect of the above-mentioned aspect, the polymer resin is HDPE.
In summary, the application has the following beneficial effects:
1. according to the application, the wood powder is firstly subjected to plasticizing modification by using the low molecular weight resin to impregnate the wood powder, so that not only can the hydrophobicity of the wood powder be improved, but also the compatibility of the wood powder and the resin can be obviously improved, and the effect of uniform mixing under microcosmic can be achieved by treating the wood powder by a high-speed mixer, so that the mechanical property of the wood-plastic composite board in a humid environment can be improved;
2. the application also pretreats the wood powder by acid liquor or alkali liquor before impregnating the wood powder with low molecular weight resin; the water absorption characteristic of wood powder is mainly caused by free hydrophilic substances and combined hydrophilic substances contained in the wood powder; free hydrophilic substances such as nutrient substances contained in wood flour, and bonded hydrophilic substances such as cellulose and hemicellulose; the hydrophilic substances can be removed under the acid-base condition, so that the impregnation effect of the low molecular weight resin can be improved, and the hydrophobicity of the modified wood powder can be improved;
3. the application also carries out post-treatment on the modified wood powder by using diisocyanate containing NCO groups, and the NCO groups of the modified wood powder after the post-treatment can react with bare OH groups to generate urethane or polyurethane with low molecular weight, which obviously improves the hydrophobicity of the wood powder.
Detailed Description
This detailed description is merely illustrative of the application and is not intended to be limiting. Any alterations, modifications, and variations which may be practiced by those of ordinary skill in the art after reading this disclosure are intended to be within the scope of the claims.
Example 1
The preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps:
a) Providing wood powder; making wood processing leftovers by using a superfine pulverizer, and passing through 80 meshes;
b) Immersing the wood powder in an aqueous phenolic resin emulsion, wherein the polymerization degree of the phenolic resin is 2-50, the average weight molecular weight is not more than 6000, and the solid content is about 30wt%; taking out after soaking, and drying to obtain impregnated wood powder;
c) Mixing and granulating the impregnated wood powder and HDPE in a mass ratio of 2:1 to obtain modified wood-plastic master batch;
d) And (2) melting and extruding the modified wood-plastic master batch, the processing aid calcium stearate (the dosage is 0.5 percent) and the filler superfine calcium carbonate (the dosage is 10.0 percent) by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the resin-impregnated modified wood powder filled wood-plastic composite plate.
Example 2
The preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps:
a) Providing wood powder; making wood processing leftovers by using a superfine pulverizer, and passing through 80 meshes;
b) Pretreating the wood powder by adopting alkali liquor, wherein in the pretreatment process, the alkali liquor contains alkaline substance caustic soda and 20vol% of ethanol; then, the wood flour is immersed in an aqueous phenolic resin emulsion, the polymerization degree of the phenolic resin is 2-50, the average molecular weight is not more than 6000, and the solid content is about 30wt%; the dipping in the step adopts vacuum pressurizing dipping, firstly placing wood powder in a vacuum dipping tank for vacuumizing, then injecting the aqueous phenolic resin emulsion, taking out after dipping, and drying to obtain dipping wood powder; when vacuumizing, controlling the vacuum degree at-65 KPa to-50 KPa; the vacuumizing time is controlled to be 30min;
c) Mixing and granulating the impregnated wood powder and HDPE in a mass ratio of 2:1 to obtain modified wood-plastic master batch;
d) And (2) melting and extruding the modified wood-plastic master batch, the processing aid calcium stearate (the dosage is 0.5 percent) and the filler superfine calcium carbonate (the dosage is 10.0 percent) by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the resin-impregnated modified wood powder filled wood-plastic composite plate.
Example 3
The preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps:
a) Providing wood powder; making wood processing leftovers by using a superfine pulverizer, and passing through 80 meshes; ball milling and sieving with 200 meshes;
b) Pretreating the wood powder by adopting alkali liquor, wherein in the pretreatment process, the alkali liquor contains alkaline substance caustic soda and 20vol% of ethanol; then, the wood flour is immersed in an aqueous phenolic resin emulsion, the polymerization degree of the phenolic resin is 2-50, the average molecular weight is not more than 6000, and the solid content is about 30wt%; the dipping in the step adopts vacuum pressurizing dipping, firstly placing wood powder in a vacuum dipping tank for vacuumizing, then injecting the aqueous phenolic resin emulsion, taking out after dipping, and drying to obtain dipping wood powder; when vacuumizing, controlling the vacuum degree at-65 KPa to-50 KPa; the vacuumizing time is controlled to be 30min; then mixing and stirring the impregnated wood powder and the polymeric MDI, and fully mixing to obtain modified wood powder;
c) Mixing and granulating the modified wood powder and HDPE in a mass ratio of 2:1 to obtain modified wood-plastic master batches;
d) And (2) melting and extruding the modified wood-plastic master batch, the processing aid calcium stearate (the dosage is 0.5 percent) and the filler superfine calcium carbonate (the dosage is 10.0 percent) by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the resin-impregnated modified wood powder filled wood-plastic composite plate.
Example 4
The preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps:
a) Providing wood powder; making wood processing leftovers by using a superfine pulverizer, and passing through 80 meshes;
b) Immersing the wood flour in a mixed liquid containing polyurethane prepolymer and diisocyanate monomer (MDI is adopted in the embodiment), wherein the solid content is about 35wt%; taking out after soaking, and drying to obtain impregnated wood powder;
c) Mixing and granulating the impregnated wood powder and HDPE in a mass ratio of 2:1 to obtain modified wood-plastic master batch;
d) And (2) melting and extruding the modified wood-plastic master batch, the processing aid calcium stearate (the dosage is 0.5 percent) and the filler superfine calcium carbonate (the dosage is 10.0 percent) by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the resin-impregnated modified wood powder filled wood-plastic composite plate.
Example 5
The preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps:
a) Providing wood powder; making wood processing leftovers by using a superfine pulverizer, and passing through 80 meshes; ball milling and sieving with 200 mesh sieve
b) Pretreating the wood powder by adopting alkali liquor, wherein in the pretreatment process, the alkali liquor contains alkaline substance caustic soda and 20vol% of ethanol; the wood flour was then immersed in a mixed liquid containing polyurethane prepolymer and diisocyanate monomer (MDI is used in this example) with a solids content of about 35wt%; taking out after soaking, and drying to obtain impregnated wood powder; the dipping in the step adopts vacuum pressurizing dipping, firstly placing wood powder in a vacuum dipping tank for vacuumizing, then injecting the aqueous phenolic resin emulsion, taking out after dipping, and drying to obtain dipping wood powder;
c) Mixing and granulating the impregnated wood powder and HDPE in a mass ratio of 2:1 to obtain modified wood-plastic master batch;
d) And (2) melting and extruding the modified wood-plastic master batch, the processing aid calcium stearate (the dosage is 0.5 percent) and the filler superfine calcium carbonate (the dosage is 10.0 percent) by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the resin-impregnated modified wood powder filled wood-plastic composite plate.
Comparative example 1
The preparation method of the wood-plastic composite board comprises the following steps:
a) Providing wood powder; making wood processing leftovers by using a superfine pulverizer, and passing through 80 meshes;
b) Mixing and granulating the wood powder and HDPE in a mass ratio of 2:1 to obtain wood-plastic master batches;
d) And (3) melting and extruding the wood-plastic master batch, the processing aid calcium stearate (the dosage is 0.5 percent) and the filler superfine calcium carbonate (the dosage is 10.0 percent) by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the wood-plastic composite plate.
Comparative example 2
The preparation method of the wood-plastic composite board comprises the following steps:
a) Providing wood powder; making wood processing leftovers by using a superfine pulverizer, and passing through 80 meshes; ball milling and sieving with 200 meshes;
b) Mixing and granulating the wood powder and HDPE in a mass ratio of 2:1 to obtain wood-plastic master batches;
d) And (3) melting and extruding the wood-plastic master batch, the processing aid calcium stearate (the dosage is 0.5 percent) and the filler superfine calcium carbonate (the dosage is 10.0 percent) by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the wood-plastic composite plate.
The boards of examples 1-5 and comparative examples 1-2 were tested for water absorption after 24h of water immersion test according to the method of GB/T17657-2013, and the flexural modulus of the wood-plastic boards after 3 freeze thawing cycles according to the method of GB/T24508-2009 wood-plastic floor 6.5.10 were tested, the results are shown in the following table:
Claims (3)
1. the preparation method of the resin-impregnated modified wood powder filled wood-plastic composite material comprises the following steps:
a) Providing wood powder;
b) Pretreating the wood powder by adopting alkali liquor, wherein in the pretreatment process, 20vol% of ethanol is added into the alkali liquor; then, immersing wood powder in the dispersion liquid of the low molecular weight resin, adopting vacuum pressurizing for immersing, firstly placing the wood powder in a vacuum immersing tank for vacuumizing, then injecting the dispersion liquid of the low molecular weight resin, taking out after immersing, and drying to obtain the immersed wood powder; then, carrying out post-treatment on the impregnated wood powder by diisocyanate to obtain modified wood powder;
c) Mixing the modified wood powder with high polymer resin according to a ratio of 2:1, mixing and granulating to obtain modified wood-plastic master batch;
d) Melting and extruding the modified wood-plastic master batch by using an extruder loaded with a wood-plastic extrusion die to prepare a plate blank, and cooling and shaping the plate blank to prepare the resin-impregnated modified wood powder filled wood-plastic composite material;
the dispersion liquid of the low molecular weight resin is water-soluble resin, the polymerization degree is 2-50, and the average molecular weight is not more than 6000;
the dispersion of the low molecular weight resin has a solids content of 30wt%;
the dispersion liquid of the low molecular weight resin is water soluble phenolic resin.
2. The method for preparing the resin-impregnated wood powder filled wood-plastic composite according to claim 1, wherein the method comprises the following steps: when vacuumizing, controlling the vacuum degree at-95 KPa to-10 KPa; the vacuumizing time is controlled to be 30-60 min.
3. The method for preparing the resin-impregnated wood powder filled wood-plastic composite according to claim 1, wherein the method comprises the following steps: the polymer resin is polyolefin resin.
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