CN111015858A - Novel mildew-proof recombined bamboo based on pyrolysis oil phenolic resin and preparation method thereof - Google Patents
Novel mildew-proof recombined bamboo based on pyrolysis oil phenolic resin and preparation method thereof Download PDFInfo
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- CN111015858A CN111015858A CN201911166090.0A CN201911166090A CN111015858A CN 111015858 A CN111015858 A CN 111015858A CN 201911166090 A CN201911166090 A CN 201911166090A CN 111015858 A CN111015858 A CN 111015858A
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Images
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- 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
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- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
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Abstract
The application belongs to the technical field of bamboo processing and forest industry. The recombined bamboo is easy to mildew under the damp and hot environmental condition, so that the use value and the appearance of the recombined bamboo are influenced, and the large-scale popularization and application of the recombined bamboo are further limited. The application provides a novel mildew-proof recombined bamboo based on pyrolysis oil phenolic resin, which sequentially comprises a first surface layer, a first adhesive layer, a core layer, a second adhesive layer and a second surface layer, wherein the first surface layer is connected with the core layer through the first adhesive layer, and the second surface layer is connected with the core layer through the second adhesive layer; the first adhesive layer is a pyrolytic oil phenolic resin adhesive layer, and the second adhesive layer is a pyrolytic oil phenolic resin adhesive layer. The method adopts thermal cracking refining and resin synthesis technologies, fully utilizes the residues of bamboo processing enterprises, adds the residues into the production process of the recombined bamboo, and endows the product with certain mildew resistance and antibacterial property, thereby reducing the production cost of the recombined bamboo and improving the product performance.
Description
Technical Field
The application belongs to the technical field of bamboo processing and forest industry, and particularly relates to novel mildew-proof recombined bamboo based on pyrolysis oil phenolic resin and a preparation method thereof.
Background
The recombined bamboo is a bamboo recombined material which is prepared by mechanically fluffing bamboo into fibrous bamboo bundle filaments, drying, carbonizing, dipping in glue, drying, laying in a mould along the grain and performing high-temperature high-pressure thermal curing. Specifically, bamboo is split and defibered into loose fiber bamboo bundle fibers, then the loose fiber bamboo bundle fibers are impregnated with chemical polymers such as low-molecular-weight resin, micro-cracks formed through defibering are purposefully introduced into different tissues such as cell cavities, walls, grain holes and the like, and after the micro-cracks are assembled along grains, the fiber bamboo bundles are pressed into recombined bamboo by adopting a hot pressing or cold pressing and hot curing forming method. The main process flow of the recombined bamboo production comprises the working procedures of sawing, subdividing, green removing, untwining, drying, carbonizing, gum dipping, secondary drying, assembling, synthesizing and molding by glue and the like.
In recent years, the industrial scale and the output value of the recombined bamboo industry in China are continuously improved under the support of abundant raw material resources and relevant national industrial policies. The recombined bamboo product is not only widely applied to the fields of indoor and outdoor floors, furniture, building structural materials, decoration and decoration materials, wind power blades and other high-strength material requirements, but also expands the application field of the recombined bamboo to outdoor materials, successfully realizes large-scale industrialization, becomes one of the most advantageous industries with development potential in the bamboo industry in China, and is also a current research hotspot and leading-edge technology of the bamboo industry and the forest industry.
However, the recombined bamboo is easy to mildew under the environment of damp and hot, which affects the use value and appearance of the recombined bamboo and further limits the large-scale popularization and application of the recombined bamboo.
Disclosure of Invention
1. Technical problem to be solved
The recombined bamboo is easy to mildew under the damp and hot environmental condition, the use value and the appearance of the recombined bamboo are influenced, and further the problem of large-scale popularization and application of the recombined bamboo is limited.
2. Technical scheme
In order to achieve the purpose, the application provides a novel mildew-proof recombined bamboo based on pyrolysis oil phenolic resin, which sequentially comprises a first surface layer, a first adhesive layer, a core layer, a second adhesive layer and a second surface layer, wherein the first surface layer is connected with the core layer through the first adhesive layer, and the second surface layer is connected with the core layer through the second adhesive layer; the first adhesive layer is a pyrolytic oil phenolic resin adhesive layer, and the second adhesive layer is a pyrolytic oil phenolic resin adhesive layer.
Another embodiment provided by the present application is: the first surface layer comprises 2-5 layers of bamboo bundles, and the bamboo bundles in each layer are connected through an adhesive layer; the second surface layer comprises 2-5 layers of bamboo bundles, and the bamboo bundles on each layer are connected through an adhesive layer.
Another embodiment provided by the present application is: the bamboo bundle is subjected to biomass pyrolysis oil impregnation treatment, and the bamboo bundle comprises a mildew-proof antibacterial sublayer.
Another embodiment provided by the present application is: the core layer comprises 3-30 layers of netted bamboo bundles.
The application also provides an adhesive layer, the adhesive layer comprises following raw materials:
phenol, formaldehyde solution, sodium hydroxide solution and pyrolysis oil;
the mass ratio of the phenol to the formaldehyde solution is 1: 1.5-2, the mass ratio of the sodium hydroxide solution to the phenol is 0.6-0.8: 1, and the mass ratio of the pyrolysis oil to the phenol is 0.15-0.3: 1.
Another embodiment provided by the present application is: the concentration of the formaldehyde solution is 37 percent, and the concentration of the sodium hydroxide solution is 30 percent.
The application also provides a preparation method of the adhesive layer, which comprises the following steps:
1) taking phenol, formaldehyde solution, pyrolysis oil and sodium hydroxide solution according to a certain proportion, sequentially adding the phenol, the formaldehyde solution, the pyrolysis oil and the sodium hydroxide solution into a synthesis reaction kettle, and stirring a reaction raw material mixed solution;
2) starting a heating device, slowly and gradually heating the mixed solution to 90 +/-3 ℃ within 20min, and keeping the temperature for 40-60 min;
3) starting a cooling device, cooling the mixed solution obtained in the step 2) to 75 ℃, and adding a formaldehyde solution, pyrolysis oil and a sodium hydroxide solution;
4) slowly heating the mixed solution in the step 3) to 90 +/-3 ℃ within 10-15 min, and keeping the temperature for 15-25 min;
5) adding sodium hydroxide solution, continuously reacting for 10-20 min, cooling to below 50 ℃, and discharging.
The application also provides a novel mildew-proof recombined bamboo preparation method based on the pyrolysis oil phenolic resin, which comprises the following steps:
(1) preparing bamboo bundles: cutting raw bamboos into bamboo tubes with different lengths, longitudinally splitting the bamboo tubes into two semicircular bamboo tubes along the diameter of the bamboo tubes, and removing inner joints; then, a fluffer is adopted to directionally fluff the fibers into long mesh loose bundle-shaped units which are mutually cross-linked and keep the original arrangement mode of the fibers; collecting the waste generated in the preparation process of the bamboo bundles for later use;
(2) thermal cracking liquefaction of bamboo wood residues: crushing and drying processing residues such as bamboo scraps, bamboo filaments, bamboo parenchyma cells and the like generated in the raw bamboo material preparation process until the particle size is less than or equal to 40 meshes and the moisture content is less than 5%; carrying out thermal cracking liquefaction on the dried bamboo particles in a pyrolysis reactor, and collecting the obtained bamboo pyrolysis oil for cold storage for later use;
(3) and (3) surface layer bamboo bundle pyrolysis oil impregnation treatment: performing pyrolysis oil soaking treatment on the bamboo bundles with good quality and used for the surface layer;
(4) drying the bamboo bundles: taking the bamboo bundles in the step (1) as a core layer, taking the bamboo bundles in the step (3) as a first surface layer and a second surface layer, and drying the first surface layer, the second surface layer and the core layer;
(5) sizing: bonding the first surface layer, the core layer and the second surface layer by using the adhesive layer;
(6) hot pressing: hot pressing the recombined bamboo by adopting a hot-in-cold-out process, putting a plate blank after the temperature of a hot press reaches a set temperature, starting boosting, starting heat preservation after the temperature of the press reaches a hot pressing pressure, stopping heating, starting cooling, and taking out the plate blank;
(7) and taking out the plate blank, and packaging to obtain the novel mildew-proof recombined bamboo based on the pyrolysis oil phenolic resin.
Another embodiment provided by the present application is: the raw bamboo is one or more of Phyllostachys Pubescens, giant dragon bamboo, green bamboo, Sagittaria trifoliata, dendrocalamus latiflorus and Phyllostachys bambusoides.
Another embodiment provided by the present application is: the pyrolysis reactor is a fluidized bed type, a rotating cone type, a descending tube type or a microwave pyrolysis reactor.
3. Advantageous effects
Compared with the prior art, the novel mildew-proof recombined bamboo based on the pyrolysis oil phenolic resin and the preparation method thereof have the beneficial effects that:
the application provides a pair of novel mould proof reorganization bamboo based on pyrolysis oil phenolic resin, effectively utilizes the remainder of bamboo timber processing enterprise, adds in the production process of reorganization bamboo and gives the certain mould proof bacterinertness of product, improves its product property ability when reducing reorganization bamboo manufacturing cost.
The application provides a pair of novel mould proof reorganization bamboo based on pyrolysis oil phenolic resin improves the raw materials utilization ratio in the bamboo timber course of working, when reducing reorganization bamboo manufacturing cost, improves product mould proof corrosion protection performance. Thereby promoting the further rapid development of the recombined bamboo industry.
The application provides a novel mould proof reorganization bamboo preparation method based on pyrolysis oil phenolic resin, has realized that the bamboo timber prepares full component raw materials utilization of reorganization bamboo product, and components such as the bamboo bits that the workshop section of will prepareeing material produced, bamboo filament and the relatively poor thin-walled cell of mechanical properties reprocess the utilization after the thermal cracking refining, regard as reorganization bamboo surface treatment protective agent and slabbing adhesive respectively, realized that waste utilization, changing waste into valuables, effectively improved the processing utilization ratio of bamboo timber raw materials.
According to the adhesive layer preparation method, the bamboo remainder pyrolysis oil is used for replacing an expensive phenol raw material to prepare the phenolic resin, dependence on petrochemical resources is reduced, and meanwhile, the raw material cost of the phenolic resin can be obviously reduced, so that the production cost of the recombined bamboo is further reduced, and the cost performance of products is improved.
According to the novel mildew-proof recombined bamboo preparation method based on the pyrolysis oil phenolic resin, the adopted substances such as phenols, acids and terpenes contained in the pyrolysis oil have the effects of mildew resistance, bacteria resistance and the like, and when the method is used for manufacturing recombined bamboo products, the protection performance of the recombined bamboo can be effectively enhanced, the phenomena of worm damage, mildew and decay of the recombined bamboo when the recombined bamboo is used outdoors are reduced, the service function of the recombined bamboo is enhanced, and the service life of the recombined bamboo is prolonged.
Drawings
FIG. 1 is a schematic structural diagram of a novel mildew-resistant reconstituted bamboo based on a pyrolysis oil phenolic resin according to the application;
FIG. 2 is a schematic representation of a bonding object of the skin layer and the adhesive layer of the present application;
FIG. 3 is a schematic illustration of a slab embodiment of the present application;
FIG. 4 is a schematic representation of the novel mildewproof reconstituted bamboo article based on a pyrolysis oil phenolic resin of the present application;
in the figure: 1-a first surface layer, 2-a first adhesive layer, 3-a core layer, 4-a second adhesive layer, and 5-a second surface layer.
Detailed Description
Hereinafter, specific embodiments of the present application will be described in detail with reference to the accompanying drawings, and it will be apparent to those skilled in the art from this detailed description that the present application can be practiced. Features from different embodiments may be combined to yield new embodiments, or certain features may be substituted for certain embodiments to yield yet further preferred embodiments, without departing from the principles of the present application.
China is the most important world for producing bamboo, and bamboo resources, bamboo forest area, bamboo storage and yield and the external trade volume of bamboo products are in the top of the world. Bamboo is used as an important forest resource in China, has the characteristics of rich resources, strong reproduction and regeneration capacity, short growth period, excellent material performance and the like, has high industrial production and commercial application values, and is called as the second forest in China. The bamboo can be used for producing bamboo products with multiple purposes by various mechanical, chemical and biological processing methods, and the like, so that the bamboo is used for replacing wood, the consumption of the wood is reduced, the contradiction between supply and demand of the wood is relieved, and the like.
In the production process of the recombined bamboo, about 30% of bamboo processing residues such as bamboo scraps, bamboo filaments, parenchyma cells and the like are generated in the raw material treatment processes such as raw bamboo cutting, flattening, splitting, defibering and the like, and the processing residues are generally directly burned in a boiler, so that the resource utilization efficiency is low; the main raw materials of adhesives such as phenolic resin and the like required by the recombined bamboo gluing are derived from petrochemical resources, so that the raw materials are non-renewable and expensive, and the adhesives are main production elements influencing the production cost of recombined bamboo products.
Referring to fig. 1 to 4, the application provides a novel mildew-proof recombined bamboo based on pyrolytic oil phenolic resin, which sequentially comprises a first surface layer 1, a first adhesive layer 2, a core layer 3, a second adhesive layer 4 and a second surface layer 5, wherein the first surface layer 1 is connected with the core layer 3 through the first adhesive layer 2, and the second surface layer 5 is connected with the core layer 3 through the second adhesive layer 4; the first adhesive layer 2 is a pyrolytic oil phenolic resin adhesive layer, and the second adhesive layer 4 is a pyrolytic oil phenolic resin adhesive layer.
Further, the first surface layer 1 comprises 2-5 layers of bamboo bundles, and the bamboo bundles in each layer are connected through an adhesive layer; the second surface layer 5 comprises 2-5 layers of bamboo bundles, and the bamboo bundles on each layer are connected through an adhesive layer.
Further, the bamboo bundle is subjected to biomass pyrolysis oil impregnation treatment, and the bamboo bundle comprises a mildew-proof antibacterial sublayer.
Further, the core layer 3 comprises 3-30 layers of reticular bamboo bundles.
The application relates to a novel mildew-proof recombined bamboo based on pyrolysis oil phenolic resin, which comprises two surface layers, a core layer 3 and the like, and is formed by gluing and hot pressing through an adhesive layer, wherein the density is about 0.70g/cm3～1.40g/cm3(ii) a The first surface layer 1 and the second surface layer 5 are respectively composed of 2-5 layers of bamboo bundles with good quality and smooth fibers, the bamboo bundles are subjected to biomass pyrolysis oil immersion treatment and loaded with mildew-proof antibacterial substances, the loading rate is about 2% -8% of the oven-dry mass of the bamboo bundles, the bamboo bundles are further subjected to adhesive immersion treatment to form an adhesive layer, and the loading capacity of the adhesive is about 10% -18%; the core layer 3 is composed of 3-0 layers of ordinary netted bamboo bundles obtained through defibering, the specific number of layers is determined according to the size and the density of the board, the bamboo bundles are subjected to adhesive dipping treatment, and the loading capacity of the adhesive is about 8% -16%; the upper and lower surface layers are mainly used for providing high-strength and weather-resistant surface for the plate, and the core layer 3 is mainly used for providing high-strength and weather-resistant surface for the plateThe base material part and the surface layer part are supported, and certain overall strength and density of the plate are provided.
The utility model relates to a novel mould proof reorganization bamboo based on pyrolysis oil phenolic resin, carry out bamboo bundle layering at two top layers and sandwich layer 3, the glueing is with mating formation, the top layer is put to the better bamboo bundle of preferred quality, and carry out the fast hot oil stain mould proof treatment of pyrolysis to the top layer bamboo that takes place to milden easily, and select ordinary bamboo bundle and only carry out the glueing at sandwich layer 3 and handle, the layering is handled and the structure and the performance advantage of laying down each partial material have effectively been played, guaranteeing the colleague of reorganization bamboo product performance, the raw and other materials utilization ratio has been improved, and save the industrial chemicals for the production.
The application also provides an adhesive layer, the adhesive layer comprises following raw materials:
phenol, formaldehyde solution, sodium hydroxide solution and pyrolysis oil;
the mass ratio of the phenol to the formaldehyde solution is 1: 1.5-2, the mass ratio of the sodium hydroxide solution to the phenol is 0.6-0.8: 1, and the mass ratio of the pyrolysis oil to the phenol is 0.15-0.3: 1.
Further, the concentration of the formaldehyde solution is 37%, and the concentration of the sodium hydroxide solution is 30%.
The application also provides a preparation method of the adhesive layer, which comprises the following steps:
1) resin synthesis raw materials such as phenol, formaldehyde, pyrolysis oil, sodium hydroxide solution and the like are weighed according to a certain proportion.
2) And sequentially adding all the metered phenol, part of formaldehyde solution (70-80 percent of the total mass) and part of sodium hydroxide solution (40-50 percent of the total mass) into a synthesis reaction kettle, and stirring the reaction raw material mixed solution.
3) Starting the heating device, slowly and gradually heating the mixed solution to 90 + -3 deg.C within 20min, and keeping the temperature for 40-60 min;
4) starting a cooling device, cooling the mixed solution to 75 ℃, and adding the residual formaldehyde solution (20-30% of the total mass), pyrolysis oil and sodium hydroxide solution (25-30% of the total mass);
5) slowly heating the mixed solution to 90 +/-3 ℃ within 10-15 min, and keeping the temperature for 15-25 min;
6) adding the rest sodium hydroxide solution (25-30% of the total mass), continuously reacting for 10-20 min, cooling to below 50 ℃, and discharging.
The pyrolysis oil is obtained from the thermal cracking liquefaction process of processing residues such as bamboo scraps, bamboo filaments, bamboo parenchyma cells and the like generated in the raw bamboo material preparation process.
The application also provides a novel mildew-proof recombined bamboo preparation method based on the pyrolysis oil phenolic resin, which comprises the following steps:
(1) preparing bamboo bundles: cutting the raw bamboo into bamboo tubes with different lengths (the size is adjusted according to the breadth of a press and the technological requirements), then longitudinally splitting the bamboo tubes into two semicircular bamboo tubes along the diameter of the bamboo tubes, and removing inner sections; then, a fluffer is adopted to directionally fluff the fibers into long mesh loose bundle-shaped units which are mutually cross-linked and keep the original arrangement mode of the fibers; collecting the waste generated in the preparation process of the bamboo bundles for later use;
(2) thermal cracking liquefaction of bamboo wood residues: crushing and drying processing residues such as bamboo scraps, bamboo filaments, bamboo parenchyma cells and the like generated in the raw bamboo material preparation process until the particle size is less than or equal to 40 meshes and the moisture content is less than 5%; carrying out thermal cracking liquefaction on the dried bamboo particles in a pyrolysis reactor, wherein the reaction conditions are as follows: the reaction temperature is 450-550 ℃, the gas phase retention time is less than or equal to 2s, the condensation temperature is less than or equal to 4 ℃, the collected bamboo pyrolytic oil is stored for later use, the bamboo pyrolytic gas can be used as an energy source in the pyrolysis process after being combusted, and the bamboo pyrolytic carbon can be further used as active carbon after being activated; under the condition, the yield of the bamboo pyrolytic oil is 45-60%, the yield of the pyrolytic carbon is 20-30%, and the rest pyrolytic gas is directly combusted to supply heat; the pyrolysis reactor can be a fluidized bed type, a rotating cone type, a descending tube type or a microwave cracking reactor;
(3) and (3) surface layer bamboo bundle pyrolysis oil impregnation treatment: performing pyrolysis oil impregnation treatment on the bamboo bundles with good quality and used on the surface layer (including the upper surface layer and the lower surface layer), and endowing the recombined bamboo wood with mildew-proof and antibacterial properties by using substances such as acids, phenols and the like in pyrolysis oil, wherein the drug loading of the pyrolysis oil is about 2-8% of the oven dry mass of the bamboo bundles;
(4) drying the bamboo bundles: drying (drying by an oven or by solar air) the bamboo bundles subjected to defibering and not impregnated for core layer pavement and the bamboo bundles subjected to defibering and impregnated for surface layer pavement until the water content is 3-10%;
(5) sizing: the self-made pyrolytic oil phenolic resin is used as an adhesive, the initial solid content is about 45-50%, and the glue is applied by adopting a gum dipping mode; firstly, adding a proper amount of distilled water into the original pyrolysis oil phenolic resin adhesive to adjust the solid content of the adhesive to be 15-25%, and uniformly mixing; and (3) dipping at normal temperature, wherein the dipping time of the bamboo bundles in the glue solution is 10-15 min, taking out the bamboo bundles after dipping, and then vertically placing the bamboo bundles for 5-8 min to ensure that the glue on the surfaces of the bamboo bundles does not drip any more, thereby finishing gluing.
(6) And (3) drying after sizing: drying the bamboo bundles after the gum dipping in an oven at 40-60 ℃ or airing the bamboo bundles at a ventilated position to control the water content of the bamboo bundles to be between 6 and 10 percent.
(7) Assembling: weighing the bamboo bundles subjected to glue application and drying according to preset recombined bamboo target density, thickness, volume and the like, and assembling in a mold, wherein the bamboo bundles which are high in quality, compact and subjected to pyrolysis oil impregnation treatment are placed on the surface layer, and the bamboo bundles which are not subjected to impregnation treatment are placed on the core layer.
The target density of the recombined bamboo can be 0.70g/cm3～1.40g/cm3The thickness can be adjusted according to production requirements.
(8) Hot pressing: hot pressing the recombined bamboo by adopting a hot-in-cold-out process, wherein the hot pressing temperature is 140-160 ℃, the plate blank is placed after the temperature of a hot press reaches a set temperature, then boosting is started, the hot pressing pressure is set to be 3.5-4.5 MPa, heat preservation is started after the press reaches the hot pressing pressure, the heat preservation time is 1.0-1.5 min/mm, then heating is stopped, cooling is started, the pressure is released after the temperature of the press is reduced to 40-60 ℃, and the plate blank is taken out.
Wherein the hot pressing time unit is min/mm, which means that the corresponding hot pressing time (min) is determined according to the thickness (mm) of the hot-pressed plate.
(9) And cutting and packaging the board obtained by hot pressing to obtain a novel recombined bamboo product.
The biomass pyrolysis oil is a liquid product obtained by performing thermal cracking liquefaction on raw materials such as agricultural and forestry residues such as bamboo wastes, has wide raw material sources, rich chemical components and lower production cost, and is a green and environment-friendly clean chemical raw material. The pyrolysis oil is rich in components such as phenols, aldehydes and esters, has the potential of participating in the synthetic reaction of phenol-formaldehyde resin, can reduce the preparation cost of the phenolic aldehyde (PF) resin adhesive, and is more environment-friendly. In addition, the phenolic compounds contained in the pyrolysis oil have the capabilities of scavenging free radicals, resisting oxidation, preventing mildew and killing insects, have the effects of resisting insects and preventing mildew, and are beneficial to preventing mildew, worm damage and rot of the recombined bamboo products in the outdoor use process and improving the corrosion resistance and durability of the recombined bamboo products.
Further, the raw bamboo is one or more of moso bamboo, giant dragon bamboo, green bamboo, arrowroot bamboo, hemp bamboo and bamboo.
Further, the pyrolysis reactor is a fluidized bed type, rotating cone type, downcomer type or microwave cracking reactor.
Example 1
(1) Preparing bamboo bundles: cutting raw moso bamboos into bamboo tubes with certain length by taking the moso bamboos as raw materials, longitudinally splitting the bamboo tubes into two semicircular bamboo tubes along the diameter of the bamboo tubes, and removing inner joints; the fiber is directionally defibered into long mesh loose bundle-shaped units which are mutually cross-linked and keep the original arrangement mode of the fibers by a defibering machine.
(2) Thermal cracking liquefaction of bamboo wood residues: crushing and drying bamboo processing residues such as bamboo scraps, bamboo filaments and the like generated in the raw bamboo material preparation process until the particle size is less than or equal to 40 meshes and the moisture content is less than 5%; carrying out thermal cracking liquefaction on the dried bamboo particles in a fluidized bed type pyrolysis reactor, wherein the reaction conditions are as follows: the reaction temperature is 500 +/-10 ℃, the gas phase retention time is less than or equal to 2s, the condensation temperature is less than or equal to 4 ℃, the collected bamboo pyrolytic oil is stored for later use, the bamboo pyrolytic gas can be used as an energy source in the pyrolysis process after being combusted, and the bamboo pyrolytic carbon can be further used as active carbon after being activated; under the condition, the yield of the bamboo pyrolytic oil is 56%, the yield of the pyrolytic carbon is 26%, and the rest pyrolytic gas is directly combusted to supply heat.
(3) And (3) surface layer bamboo bundle pyrolysis oil impregnation treatment: and (3) performing pyrolysis oil impregnation treatment on the bamboo bundles with good quality and used on the surface layer (comprising the upper surface layer and the lower surface layer), and endowing the recombined bamboo wood with mildew-proof and antibacterial properties by using substances such as acids, phenols and the like in the pyrolysis oil, wherein the medicine loading of the pyrolysis oil is about 3% of the oven dry mass of the bamboo bundles.
(4) Drying the bamboo bundles: and (3) drying (drying by an oven or by solar air) the bamboo bundles subjected to defibering and not impregnated for core layer pavement and the bamboo bundles subjected to defibering and impregnated for surface layer pavement until the water content is 8%.
(5) Preparing a pyrolytic oil phenolic resin adhesive: the method for synthesizing the pyrolysis oil phenolic resin by adopting secondary polycondensation and batch feeding comprises the following specific processes: 1) the pyrolysis oil phenolic resin comprises the following raw materials in percentage by weight: the mass ratio of the phenol to the formaldehyde solution is 1:1.6, the mass ratio of the sodium hydroxide solution to the phenol is 0.7:1, and the mass ratio of the pyrolysis oil to the phenol is 0.25: 1; the concentration of the formaldehyde solution is 37 percent, and the concentration of the sodium hydroxide solution is 30 percent. 2) And sequentially adding all the metered phenol, part of formaldehyde solution (75 percent of the total mass) and part of sodium hydroxide solution (50 percent of the total mass) into the synthesis reaction kettle, and stirring the reaction raw material mixed solution. 3) Starting a heating device, slowly and gradually heating the mixed solution to 90 +/-3 ℃ within 20min, and keeping the temperature for 50 min; 4) starting a cooling device, cooling the mixed solution to 75 ℃, and adding the residual formaldehyde solution (25% of the total mass), pyrolysis oil and sodium hydroxide solution (25% of the total mass); 5) slowly heating the mixed solution to 90 +/-3 ℃ within 10-15 min, and keeping the temperature for 20 min. 6) Adding the rest sodium hydroxide solution (25% of the total mass), continuously reacting for 15min, cooling to below 50 ℃, and discharging.
According to the analysis method of the physical and chemical properties of the resin adhesive for the artificial board, the pH value, viscosity, solid content and the like of the bamboo pyrolytic oil phenolic resin are tested, and the results are shown in table 1.
(6) Sizing: the self-made pyrolytic oil phenolic resin is used as an adhesive, the initial solid content is shown in table 1, and the sizing is carried out by adopting a gum dipping mode; firstly, adding a proper amount of distilled water into the original pyrolysis oil phenolic resin adhesive to adjust the solid content of the adhesive to 20%, and uniformly mixing; and (3) dipping at normal temperature, wherein the dipping time of the bamboo bundles in the glue solution is 12 minutes, taking out the bamboo bundles after dipping, and then vertically placing the bamboo bundles for 6 minutes to ensure that the adhesive on the surfaces of the bamboo bundles does not drip any more, thereby finishing gluing.
(7) And (3) drying after sizing: drying the bamboo bundle subjected to gum dipping in an oven at 50 ℃ or airing at a ventilated place, and controlling the water content of the bamboo bundle to be about 8%.
(8) Assembling: according to 0.80g/cm3Weighing the bamboo bundles after glue application and drying according to the recombined bamboo target density, and uniformly paving the bamboo bundles in a mould, wherein the bamboo bundles with better quality and compactness are placed on the surface layer.
(9) Hot pressing: and (3) carrying out hot pressing on the recombined bamboo by adopting a hot-in-cold-out process, wherein the hot pressing temperature is 140 ℃, putting the plate blank into the hot pressing machine after the temperature of the hot pressing machine reaches a set temperature, then starting boosting, the hot pressing pressure is set to be 3.5MPa, keeping the temperature of the pressing machine after the hot pressing pressure is reached, keeping the temperature for 1.1min/mm, then stopping heating, starting cooling, reducing the temperature of the pressing machine to 50 ℃, releasing the pressure, and taking out the plate blank.
(10) And cutting and packaging the hot-pressed board to obtain the recombined bamboo product. According to the mechanical property test method of the wood and the artificial board, the physical mechanical property and the new water resistance of the novel recombined bamboo material are tested, wherein the tests comprise density, static bending strength, elastic modulus, dipping stripping rate, water absorption thickness expansion rate and the like, and the results are shown in table 2. According to GB/T13942.1-2009 Wood durability Performance part 1: the natural decay resistance laboratory test protocol requires that a 12 week old decay test be performed with results as shown in table 3.
Example 2
(1) Preparing bamboo bundles: cutting a raw Sagittaria sagittifolia into bamboo tubes with certain length, longitudinally splitting the bamboo tubes into two semicircular bamboo tubes along the diameter of the bamboo tubes, and removing inner joints; the fiber is directionally defibered into long mesh loose bundle-shaped units which are mutually cross-linked and keep the original arrangement mode of the fibers by a defibering machine.
(2) Thermal cracking liquefaction of bamboo wood residues: crushing and drying bamboo processing residues such as bamboo scraps, bamboo filaments and the like generated in the raw bamboo material preparation process until the particle size is less than or equal to 40 meshes and the moisture content is less than 5%; carrying out thermal cracking liquefaction on the dried bamboo particles in a fluidized bed type pyrolysis reactor, wherein the reaction conditions are as follows: the reaction temperature is 520 +/-10 ℃, the gas phase retention time is less than or equal to 2s, the condensation temperature is less than or equal to 4 ℃, the collected bamboo pyrolytic oil is stored for later use, the bamboo pyrolytic gas can be used as an energy source in the pyrolysis process after being combusted, and the bamboo pyrolytic carbon can be further used as active carbon after being activated; under the condition, the yield of the bamboo pyrolytic oil is 52%, the yield of the pyrolytic carbon is 28%, and the rest pyrolytic gas is directly combusted to supply heat.
(3) And (3) surface layer bamboo bundle pyrolysis oil impregnation treatment: and (3) performing pyrolysis oil impregnation treatment on the bamboo bundles with good quality and used on the surface layer (comprising the upper surface layer and the lower surface layer), and endowing the recombined bamboo wood with mildew-proof and antibacterial properties by using substances such as acids, phenols and the like in the pyrolysis oil, wherein the medicine loading of the pyrolysis oil is about 5% of the oven dry mass of the bamboo bundles.
(4) Drying the bamboo bundles: and (3) drying (drying by an oven or by solar air) the bamboo bundles subjected to defibering and not impregnated for core layer pavement and the bamboo bundles subjected to defibering and impregnated for surface layer pavement until the water content is 6%.
(5) Preparing a pyrolytic oil phenolic resin adhesive: the method for synthesizing the pyrolysis oil phenolic resin by adopting secondary polycondensation and batch feeding comprises the following specific processes: 1) the pyrolysis oil phenolic resin comprises the following raw materials in percentage by weight: the mass ratio of the phenol to the formaldehyde solution is 1:1.8, the mass ratio of the sodium hydroxide solution to the phenol is 0.65:1, and the mass ratio of the pyrolysis oil to the phenol is 0.20: 1; the concentration of the formaldehyde solution is 37 percent, and the concentration of the sodium hydroxide solution is 30 percent. 2) And sequentially adding all the metered phenol, part of formaldehyde solution (70 percent of the total mass) and part of sodium hydroxide solution (40 percent of the total mass) into the synthesis reaction kettle, and stirring the reaction raw material mixed solution. 3) Starting a heating device, slowly and gradually heating the mixed solution to 90 +/-3 ℃ within 20min, and keeping the temperature for 50 min; 4) starting a cooling device, cooling the mixed solution to 75 ℃, and adding the residual formaldehyde solution (30% of the total mass), pyrolysis oil and sodium hydroxide solution (30% of the total mass); 5) slowly heating the mixed solution to 90 +/-3 ℃ within 10-15 min, and keeping the temperature for 15 min. 6) Adding the rest sodium hydroxide solution (30% of the total mass), continuously reacting for 20min, cooling to below 45 ℃, and discharging.
According to the analysis method of the physical and chemical properties of the resin adhesive for the artificial board, the pH value, viscosity, solid content and the like of the bamboo pyrolytic oil phenolic resin are tested, and the results are shown in table 1.
(6) Sizing: the self-made pyrolytic oil phenolic resin is used as an adhesive, the initial solid content is shown in table 1, and the sizing is carried out by adopting a gum dipping mode; firstly, adding a proper amount of distilled water into the original pyrolysis oil phenolic resin adhesive to adjust the solid content to 23%, and uniformly mixing; and (3) dipping at normal temperature, wherein the dipping time of the bamboo bundles in the glue solution is 10 minutes, taking out the bamboo bundles after dipping, and then vertically placing the bamboo bundles for 5 minutes to ensure that the adhesive on the surfaces of the bamboo bundles does not drip any more, thereby finishing gluing.
(7) And (3) drying after sizing: drying the bamboo bundle subjected to gum dipping in an oven at 50 ℃ or airing at a ventilated place, and controlling the water content of the bamboo bundle to be about 8%.
(8) Assembling: according to 1.0g/cm3Weighing the bamboo bundles after glue application and drying according to the recombined bamboo target density, and uniformly paving the bamboo bundles in a mould, wherein the bamboo bundles with better quality and compactness are placed on the surface layer.
(9) Hot pressing: and (3) carrying out hot pressing on the recombined bamboo by adopting a hot-in-cold-out process, wherein the hot pressing temperature is 145 ℃, putting the plate blank into the hot pressing machine after the temperature of the hot pressing machine reaches a set temperature, then starting boosting, the hot pressing pressure is set to be 4.0MPa, keeping the temperature of the pressing machine after the hot pressing pressure is reached, keeping the temperature for 1.2min/mm, then stopping heating, starting cooling, reducing the temperature of the pressing machine to 50 ℃, releasing the pressure, and taking out the plate blank.
(10) And cutting and packaging the hot-pressed board to obtain the recombined bamboo product. According to the mechanical property test method of the wood and the artificial board, the physical mechanical property and the new water resistance of the novel recombined bamboo material are tested, wherein the tests comprise density, static bending strength, elastic modulus, dipping stripping rate, water absorption thickness expansion rate and the like, and the results are shown in table 2. According to GB/T13942.1-2009 Wood durability Performance part 1: the natural decay resistance laboratory test protocol requires that a 12 week old decay test be performed with results as shown in table 3.
Example 3
(1) Preparing bamboo bundles: cutting a raw bamboo into bamboo tubes with certain length by taking a mixed bamboo of a moso bamboo and a sagittaria sagittifolia as a raw material, longitudinally splitting the bamboo tubes into two semicircular bamboo tubes along the diameter of the bamboo tubes, and removing inner joints; the fiber is directionally defibered into long mesh loose bundle-shaped units which are mutually cross-linked and keep the original arrangement mode of the fibers by a defibering machine.
(2) Thermal cracking liquefaction of bamboo wood residues: crushing and drying bamboo processing residues such as bamboo scraps, bamboo filaments and the like generated in the process of preparing raw bamboo materials by mixing moso bamboos, arrowheads and the like, wherein the particle size of the crushed bamboo processing residues is less than or equal to 40 meshes, and the crushed bamboo processing residues are dried until the water content is less than 5%; carrying out thermal cracking liquefaction on the dried bamboo particles in a fluidized bed type pyrolysis reactor, wherein the reaction conditions are as follows: the reaction temperature is 530 +/-10 ℃, the gas phase retention time is less than or equal to 2s, the condensation temperature is less than or equal to 4 ℃, the collected bamboo pyrolytic oil is stored for later use, the bamboo pyrolytic gas can be used as an energy source in the pyrolysis process after being combusted, and the bamboo pyrolytic carbon can be further used as active carbon after being activated; under the condition, the yield of the bamboo pyrolytic oil is 55%, the yield of the pyrolytic carbon is 27%, and the rest pyrolytic gas is directly combusted to supply heat.
(3) And (3) surface layer bamboo bundle pyrolysis oil impregnation treatment: and (3) performing pyrolysis oil impregnation treatment on the bamboo bundles with good quality and used on the surface layer (comprising the upper surface layer and the lower surface layer), and endowing the recombined bamboo wood with mildew-proof and antibacterial properties by using substances such as acids, phenols and the like in pyrolysis oil, wherein the drug loading of the pyrolysis oil is about 6.5% of the oven dry mass of the bamboo bundles.
(4) Drying the bamboo bundles: and (3) drying (drying by an oven or by solar air) the bamboo bundles subjected to defibering and not impregnated for core layer pavement and the bamboo bundles subjected to defibering and impregnated for surface layer pavement until the water content is 4%.
(5) Preparing a pyrolytic oil phenolic resin adhesive: the method for synthesizing the pyrolysis oil phenolic resin by adopting secondary polycondensation and batch feeding comprises the following specific processes: 1) the pyrolysis oil phenolic resin comprises the following raw materials in percentage by weight: the mass ratio of the phenol to the formaldehyde solution is 1:1.9, the mass ratio of the sodium hydroxide solution to the phenol is 0.75:1, and the mass ratio of the pyrolysis oil to the phenol is 0.25: 1; the concentration of the formaldehyde solution is 37 percent, and the concentration of the sodium hydroxide solution is 30 percent. 2) And sequentially adding all the metered phenol, part of formaldehyde solution (70 percent of the total mass) and part of sodium hydroxide solution (40 percent of the total mass) into the synthesis reaction kettle, and stirring the reaction raw material mixed solution. 3) Starting a heating device, slowly and gradually heating the mixed solution to 90 +/-3 ℃ within 20min, and keeping the temperature for 40 min; 4) starting a cooling device, cooling the mixed solution to 75 ℃, and adding the residual formaldehyde solution (30% of the total mass), pyrolysis oil and sodium hydroxide solution (30% of the total mass); 5) slowly heating the mixed solution to 90 +/-3 ℃ within 10min, and keeping the temperature for 15 min. 6) Adding the rest sodium hydroxide solution (30% of the total mass), continuously reacting for 15min, cooling to below 45 ℃, and discharging.
According to the analysis method of the physical and chemical properties of the resin adhesive for the artificial board, the pH value, viscosity, solid content and the like of the bamboo pyrolytic oil phenolic resin are tested, and the results are shown in table 1.
(6) Sizing: the self-made pyrolytic oil phenolic resin is used as an adhesive, the initial solid content is shown in table 1, and the sizing is carried out by adopting a gum dipping mode; firstly, adding a proper amount of distilled water into the original pyrolysis oil phenolic resin adhesive to adjust the solid content of the adhesive to 21%, and uniformly mixing; and (3) dipping at normal temperature, wherein the dipping time of the bamboo bundles in the glue solution is 13 minutes, taking out the bamboo bundles after dipping, and then vertically placing the bamboo bundles for 7 minutes to ensure that the adhesive on the surfaces of the bamboo bundles does not drip any more, thereby finishing gluing.
(7) And (3) drying after sizing: drying the bamboo bundle subjected to gum dipping in an oven at 50 ℃ or airing at a ventilated place, and controlling the water content of the bamboo bundle to be about 8%.
(8) Assembling: according to 1.2g/cm3Weighing the bamboo bundles after glue application and drying according to the recombined bamboo target density, and uniformly paving the bamboo bundles in a mould, wherein the bamboo bundles with better quality and compactness are placed on the surface layer.
(9) Hot pressing: hot pressing of the recombined bamboo is carried out by adopting a hot-in-cold-out process, the hot pressing temperature is 150 ℃, a plate blank is placed after the temperature of a hot press reaches a set temperature, then boosting is started, the hot pressing pressure is set to be 4.2MPa, heat preservation is started after the press reaches the hot pressing pressure, the heat preservation time is 1.3min/mm, then heating is stopped, temperature reduction is started, the pressure is relieved after the temperature of the press is reduced to 50 ℃, and the plate blank is taken out.
(10) And cutting and packaging the hot-pressed board to obtain the recombined bamboo product. According to the mechanical property test method of the wood and the artificial board, the physical mechanical property and the new water resistance of the novel recombined bamboo material are tested, wherein the tests comprise density, static bending strength, elastic modulus, dipping stripping rate, water absorption thickness expansion rate and the like, and the results are shown in table 2. According to GB/T13942.1-2009 Wood durability Performance part 1: the natural decay resistance laboratory test protocol requires that a 12 week old decay test be performed with results as shown in table 3.
TABLE 1 analysis of the properties of the phenolic resin in the pyrolysis oil of bamboo
The physical and chemical properties of the bamboo pyrolytic oil phenolic resin shown in the table 1 are close to those of the traditional industrial phenolic resin, and the requirements of the phenolic resin for recombined bamboo are met.
TABLE 2 analysis results of physical and mechanical properties of novel recombined bamboo materials
Table 2 shows that the results of the analysis of the physical mechanics and water resistance of the novel recombined bamboo material prepared by the invention all meet the quality requirements of the related artificial board products, wherein the static bending strength, the elastic modulus and the like have strong correlation with the density and increase with the increase of the density.
TABLE 3 Corrosion resistance test results of novel recombined bamboo materials
As can be seen from Table 3, after the novel recombined bamboo material is subjected to decay experiments for 12 weeks, the mass loss rates of the novel recombined bamboo material are respectively 5.8%, 6.9% and 7.4%, which are all below 10%, and the novel recombined bamboo material belongs to I-grade decay resistance, which indicates that the novel recombined bamboo prepared by the method has better decay resistance.
Although the present application has been described above with reference to specific embodiments, those skilled in the art will recognize that many changes may be made in the configuration and details of the present application within the principles and scope of the present application. The scope of protection of the application is determined by the appended claims, and all changes that come within the meaning and range of equivalency of the technical features are intended to be embraced therein.
Claims (10)
1. A novel mould proof reorganization bamboo based on pyrolysis oil phenolic resin which characterized in that: the adhesive tape sequentially comprises a first surface layer, a first adhesive layer, a core layer, a second adhesive layer and a second surface layer, wherein the first surface layer is connected with the core layer through the first adhesive layer, and the second surface layer is connected with the core layer through the second adhesive layer; the first adhesive layer is a pyrolytic oil phenolic resin adhesive layer, and the second adhesive layer is a pyrolytic oil phenolic resin adhesive layer.
2. The novel mildewproof reconstituted bamboo based on the pyrolysis oil phenolic resin as claimed in claim 1, wherein the mildewproof reconstituted bamboo comprises the following components in percentage by weight: the first surface layer comprises 2-5 layers of bamboo bundles, and the bamboo bundles in each layer are connected through an adhesive layer; the second surface layer comprises 2-5 layers of bamboo bundles, and the bamboo bundles on each layer are connected through an adhesive layer.
3. The novel mildewproof reconstituted bamboo based on the pyrolysis oil phenolic resin as claimed in claim 2, wherein: the bamboo bundle is subjected to biomass pyrolysis oil impregnation treatment, and the bamboo bundle comprises a mildew-proof antibacterial sublayer.
4. The novel mildewproof reconstituted bamboo based on the pyrolysis oil phenolic resin as claimed in claim 1, wherein the mildewproof reconstituted bamboo comprises the following components in percentage by weight: the core layer comprises 3-30 layers of netted bamboo bundles.
5. An adhesive layer characterized in that: the adhesive layer is composed of the following raw materials:
phenol, formaldehyde solution, sodium hydroxide solution and pyrolysis oil;
the mass ratio of the phenol to the formaldehyde solution is 1: 1.5-2, the mass ratio of the sodium hydroxide solution to the phenol is 0.6-0.8: 1, and the mass ratio of the pyrolysis oil to the phenol is 0.15-0.3: 1.
6. The adhesive layer according to claim 5, wherein: the concentration of the formaldehyde solution is 37 percent, and the concentration of the sodium hydroxide solution is 30 percent.
7. A preparation method of an adhesive layer is characterized by comprising the following steps: the method comprises the following steps:
1) taking phenol, formaldehyde solution, pyrolysis oil and sodium hydroxide solution according to a certain proportion, sequentially adding the phenol, the formaldehyde solution, the pyrolysis oil and the sodium hydroxide solution into a synthesis reaction kettle, and stirring a reaction raw material mixed solution;
2) starting a heating device, slowly and gradually heating the mixed solution to 90 +/-3 ℃ within 20min, and keeping the temperature for 40-60 min;
3) starting a cooling device, cooling the mixed solution obtained in the step 2) to 75 ℃, and adding a formaldehyde solution, pyrolysis oil and a sodium hydroxide solution;
4) slowly heating the mixed solution in the step 3) to 90 +/-3 ℃ within 10-15 min, and keeping the temperature for 15-25 min;
5) adding sodium hydroxide solution, continuously reacting for 10-20 min, cooling to below 50 ℃, and discharging.
8. A novel mildew-proof recombined bamboo preparation method based on pyrolysis oil phenolic resin is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing bamboo bundles: cutting raw bamboos into bamboo tubes with different lengths, longitudinally splitting the bamboo tubes into two semicircular bamboo tubes along the diameter of the bamboo tubes, and removing inner joints; then, a fluffer is adopted to directionally fluff the fibers into long mesh loose bundle-shaped units which are mutually cross-linked and keep the original arrangement mode of the fibers; collecting the waste generated in the preparation process of the bamboo bundles for later use;
(2) thermal cracking liquefaction of bamboo wood residues: crushing and drying bamboo scraps, bamboo filaments and bamboo parenchyma cell processing residues generated in the raw bamboo material preparation process until the particle size is less than or equal to 40 meshes and the moisture content is less than 5%; carrying out thermal cracking liquefaction on the dried bamboo particles in a pyrolysis reactor, and collecting the obtained bamboo pyrolysis oil for cold storage for later use;
(3) and (3) surface layer bamboo bundle pyrolysis oil impregnation treatment: performing pyrolysis oil soaking treatment on the bamboo bundles with good quality and used for the surface layer;
(4) drying the bamboo bundles: taking the bamboo bundles in the step (1) as a core layer, taking the bamboo bundles in the step (3) as a first surface layer and a second surface layer, and drying the first surface layer, the second surface layer and the core layer;
(5) sizing: bonding the first surface layer, the core layer and the second surface layer by using the adhesive layer;
(6) hot pressing: hot pressing the recombined bamboo by adopting a hot-in-cold-out process, putting a plate blank after the temperature of a hot press reaches a set temperature, starting boosting, starting heat preservation after the temperature of the press reaches a hot pressing pressure, stopping heating, starting cooling, and taking out the plate blank;
(7) and taking out the plate blank, and packaging to obtain the novel mildew-proof recombined bamboo based on the pyrolysis oil phenolic resin.
9. A novel method for making mouldproof reconstituted bamboo based on pyrolysis oil phenolic resin according to claim 8, wherein: the raw bamboo is one or more of Phyllostachys Pubescens, giant dragon bamboo, green bamboo, Sagittaria trifoliata, dendrocalamus latiflorus and Phyllostachys bambusoides.
10. A novel method for making mouldproof reconstituted bamboo based on pyrolysis oil phenolic resin according to claim 8, wherein: the pyrolysis reactor is a fluidized bed type, a rotating cone type, a descending tube type or a microwave pyrolysis reactor.
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