CN113715426A - Preparation process of flame-retardant environment-friendly board - Google Patents

Preparation process of flame-retardant environment-friendly board Download PDF

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Publication number
CN113715426A
CN113715426A CN202111004102.7A CN202111004102A CN113715426A CN 113715426 A CN113715426 A CN 113715426A CN 202111004102 A CN202111004102 A CN 202111004102A CN 113715426 A CN113715426 A CN 113715426A
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parts
board
flame
phenolic resin
preparation process
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李银
黄文哲
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Xuebao Home Group Co ltd
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Xuebao Home Group Co ltd
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Priority to CN202111004102.7A priority Critical patent/CN113715426A/en
Publication of CN113715426A publication Critical patent/CN113715426A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—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
    • B32B5/02—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 structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/08—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—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
    • B32B5/18—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 features of a layer of foamed material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—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
    • B32B5/22—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
    • 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
    • B32B5/245—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 another layer next to it being a foam layer
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014—Use of organic additives
    • C08J9/0038—Use of organic additives containing phosphorus
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066—Use of inorganic compounding ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/06—Vegetal fibres
    • B32B2262/062—Cellulose fibres, e.g. cotton
    • B32B2262/065—Lignocellulosic fibres, e.g. jute, sisal, hemp, flax, bamboo
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2266/00—Composition of foam
    • B32B2266/02—Organic
    • B32B2266/0214—Materials belonging to B32B27/00
    • B32B2266/0285—Condensation resins of aldehydes, e.g. with phenols, ureas, melamines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
    • C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
    • C08K5/5333—Esters of phosphonic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C08K7/26—Silicon- containing compounds

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  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Fluid Mechanics (AREA)
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Abstract

The invention provides a preparation process of a flame-retardant environment-friendly plate, and belongs to the technical field of household plates. The preparation process of the flame-retardant environment-friendly board comprises the following steps: s1: preparing phenolic resin liquid; s2: preparing a phenolic foam board; s3: preparing a plate; s4: preparing a composite board; s5: and (5) preparing a finished plate. According to the invention, the flame retardants of dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder are added into the phenolic resin, so that the surface of the plate has a flame retardant effect; meanwhile, the phenolic foam board is arranged in the middle of the board, and the phenolic foam board and the board are coated with adhesives to form a sandwich structure, so that the board has a flame retardant function.

Description

Preparation process of flame-retardant environment-friendly board
Technical Field
The invention belongs to the technical field of household plates, and particularly relates to a preparation process of a flame-retardant environment-friendly plate.
Background
Furniture panels mainly come in the following categories: the wood composite board is characterized by comprising a wood composite board, a malaxad board, a density board and a particle board, wherein the wood composite board is defined in the simplest and most clear manner that wood is cut into thin sheets and then is adhered layer by glue, the malaxad board belongs to the category of wood composite boards, the malaxad board is lighter than the wood composite board, the density board is manufactured by the density board in the majority of furniture, the particle board and the particle board are also commonly called as shaving boards, and the flame-retardant board is one of important materials for furniture processing.
Since the panels mostly contain wood inflammable materials, they are used to catch fire when a fire breaks out. Therefore, the board for furniture needs to have a flame retardant function, but the existing flame retardant board has poor flame retardant effect and fewer layers of boards, and in addition, the processed board often generates harmful odor, so that a safe and environment-friendly board structure with a flame retardant function is necessary.
Disclosure of Invention
The invention provides a preparation process of a flame-retardant environment-friendly plate, and solves the technical problem of poor flame-retardant effect in the prior art.
In order to achieve the purpose, the technical solution of the invention is as follows:
a preparation process of a flame-retardant environment-friendly plate comprises the following steps:
s1: preparing phenolic resin liquid: putting phenolic resin into a container filled with ethanol, stirring for dissolving, adding dimethyl methylphosphonate, uniformly stirring, adding zinc borate, expandable graphite, zeolite powder and water, mixing, rapidly stirring at low temperature for 5-10min, uniformly mixing, and then adjusting the pH to 7 by 1mol/L phosphoric acid aqueous solution to obtain phenolic resin liquid;
s2: preparing a phenolic foam board: putting phenolic resin into a container, adding a foam stabilizer, dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder, quickly stirring for 5-10min at a low temperature, then adding a foaming agent, uniformly stirring, adding a curing agent, stirring for 2-5min, pouring the uniformly mixed material into a preheating mold, foaming and curing in an oven at 70-80 ℃, taking out the mold after 1-2h, cooling and demolding, wherein the thickness of the phenolic foam plate is 0.2-0.5 cm;
s3: plate preparation: processing the bamboo fiber board into a board with the thickness of 0.8-1cm, and drying until the water content is 20-25 wt%; placing the dried plate between two press rollers of a roller press to carry out cross grain radial rolling, so that both sides of the plate are provided with cross grains;
s4: preparing a composite board: placing the phenolic foam board prepared in the step S2 between the two boards prepared in the step S3, coating adhesives on the phenolic foam board and the boards to form a sandwich structure, and then performing hot press molding to obtain a composite board;
s5: completely soaking the composite board in the phenolic resin liquid prepared in the step S1 for 4-5 h; then softening the soaked composite board; and (3) pressurizing the softened plate in a hot press, cooling to normal temperature after pressurization, and then releasing pressure and discharging to obtain a finished product.
Preferably, the phenolic resin liquid in the step S1 includes the following raw materials in parts by weight: 20-30 parts of phenolic resin, 10-14 parts of dimethyl methylphosphonate, 6-10 parts of zinc borate, 4-8 parts of expandable graphite, 2-6 parts of zeolite powder and 40-50 parts of ethanol.
Preferably, the phenolic resin liquid comprises the following raw materials in parts by weight: 25 parts of phenolic resin, 12 parts of dimethyl methylphosphonate, 8 parts of zinc borate, 6 parts of expandable graphite, 4 parts of zeolite powder and 45 parts of ethanol.
Preferably, the phenolic foam board in S2 comprises, by weight, 30 to 40 parts of the following raw material phenolic resin, 12 to 16 parts of a foam stabilizer, 12 to 16 parts of dimethyl methylphosphonate, 8 to 14 parts of zinc borate, 7 to 15 parts of expandable graphite, 4 to 8 parts of zeolite powder, 4 to 8 parts of a foaming agent, and 8 to 13 parts of a curing agent.
Preferably, the foam stabilizer is one of alkylolamide and amine oxide; the foaming agent is one of calcium carbonate, sodium silicate and silicon carbide; the curing agent is one of vinyl triamine, aromatic polyamine and acid anhydride.
Preferably, the depth of the cross striations in the step S3 is 0.1-1mm, and the distance between the cross striations is 0.5-1 cm.
Preferably, the hot press molding in the step S4 is performed at a temperature of 170-200 ℃ and a pressure of 3-4MPa, and the hot press time is 60-120 seconds.
Preferably, the softening in the step S5 is performed at the temperature of 120-130 ℃, and the softening time is 30-40 min.
Preferably, the hot-pressing temperature in the step S5 is 170-185 ℃, the pressure is 2.5-4MPa, and the heating is stopped after the pressure is maintained for 30 min.
The invention has the beneficial effects that:
according to the invention, the flame retardants of dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder are added into the phenolic resin, so that the surface of the plate has a flame retardant effect; meanwhile, the phenolic foam board is arranged in the middle of the board, and the phenolic foam board and the board are coated with adhesives to form a sandwich structure, so that the board has a flame retardant function. In addition, the transverse grains are arranged on the plate, so that the friction force of the plate in contact with other materials is improved, and the glue is prevented from cracking.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
Example 1
A preparation process of a flame-retardant environment-friendly plate comprises the following steps:
s1: preparing phenolic resin liquid: the phenolic resin liquid comprises the following raw materials in parts by weight: 25 parts of phenolic resin, 12 parts of dimethyl methylphosphonate, 10 parts of zinc borate, 8 parts of expandable graphite, 2 parts of zeolite powder and 44 parts of ethanol;
proportionally placing phenolic resin into a container filled with ethanol, stirring for dissolving, adding dimethyl methylphosphonate, uniformly stirring, adding zinc borate, expandable graphite, zeolite powder and water, mixing, rapidly stirring at low temperature for 5min, uniformly mixing, and then adjusting the pH to 7 by 1mol/L phosphoric acid water solution to obtain phenolic resin liquid;
s2: preparing a phenolic foam board: the phenolic foam board comprises the following raw materials of 30 parts of phenolic resin, 12 parts of foam stabilizer, 14 parts of dimethyl methyl phosphonate, 8 parts of zinc borate, 7 parts of expandable graphite, 8 parts of zeolite powder, 8 parts of foaming agent and 11 parts of curing agent by weight;
putting phenolic resin into a container according to a proportion, adding a foam stabilizer, dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder, quickly stirring for 8min at a low temperature, then adding a foaming agent, uniformly stirring, adding a curing agent, stirring for 2min, pouring the uniformly mixed material into a preheating mold, foaming and curing in an oven at 80 ℃, taking out the mold after 1h, cooling and demolding, wherein the thickness of the phenolic foam plate is 0.5 cm;
the foam stabilizer is one of alkylolamide and amine oxide; the foaming agent is one of calcium carbonate, sodium silicate and silicon carbide; the curing agent is one of vinyl triamine, aromatic polyamine and acid anhydride;
s3: plate preparation: processing the bamboo fiberboard into a board with the thickness of 1cm, and drying the board until the water content is 20 wt%; placing the dried plate between two press rollers of a roller press to carry out cross grain radial rolling, so that both sides of the plate are provided with cross grains; the depth of the transverse striations is 1mm, and the distance between the transverse striations is 0.5 cm;
s4: preparing a composite board: placing the phenolic foam board prepared in the step S2 between the two boards prepared in the step S3, coating adhesives on the phenolic foam board and the boards to form a sandwich structure, and then performing hot press molding, wherein the hot press molding is performed at 185 ℃ and 4MPa for 60 seconds to prepare a composite board;
s5: completely soaking the composite board in the phenolic resin liquid prepared in the step S1 for 5 hours; softening the soaked composite board at 125 ℃ for 30 min; and (3) pressurizing the softened sheet in a hot press at 185 ℃ under 2.5MPa for 30min, stopping heating, cooling to normal temperature after pressurization, and then releasing pressure and discharging to obtain a finished product.
Example 2
A preparation process of a flame-retardant environment-friendly plate comprises the following steps:
s1: preparing phenolic resin liquid: the phenolic resin liquid comprises the following raw materials in parts by weight: 30 parts of phenolic resin, 14 parts of dimethyl methylphosphonate, 6 parts of zinc borate, 4 parts of expandable graphite, 4 parts of zeolite powder and 50 parts of ethanol;
proportionally placing phenolic resin into a container filled with ethanol, stirring for dissolving, adding dimethyl methylphosphonate, uniformly stirring, adding zinc borate, expandable graphite, zeolite powder and water, mixing, rapidly stirring at low temperature for 8min, uniformly mixing, and then adjusting the pH to 7 by 1mol/L phosphoric acid water solution to obtain phenolic resin liquid;
s2: preparing a phenolic foam board: the phenolic foam board comprises the following raw materials of 35 parts of phenolic resin, 14 parts of foam stabilizer, 16 parts of dimethyl methyl phosphonate, 12 parts of zinc borate, 12 parts of expandable graphite, 4 parts of zeolite powder, 4 parts of foaming agent and 13 parts of curing agent by weight;
putting phenolic resin into a container according to a proportion, adding a foam stabilizer, dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder, quickly stirring for 10min at a low temperature, then adding a foaming agent, uniformly stirring, then adding a curing agent, stirring for 3min, pouring the uniformly mixed material into a preheating mold, foaming and curing in an oven at 70 ℃, taking out the mold after 1.5h, cooling and demolding, wherein the thickness of the phenolic foam plate is 0.2 cm;
the foam stabilizer is one of alkylolamide and amine oxide; the foaming agent is one of calcium carbonate, sodium silicate and silicon carbide; the curing agent is one of vinyl triamine, aromatic polyamine and acid anhydride;
s3: plate preparation: processing the bamboo fiberboard into a board with the thickness of 0.8cm, and drying the board until the water content is 22 wt%; placing the dried plate between two press rollers of a roller press to carry out cross grain radial rolling, so that both sides of the plate are provided with cross grains; the depth of the transverse striations is 0.1mm, and the distance between the transverse striations is 0.8 cm;
s4: preparing a composite board: placing the phenolic foam board prepared in the step S2 between the two boards prepared in the step S3, coating adhesives on the phenolic foam board and the boards to form a sandwich structure, and then performing hot press molding, wherein the hot press molding is performed at the temperature of 200 ℃ and the pressure of 3MPa for 80 seconds to prepare a composite board;
s5: completely soaking the composite board in the phenolic resin liquid prepared in the step S1 for 4 hours; softening the soaked composite board at 130 ℃ for 35 min; and (3) pressurizing the softened sheet in a hot press at the temperature of 170 ℃ under the pressure of 3MPa, maintaining the pressure for 30min, stopping heating, cooling to normal temperature after pressurization, and then releasing pressure and discharging to obtain a finished product.
Example 3
A preparation process of a flame-retardant environment-friendly plate comprises the following steps:
s1: preparing phenolic resin liquid: the phenolic resin liquid comprises the following raw materials in parts by weight: 20 parts of phenolic resin, 10 parts of dimethyl methylphosphonate, 8 parts of zinc borate, 6 parts of expandable graphite, 6 parts of zeolite powder and 40 parts of ethanol;
proportionally placing phenolic resin into a container filled with ethanol, stirring for dissolving, adding dimethyl methylphosphonate, uniformly stirring, adding zinc borate, expandable graphite, zeolite powder and water, mixing, rapidly stirring at low temperature for 10min, uniformly mixing, and then adjusting the pH to 7 by 1mol/L phosphoric acid water solution to obtain phenolic resin liquid;
s2: preparing a phenolic foam board: the phenolic foam board comprises the following raw materials of 40 parts of phenolic resin, 16 parts of foam stabilizer, 12 parts of dimethyl methyl phosphonate, 14 parts of zinc borate, 15 parts of expandable graphite, 6 parts of zeolite powder, 6 parts of foaming agent and 8 parts of curing agent by weight;
putting phenolic resin into a container according to a proportion, adding a foam stabilizer, dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder, quickly stirring for 5min at a low temperature, then adding a foaming agent, uniformly stirring, adding a curing agent, stirring for 5min, pouring the uniformly mixed material into a preheating mold, foaming and curing in an oven at 75 ℃, taking out the mold after 2h, cooling and demolding, wherein the thickness of the phenolic foam plate is 0.3 cm;
the foam stabilizer is one of alkylolamide and amine oxide; the foaming agent is one of calcium carbonate, sodium silicate and silicon carbide; the curing agent is one of vinyl triamine, aromatic polyamine and acid anhydride;
s3: plate preparation: processing the bamboo fiberboard into a board with the thickness of 0.9cm, and drying the board until the water content is 25 wt%; placing the dried plate between two press rollers of a roller press to carry out cross grain radial rolling, so that both sides of the plate are provided with cross grains; the depth of the transverse striations is 0.5mm, and the distance between the transverse striations is 1 cm;
s4: preparing a composite board: placing the phenolic foam board prepared in the step S2 between the two boards prepared in the step S3, coating adhesives on the phenolic foam board and the boards to form a sandwich structure, and then performing hot press molding, wherein the hot press molding is performed at the temperature of 170 ℃ and the pressure of 3.5MPa for 120 seconds to prepare a composite board;
s5: completely soaking the composite board in the phenolic resin liquid prepared in the step S1 for 4.5 hours; softening the soaked composite board at 120 ℃ for 40 min; and (3) pressurizing the softened sheet in a hot press at 180 ℃ under 4MPa, maintaining the pressure for 30min, stopping heating, cooling to normal temperature after pressurization, and then releasing pressure and discharging to obtain a finished product.
Example 4
A preparation process of a flame-retardant environment-friendly plate comprises the following steps:
s1: preparing phenolic resin liquid: the phenolic resin liquid comprises the following raw materials in parts by weight: 25 parts of phenolic resin, 12 parts of dimethyl methylphosphonate, 8 parts of zinc borate, 6 parts of expandable graphite, 4 parts of zeolite powder and 45 parts of ethanol;
proportionally placing phenolic resin into a container filled with ethanol, stirring for dissolving, adding dimethyl methylphosphonate, uniformly stirring, adding zinc borate, expandable graphite, zeolite powder and water, mixing, rapidly stirring at low temperature for 8min, uniformly mixing, and then adjusting the pH to 7 by 1mol/L phosphoric acid water solution to obtain phenolic resin liquid;
s2: preparing a phenolic foam board: the phenolic foam board comprises the following raw materials, by weight, 34 parts of phenolic resin, 14 parts of a foam stabilizer, 15 parts of dimethyl methyl phosphonate, 12 parts of zinc borate, 11 parts of expandable graphite, 6 parts of zeolite powder, 7 parts of a foaming agent and 10 parts of a curing agent;
putting phenolic resin into a container according to a proportion, adding a foam stabilizer, dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder, quickly stirring for 9min at a low temperature, then adding a foaming agent, uniformly stirring, then adding a curing agent, stirring for 3min, pouring the uniformly mixed material into a preheating mold, foaming and curing in an oven at 75 ℃, taking out the mold after 1.2h, cooling and demolding, wherein the thickness of the phenolic foam plate is 0.4 cm;
the foam stabilizer is one of alkylolamide and amine oxide; the foaming agent is one of calcium carbonate, sodium silicate and silicon carbide; the curing agent is one of vinyl triamine, aromatic polyamine and acid anhydride;
s3: plate preparation: processing the bamboo fiberboard into a board with the thickness of 0.9cm, and drying the board until the water content is 22 wt%; placing the dried plate between two press rollers of a roller press to carry out cross grain radial rolling, so that both sides of the plate are provided with cross grains; the depth of the transverse striations is 0.6mm, and the distance between the transverse striations is 0.8 cm;
s4: preparing a composite board: placing the phenolic foam board prepared in the step S2 between the two boards prepared in the step S3, coating adhesives on the phenolic foam board and the boards to form a sandwich structure, and then performing hot press molding, wherein the hot press molding is performed at the temperature of 180 ℃ and the pressure of 3.4MPa for 100 seconds to prepare a composite board;
s5: completely soaking the composite board in the phenolic resin liquid prepared in the step S1 for 5 hours; softening the soaked composite board at 125 ℃ for 40 min; and (3) pressurizing the softened sheet in a hot press at 175 ℃ under 3.5MPa, maintaining the pressure for 30min, stopping heating, cooling to normal temperature after pressurization, and then releasing pressure and discharging to obtain a finished product.
Test cases
The finished products of examples 1-4 were prepared into 10 x 10cm small samples, one small sample was taken, the sample was placed in a combustion cylinder, a nitrogen-oxygen mixture was introduced from the bottom of the combustion cylinder, the sample was ignited from the upper end with an igniter, the concentration of oxygen in the mixer was changed until the flame front just reached the index of the sample, and the oxygen index of each group of samples was calculated. The thermal conductivity of the samples was edge-leaked using a thermal conductivity meter and the results are shown in the following table.
Group of Oxygen index (%) Thermal conductivity W/(m.K)
Example 1 42.31 0.025
Example 2 40.38 0.028
Example 3 41.69 0.026
Example 4 43.12 0.027
As can be seen from the table above, the sheet material of the present invention has a high oxygen index and a low thermal conductivity, and therefore has strong flame retardancy.
According to the invention, the flame retardants of dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder are added into the phenolic resin, so that the surface of the plate has a flame retardant effect; meanwhile, the phenolic foam board is arranged in the middle of the board, and the phenolic foam board and the board are coated with adhesives to form a sandwich structure, so that the board has a flame retardant function. In addition, the transverse grains are arranged on the plate, so that the friction force of the plate in contact with other materials is improved, and the glue is prevented from cracking.
According to the invention, dimethyl methylphosphonate is heated to generate gaseous products, and the gases contain PO & can capture free radicals H & and HO & in a matrix to inhibit combustion chain reaction; and the heat is decomposed into orthophosphoric acid with stronger acidity, so as to promote the carbon formation and achieve the effects of heat insulation, oxygen isolation and combustion termination. The zinc borate has the characteristics of high thermal stability, low density, good dispersibility, low toxicity and smoke abatement, and the release of crystal water can play a role in absorbing heat and diluting combustible gas and simultaneously prevent oxidation and heat from acting on a combustion substrate, so that the combustion rate is reduced. The expandable graphite contains a carbon source, an acid source and a gas source, wherein the carbon source can generate a carbon layer, and the carbon source is generally a multifunctional carbon forming agent with high carbon content, and the effectiveness of the carbon forming agent is determined by the carbon content and the number of active functional groups; the acid source releases substances with high boiling point and weak oxidizing inorganic acid under the heating condition, and can promote the dehydration of the polyhydric alcohol into carbon; the gas source is heated to release a large amount of inert gas substances, so that the viscous carbon layer can be foamed and expanded. The sheet structure of the expandable graphite blocks the open-cell phenomenon caused by foam rupture, thereby reducing the thermal conductivity of the phenolic sheet foam board. The zeolite is composed of a three-dimensional framework of silicate formed by tetrahedrons of alumina and silica, the space structure is in a space grid shape, and relatively large cavities and pore passages are arranged in the framework, and the cavities and the pore passages are all provided with crystal water molecules. The crystal water of zeolite can absorb some reaction heat and has the function of flame retardance.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or other related fields directly or indirectly are included in the scope of the present invention.

Claims (9)

1. The preparation process of the flame-retardant environment-friendly board is characterized by comprising the following steps of:
s1: preparing phenolic resin liquid: putting phenolic resin into a container filled with ethanol, stirring for dissolving, adding dimethyl methylphosphonate, uniformly stirring, adding zinc borate, expandable graphite, zeolite powder and water, mixing, rapidly stirring at low temperature for 5-10min, uniformly mixing, and then adjusting the pH to 7 by 1mol/L phosphoric acid aqueous solution to obtain phenolic resin liquid;
s2: preparing a phenolic foam board: putting phenolic resin into a container, adding a foam stabilizer, dimethyl methylphosphonate, zinc borate, expandable graphite and zeolite powder, quickly stirring for 5-10min at a low temperature, then adding a foaming agent, uniformly stirring, adding a curing agent, stirring for 2-5min, pouring the uniformly mixed material into a preheating mold, foaming and curing in an oven at 70-80 ℃, taking out the mold after 1-2h, cooling and demolding, wherein the thickness of the phenolic foam plate is 0.2-0.5 cm;
s3: plate preparation: processing the bamboo fiber board into a board with the thickness of 0.8-1cm, and drying until the water content is 20-25 wt%; placing the dried plate between two press rollers of a roller press to carry out cross grain radial rolling, so that both sides of the plate are provided with cross grains;
s4: preparing a composite board: placing the phenolic foam board prepared in the step S2 between the two boards prepared in the step S3, coating adhesives on the phenolic foam board and the boards to form a sandwich structure, and then performing hot press molding to obtain a composite board;
s5: completely soaking the composite board in the phenolic resin liquid prepared in the step S1 for 4-5 h; then softening the soaked composite board; and (3) pressurizing the softened plate in a hot press, cooling to normal temperature after pressurization, and then releasing pressure and discharging to obtain a finished product.
2. The preparation process of the flame-retardant environment-friendly board as claimed in claim 1, wherein the phenolic resin liquid in the step S1 comprises the following raw materials in parts by weight: 20-30 parts of phenolic resin, 10-14 parts of dimethyl methylphosphonate, 6-10 parts of zinc borate, 4-8 parts of expandable graphite, 2-6 parts of zeolite powder and 40-50 parts of ethanol.
3. The preparation process of the flame-retardant environment-friendly board as claimed in claim 2, wherein the phenolic resin liquid comprises the following raw materials in parts by weight: 25 parts of phenolic resin, 12 parts of dimethyl methylphosphonate, 8 parts of zinc borate, 6 parts of expandable graphite, 4 parts of zeolite powder and 45 parts of ethanol.
4. The preparation process of the flame-retardant environment-friendly board as claimed in claim 1, wherein the phenolic foam board in S2 comprises, by weight, 30-40 parts of the following raw materials, phenolic resin, 12-16 parts of a foam stabilizer, 12-16 parts of dimethyl methylphosphonate, 8-14 parts of zinc borate, 7-15 parts of expandable graphite, 4-8 parts of zeolite powder, 4-8 parts of a foaming agent, and 8-13 parts of a curing agent.
5. The preparation process of the flame-retardant environment-friendly board as claimed in claim 4, wherein the foam stabilizer is one of alkylolamide and amine oxide; the foaming agent is one of calcium carbonate, sodium silicate and silicon carbide; the curing agent is one of vinyl triamine, aromatic polyamine and acid anhydride.
6. The process for preparing the flame-retardant environment-friendly board as claimed in claim 1, wherein the depth of the cross striations in the step S3 is 0.1-1mm, and the distance between the cross striations is 0.5-1 cm.
7. The preparation process of the flame-retardant environment-friendly board as claimed in claim 1, wherein the hot press molding in the step S4 is performed at a temperature of 170-200 ℃ and a pressure of 3-4MPa, and the hot press time is 60-120 seconds.
8. The preparation process of the flame-retardant environment-friendly board as claimed in claim 1, wherein the softening in the step S5 is performed at a temperature of 120-130 ℃, and the softening time is 30-40 min.
9. The preparation process of the flame-retardant environment-friendly board according to claim 8, wherein the hot pressing temperature in the step S5 is 170-185 ℃, the pressure is 2.5-4MPa, and the heating is stopped after the pressure is maintained for 30 min.
CN202111004102.7A 2021-08-30 2021-08-30 Preparation process of flame-retardant environment-friendly board Pending CN113715426A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1613638A (en) * 2003-11-05 2005-05-11 厦门新风机实业有限公司 Flame retardant phenolic resin foamed sandwiching material and its preparation
CN104669763A (en) * 2015-02-17 2015-06-03 中国林业科学研究院林产化学工业研究所 Preparation method of phenolic foam sandwich composite board
CN104985648A (en) * 2015-06-24 2015-10-21 中国林业科学研究院木材工业研究所 Flame-retardant composite plate containing phenolic foam crushed material and manufacturing method and application thereof
CN105733173A (en) * 2014-12-11 2016-07-06 苏州美克思科技发展有限公司 Preparation method of high efficient and energy saving phenolic foam board
CN107877625A (en) * 2017-11-05 2018-04-06 茆莉娟 A kind of compound bamboo fiberboard of thermal-insulation three-decker formula

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1613638A (en) * 2003-11-05 2005-05-11 厦门新风机实业有限公司 Flame retardant phenolic resin foamed sandwiching material and its preparation
CN105733173A (en) * 2014-12-11 2016-07-06 苏州美克思科技发展有限公司 Preparation method of high efficient and energy saving phenolic foam board
CN104669763A (en) * 2015-02-17 2015-06-03 中国林业科学研究院林产化学工业研究所 Preparation method of phenolic foam sandwich composite board
CN104985648A (en) * 2015-06-24 2015-10-21 中国林业科学研究院木材工业研究所 Flame-retardant composite plate containing phenolic foam crushed material and manufacturing method and application thereof
CN107877625A (en) * 2017-11-05 2018-04-06 茆莉娟 A kind of compound bamboo fiberboard of thermal-insulation three-decker formula

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