CN114656882A - Composite adhesive, flame-retardant wood substrate using composite adhesive and preparation process of flame-retardant wood substrate - Google Patents
Composite adhesive, flame-retardant wood substrate using composite adhesive and preparation process of flame-retardant wood substrate Download PDFInfo
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- CN114656882A CN114656882A CN202210401039.9A CN202210401039A CN114656882A CN 114656882 A CN114656882 A CN 114656882A CN 202210401039 A CN202210401039 A CN 202210401039A CN 114656882 A CN114656882 A CN 114656882A
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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
- C09J1/00—Adhesives based on inorganic constituents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/002—Manufacture of substantially flat articles, e.g. boards, from particles or fibres characterised by the type of binder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
- B27N3/10—Moulding of mats
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
- B27N3/18—Auxiliary operations, e.g. preheating, humidifying, cutting-off
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
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- Chemical And Physical Treatments For Wood And The Like (AREA)
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Abstract
The invention discloses a composite adhesive, a flame-retardant wood substrate using the same and a preparation process thereof. The composite adhesive, wood powder and water are stirred, pre-pressed and molded, hot-pressed and solidified, and maintained at room temperature to prepare the flame-retardant wood substrate, wherein the raw material components of the composite adhesive comprise light-burned magnesium oxide, magnesium chloride, sodium silicate, semi-hydrated gypsum, fly ash and aluminum oxide; a set control agent and a crosslinking agent can also be added. The invention adopts light-burned magnesium oxide, magnesium chloride and water to form a magnesium oxychloride gelling system as a main colloid of the adhesive, and sodium silicate, semi-hydrated gypsum, fly ash and alumina form an auxiliary colloid of the adhesive; wood powder and an inorganic gelling system are uniformly mixed in an impregnation mode, so that the mechanical strength and the flame retardant property of the wood base material are improved; the wood substrate prepared by the invention not only keeps the wood texture of the material, has good decoration effect, but also has the technical characteristics of flame retardance, no aldehyde, mildew resistance and moth resistance, has wide application range and can be used for large-scale production.
Description
Technical Field
The invention relates to a composite adhesive, a flame-retardant wood substrate using the same and a preparation process of the flame-retardant wood substrate, and belongs to the technical field of novel composite fiber boards.
Background
The traditional artificial fiberboard is mainly prepared by taking wood fibers such as wood chips and wood powder as main raw materials, adding an adhesive and carrying out a hot pressing process. The following industrial problems mainly exist: 1. formaldehyde and other toxic and harmful volatile substances are high; 2. the fire-resistant composite material can be combusted when meeting fire, and releases a large amount of dense smoke and toxic and harmful substances in the combustion process, so that the safety performance is not guaranteed; 3. the product can expand when meeting water, the strength of the product is rapidly reduced, and the product can not be applied in the open air environment; in an environment with high humidity, the product is easy to absorb moisture and expand, so that the product is deformed and the service life is influenced; 4. poor nail-holding power, which results in great compromise of installation and use performance of the product; 5. and the plastic film is easy to mildew and rot in a humid environment.
The artificial fiberboard taking the magnesium oxychloride inorganic gelling system as the adhesive has the advantages of corrosion resistance, moth prevention, no aldehyde, water resistance, excellent mechanical property and the like, but the artificial fiberboard prepared by the inorganic gelling system has the defects of low early strength of the board, serious surface halogen return and the like.
Patent CN105437327B discloses a preparation method of moisture-proof, mildew-proof, low-formaldehyde type medium and high density fiberboard. The preparation method comprises the following steps: (1) chipping (2), screening (3), pre-cooking and the like, and mixing wood fiber and an organic binder to prepare a board, but the product does not have the characteristic of flame resistance and zero formaldehyde.
CN 107443522A discloses a fireproof wood board, which comprises a wood board layer and a fireproof layer; the fireproof layer is formed by coating a fire retardant on the surface of the wood board; the flame retardant is prepared from the following raw materials in percentage by weight: 15-26% of silica sol, 5-20% of resin, 11-13% of titanium dioxide, 13-16% of kaolin, 8-10% of silica powder and the balance of water, but the long-term flame retardant effect cannot be achieved by only adopting the flame retardant layer for treatment.
CN 112300619 a discloses a fireproof wood board, which comprises a wood layer, a first magnesium oxide coating coated on the front surface of the wood layer, and a second magnesium oxide coating coated on the back surface of the wood layer, wherein the front surface of the first magnesium oxide coating is coated with a flame-retardant glue layer, and the back surface of the second magnesium oxide coating is coated with a flame-retardant glue layer. The wood board obtained by the invention adopts the double-layer flame-retardant coating, but the whole fire resistance is not formed, and the wood board loses the fire resistance after the coating is damaged.
CN20120336015.6 discloses a process for manufacturing a fire-freezing plate, which is a fire-proof plate made of a cement base material, is lack of wood texture, has high density and is not easy to carry, and is formed by adding melamine paster. The melamine sticker process has formaldehyde release and does not meet the existing environmental protection and green requirements.
CN 110815487A relates to a wooden fireproof pressure plate and a manufacturing method thereof, and the wooden fireproof pressure plate is formed by cold pressing 2-10 MPa after uniformly mixing a wooden powder material with the content of more than 50 wt% and an additive; the additive comprises a metal oxide, a non-metal oxide, a hydrochloride salt, a sulfate salt, a phosphate salt, a weak acid, and a strong acid. The technical method has the advantages of long cold pressing time of 12-36 hours, complex production process, low production efficiency, addition of a large amount of strong acid in the material production process, dangerous process operation and no environmental protection property, and the produced product has high density and no light weight.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a composite adhesive and a flame-retardant wood substrate using the same, and provides a preparation process of the flame-retardant wood substrate. The novel composite adhesive provided by the invention replaces the traditional organic adhesive, and avoids the introduction of formaldehyde from the source; the wood substrate prepared by the method can reach B1 flame retardant level, has the characteristics of early strength, excellent processing performance, mould prevention, moth prevention and the like, solves the biggest problem of combustibility of the wood substrate, reduces the halogen return phenomenon of a magnesium oxychloride inorganic gelling system, and expands the applicable field of the wood substrate.
The invention provides a composite adhesive, which comprises the following raw material components of light-burned magnesium oxide, magnesium chloride, sodium silicate, semi-hydrated gypsum, fly ash and aluminum oxide;
the content of active magnesium oxide in the light-burned magnesium oxide is more than 60 percent;
the molar ratio of the magnesium chloride to the active magnesium oxide in the light-burned magnesium oxide is 5-8: 1, the content of sodium silicate is 5-10% of the mass of the active magnesium oxide in the light-burned magnesium oxide, the content of semi-hydrated gypsum is 10-20% of the mass of the active magnesium oxide in the light-burned magnesium oxide, the content of fly ash is 0.5-2% of the mass of the active magnesium oxide in the light-burned magnesium oxide, and the content of aluminum oxide is 1-5% of the mass of the active magnesium oxide in the light-burned magnesium oxide;
when the composite adhesive is not used, all components can be independently stored, water is added when the composite adhesive is used, the light-burned magnesium oxide, the magnesium chloride and the water form a magnesium oxychloride gelling system as a main colloid of the adhesive, and the sodium silicate, the semi-hydrated gypsum, the fly ash and the aluminum oxide form an auxiliary colloid of the adhesive.
The invention adopts sodium silicate, semi-hydrated gypsum, fly ash and alumina to react to form auxiliary colloid. The addition of the semi-hydrated gypsum can shorten the setting time of a magnesium oxychloride gelling system and can react with sodium silicate and fly ash to generate calcium silicate and dicalcium silicate, so that the early mechanical strength of the wood substrate is improved; the active silicon dioxide component in the fly ash can react with the active magnesium oxide to generate magnesium silicate, thereby playing a role in adhesion; the aluminum oxide can react with water to generate aluminum hydroxide, and plays a role in flocculent adhesion; under the condition of water, the sodium silicate can react with unreacted active magnesium oxide and semi-hydrated gypsum to respectively generate magnesium silicate and calcium silicate, so that the mechanical property and the high-temperature resistance of an inorganic gelling system are improved.
Preferably, the composite adhesive further comprises a coagulation regulator, and the content of the coagulation regulator is 0.1-2% of the mass of active magnesium oxide in the light burned magnesium oxide.
Preferably, the composite adhesive also comprises a cross-linking agent, and the content of the cross-linking agent is 0.1-2% of the mass of active magnesium oxide in the light calcined magnesium oxide.
Preferably, the set control agent is one or more selected from citric acid, malic acid, phosphoric acid and sodium polyphosphate.
In the above aspect, the crosslinking agent is preferably selected from at least one of polyvinyl alcohol (PVA), γ -aminopropyltriethoxysilane (KH550), and γ - (2, 3-glycidoxy) propyltrimethoxysilane (KH 560).
In the above aspect, the light calcined magnesia preferably has a powder fineness of 50 to 300 meshes.
The invention also provides a flame-retardant wood base plate, which is obtained by prepressing and molding the material uniformly mixed by the composite adhesive, the wood powder and the water, and then curing the material after multi-stage mould pressing and hot press setting;
the mass ratio of the composite adhesive to the wood powder to the water is 30-70: 70-30: 24-63;
the wood powder is an organic matter which has a grain diameter not more than 2mm and takes wood fiber as a main component, and the organic matter is wood, straw, rice hull or fruit shell powder; the water content of the wood powder is not more than 5 percent;
the multistage die pressing is to perform the press forming after the materials are pre-pressed and formed by a die and then subjected to program multistage pressure boosting.
Further, the grain size of the wood powder is not more than 2mm, and the preferable grain size is not more than 0.5 mm.
The invention also provides a specific preparation process of the flame-retardant wood base plate, which comprises the following steps:
(1) weighing raw material components of the composite adhesive, namely magnesium chloride, light-burned magnesium oxide, sodium silicate, semi-hydrated gypsum, fly ash, aluminum oxide, a thickening time control agent and a cross-linking agent in sequence, and weighing wood powder and water;
(2) mixing magnesium chloride with water to prepare a magnesium chloride solution, and then adding a coagulation regulator to obtain a mixed solution of the coagulation regulator and the magnesium chloride;
(3) fully soaking the dried wood powder by adopting the mixed solution of the thickening time control agent and magnesium chloride, and then uniformly stirring the light-burned magnesium oxide, aluminum oxide, sodium silicate, semi-hydrated gypsum, fly ash and a cross-linking agent with the soaked wood powder;
(4) uniformly paving the uniformly stirred materials in the step (3) in a mould for prepressing and forming, and then carrying out multi-stage mould pressing and hot press setting to obtain an uncured wood substrate;
(5) and (5) placing the uncured wood base plate obtained in the step (4) under the conditions of constant temperature and constant humidity for curing for a period of time, and then placing the wood base plate at room temperature for curing to obtain the flame-retardant wood composite board.
The pre-pressing molding operation condition in the step (4) is normal temperature and normal pressure, and the hot press-fixing process operation condition is as follows: the temperature is 35 +/-2 ℃, the unit pressure is 5-17 MPa, and the pressing time is 3-12 h.
The constant temperature and humidity condition in the step (5) is as follows: the temperature is 20 +/-2 ℃, the humidity is 60 +/-2% RH, and the curing time is 7-28 days.
The coagulation regulator can be dissolved in magnesium chloride solution, and the dispersibility of the coagulation regulator in a wood substrate is improved.
In the invention, MgO-MgCl is adopted when preparing the flame-retardant wood substrate2-H2The O ternary gelling system is used as a main colloid, and sodium silicate, semi-hydrated gypsum, fly ash and alumina react to form an auxiliary colloid. The synergistic use of main and auxiliary colloids makes up for MgO-MgCl2-H2The O-ternary cementing system has the defect of poor early mechanical property, and the wood base material is ensured to have higher mechanical property in the whole service cycle. In addition, the introduction of auxiliary colloid reduces MgCl in the wood substrate2Thereby reducing the influence of the re-halogenation on the performance of the base material and the corrosion of chloride ions on the light steel keel.
When the adhesive is used, the main colloid is MgO-MgCl2-H2The magnesium oxychloride gel material is formed by an O ternary system. The cementing material is different from the coagulation principle of an organic adhesive and the hydration mechanism of portland cement, and the main hydration product of the cementing material is basic magnesium oxychloride crystal, namely xMg (OH)2·yMgCl2·zH2O, which is generally in the form of a needle bar, a long rod, a fiber, or the like. By formation of compact crystals of basic magnesium oxychlorideThe net structure is a direct source of mechanical properties of the magnesium oxychloride cementing material. The magnesium oxychloride gelling agent is used as a novel inorganic adhesive of the wood substrate to replace the traditional organic adhesive, so that the introduction of formaldehyde is avoided from the source. Because formaldehyde contained in the wood substrate is mainly caused by the organic adhesive. Secondly, the magnesium oxychloride cementing material is an air-hardening cementing material, has the characteristics of quick setting and hardening and high mechanical strength, and in the combustion process, crystals in the cementing material are heated and decomposed, and the generated MgO can cover the surface of the wood fiber, thereby playing the roles of heat insulation and smoke suppression. Meanwhile, crystal water in the crystal volatilizes, so that the heat of combustion is absorbed, the concentration of local combustible gas is diluted, and the flame retardant effect is realized.
Furthermore, the coagulation time of an inorganic gelling system can be improved by adding the coagulation regulator, and the early strength of the wood substrate is improved; the addition of the cross-linking agent can improve the binding capacity of the inorganic gelling system and the wood fiber and improve the mechanical property of the wood substrate.
The wood fiber adopted by the invention is wood powder with the thickness not greater than 2mm, and the purpose is to uniformly mix the wood fiber and the inorganic adhesive, so that the structure of the wood substrate is compact, and the mechanical property of the wood substrate is ensured. After being mixed with the inorganic adhesive, the wood fiber is in multi-dimensional disorientation arrangement and has the reinforcing effect on the microstructure of an inorganic gelling system. Through the reinforcement constraint of the wood fiber, the generation and growth of microcracks in the inorganic adhesive are inhibited, so that the crack resistance of the inorganic gelling system is improved.
The key point is that the impregnation dispersion system adopted in the preparation process of the invention firstly impregnates the wood fiber with the magnesium chloride solution, and the magnesium chloride solution and the wood fiber are uniformly mixed in a liquid-solid mixing mode. The impregnated wood fiber can become a micro-reaction site, and the magnesium chloride uniformly dispersed on the wood fiber is further reacted with the active magnesium oxide and the sodium silicate, so that the local agglomeration of inorganic gel is avoided, and the problem of non-uniform dispersion of the inorganic adhesive and a large amount of wood fiber is solved. Meanwhile, the main colloid and the auxiliary colloid are matched for use, so that the setting time of the inorganic adhesive can be effectively shortened, the crystal growth and reaction rate are promoted, the stability of the cementing material is improved, and the strength of the wood substrate in different use periods is ensured.
The invention effectively combines the wood fiber with various inorganic gelling systems for the first time, adopts a multi-stage mould pressing process, generates synergistic benefits and avoids respective defects, thereby obtaining the novel nonflammable zero-formaldehyde wood substrate.
Drawings
Fig. 1 is a flow chart of the preparation process of the fire-retardant wood substrate of the present invention.
FIG. 2 is a surface topography of the fire-retardant wood-based panel made in example 1 of the present invention.
Fig. 3 is a surface topography of the wood-based panel prepared in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below. It is to be understood that the described embodiments are only some of the embodiments of the present invention. Rather than 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.
Example 1
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesia (the activity of the light-burned magnesia is 60%), 425.23g of magnesium chloride, 1.79g of sodium silicate, 1.79g of semi-hydrated gypsum, 0.36g of alumina, 0.18g of fly ash, 0.04g of citric acid as a thickening time regulator, 0.04g of gamma-aminopropyltriethoxysilane (KH550) as a cross-linking agent and 400g of water are respectively weighed;
(2) preparing a magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; then adding light-burned magnesium oxide, aluminum chloride, fly ash, cross-linking agent KH550 and semi-hydrated gypsum in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Example 2
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) respectively weighing 500g of corn straw powder, 70.58g of light-burned magnesium oxide, 425.23g of magnesium chloride, 1.79g of sodium silicate, 1.79g of semi-hydrated gypsum, 0.36g of alumina, 0.18g of fly ash, 0.04g of citric acid serving as a thickening time regulator, 0.04g of gamma-aminopropyltriethoxysilane (KH550) serving as a crosslinking agent and 400g of water;
(2) preparing a magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; sequentially adding aluminum chloride, fly ash, a cross-linking agent KH550 and semi-hydrated gypsum, and stirring for 20min to uniformly mix the components;
(3) uniformly spreading the mixed materials in a die, prepressing for molding, demolding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s.
(4) And (3) trimming the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Example 3
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) respectively weighing 600g of poplar wood powder, 56.47g of light-burned magnesium oxide, 340.19g of magnesium chloride, 1.43g of sodium silicate, 1.43g of semi-hydrated gypsum, 0.29g of alumina, 0.14g of fly ash, 0.03g of sodium polyphosphate as a coagulation regulator, 0.03g of polyvinyl alcohol as a cross-linking agent and 320g of water;
(2) preparing a magnesium chloride solution, and adding sodium polyphosphate as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; sequentially adding aluminum chloride, fly ash, polyvinyl alcohol, sodium silicate and semi-hydrated gypsum, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 14d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Example 4
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) 600g of straw stalk powder, 56.47g of light-burned magnesium oxide, 340.19g of magnesium chloride, 1.43g of sodium silicate, 1.43g of semi-hydrated gypsum, 0.29g of alumina, 0.14g of fly ash, 0.03g of sodium polyphosphate as a coagulation regulator, 0.03g of polyvinyl alcohol as a crosslinking agent and 320g of water are respectively weighed.
(2) Preparing a magnesium chloride solution, and adding sodium polyphosphate as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; sequentially adding aluminum chloride, fly ash, polyvinyl alcohol, sodium silicate and semi-hydrated gypsum, and stirring for 20min to uniformly mix the components.
(3) Uniformly spreading the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa7200s, 10MPa 7200s and 15MPa7200 s.
(4) And (3) finishing the pressed board, and curing for 14d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Example 5
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) weighing 700g of pine wood powder, 42.35g of light-burned magnesia, 255.14g of magnesium chloride, 1.07g of sodium silicate, 1.07g of semi-hydrated gypsum, 0.21g of alumina, 0.11g of fly ash, 0.02g of citric acid as a thickening time regulator, 0.02g of polyvinyl alcohol as a cross-linking agent and 240g of water;
(2) preparing a magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; sequentially adding aluminum chloride, fly ash, polyvinyl alcohol, sodium silicate and semi-hydrated gypsum, and stirring for 40min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for molding, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa14400s, 10MPa 14400s and 15MPa14400 s;
(4) and (3) finishing the pressed board, and maintaining for 28 days under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the light flame-retardant wood base board.
Example 6
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) 7000g of pine wood powder, 423.5g of light-burned magnesia, 2551.4g of magnesium chloride, 10.7g of sodium silicate, 10.7g of semi-hydrated gypsum, 2.1g of alumina, 1.1g of fly ash, 0.2g of citric acid serving as a thickening time regulator, 0.2g of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane (KH560) serving as a crosslinking agent and 2400g of water are weighed respectively.
(2) Preparing magnesium chloride solution, and adding citric acid as a coagulation regulator; wood powder is soaked in the prepared solution to be fully wetted; sequentially adding aluminum chloride, fly ash, polyvinyl alcohol, sodium silicate and semi-hydrated gypsum, and stirring for 40min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for molding, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa14400s, 10MPa 14400s and 15MPa14400 s;
(4) and (3) finishing the pressed board, and maintaining for 28 days under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the light flame-retardant wood base board.
Example 7
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) 7000g of wheat straw powder, 423.5g of light-burned magnesium oxide, 2551.4g of magnesium chloride, 10.7g of sodium silicate, 10.7g of semi-hydrated gypsum, 2.1g of alumina, 1.1g of fly ash, 0.2g of citric acid serving as a thickening time regulator, 0.2g of polyvinyl alcohol serving as a cross-linking agent and 2400g of water are respectively weighed;
(2) preparing a magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; sequentially adding aluminum chloride, fly ash, polyvinyl alcohol, sodium silicate and semi-hydrated gypsum, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for molding, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa14400s, 10MPa 14400s and 15MPa14400 s;
(4) and (3) finishing the pressed board, and maintaining for 28 days under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the light flame-retardant wood base board.
Example 8 (no set control agent, otherwise identical to example 1)
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesia (the activity of the light-burned magnesia is 60%), 425.23g of magnesium chloride, 1.79g of sodium silicate, 1.79g of semi-hydrated gypsum, 0.36g of alumina, 0.18g of fly ash, 0.04g of gamma-aminopropyltriethoxysilane (KH550) serving as a cross-linking agent and 400g of water are respectively weighed;
(2) preparing a magnesium chloride solution; wood powder is soaked in the prepared solution to be fully wetted; then adding light-burned magnesium oxide, aluminum chloride, fly ash, cross-linking agent KH550 and semi-hydrated gypsum in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Example 9 (without crosslinker, otherwise in accordance with example 1)
The invention relates to a preparation method of a fire-retardant wood base plate, which comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesia (the activity of the light-burned magnesia is 60%), 425.23g of magnesium chloride, 1.79g of sodium silicate, 1.79g of semi-hydrated gypsum, 0.36g of alumina, 0.18g of fly ash, 0.04g of citric acid as a coagulation regulator and 400g of water are respectively weighed;
(2) preparing magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; then adding light-burned magnesium oxide, aluminum chloride, fly ash and semi-hydrated gypsum in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Comparative example 1 (without auxiliary gelling System)
A preparation method of a fire-retardant wood substrate comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesia (the activity of the light-burned magnesia is 60%), 425.23g of magnesium chloride, 0.04g of citric acid as a thickening time regulator, 0.04g of gamma-aminopropyltriethoxysilane (KH550) as a crosslinking agent and 400g of water are respectively weighed;
(2) preparing a magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; then adding the light burned magnesium oxide and the cross-linking agent KH550 in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the light flame-retardant wood base board.
Fig. 2 and fig. 3 are surface topography graphs of the wood base plates prepared in the embodiment of the invention and the comparative example 1, respectively, so that the phenomenon of surface halogen returning of the base plate prepared in the comparative example 1 is obvious.
Comparative example 2 (absence of sodium silicate in adhesive)
A preparation method of a fire-retardant wood substrate comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesia (the activity of the light-burned magnesia is 60%), 425.23g of magnesium chloride, 1.79g of semi-hydrated gypsum, 0.36g of alumina, 0.18g of fly ash, 0.04g of citric acid as a thickening time regulator, 0.04g of gamma-aminopropyltriethoxysilane (KH550) as a crosslinking agent and 400g of water are respectively weighed;
(2) preparing a magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; then adding light-burned magnesium oxide, aluminum chloride, fly ash, cross-linking agent KH550 and semi-hydrated gypsum in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed material in a die, prepressing for molding, demolding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Comparative example 3 (semi-hydrated gypsum is absent in the adhesive)
A preparation method of a fire-retardant wood substrate comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesium oxide (the activity of the light-burned magnesium oxide is 60%), 425.23g of magnesium chloride, 1.79g of sodium silicate, 0.36g of alumina, 0.18g of fly ash, 0.04g of citric acid serving as a thickening time regulator, 0.04g of gamma-aminopropyltriethoxysilane (KH550) serving as a cross-linking agent and 400g of water are respectively weighed;
(2) preparing magnesium chloride solution, and adding citric acid as a coagulation regulator; wood powder is soaked in the prepared solution to be fully wetted; then adding light-burned magnesium oxide, aluminum chloride, fly ash, cross-linking agent KH550 and fly ash in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Comparative example 4 (lack of alumina in adhesive)
A preparation method of a fire-retardant wood substrate comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesia (the activity of the light-burned magnesia is 60%), 425.23g of magnesium chloride, 1.79g of sodium silicate, 1.79g of semi-hydrated gypsum, 0.18g of fly ash, 0.04g of citric acid as a thickening time regulator, 0.04g of gamma-aminopropyltriethoxysilane (KH550) as a cross-linking agent and 400g of water are respectively weighed;
(2) preparing magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; then adding light-burned magnesium oxide, sodium silicate, fly ash, a cross-linking agent KH550 and semi-hydrated gypsum in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Comparative example 5 (lack of fly ash in adhesive)
A preparation method of a fire-retardant wood substrate comprises the following steps:
(1) 500g of pine wood powder, 70.58g of light-burned magnesia (the activity of the light-burned magnesia is 60%), 425.23g of magnesium chloride, 1.79g of sodium silicate, 1.79g of semi-hydrated gypsum, 0.36g of aluminum oxide, 0.04g of citric acid serving as a thickening time regulator, 0.04g of gamma-aminopropyltriethoxysilane (KH550) serving as a cross-linking agent and 400g of water are respectively weighed;
(2) preparing a magnesium chloride solution, and adding citric acid as a coagulation regulator; soaking the wood powder in the prepared solution to fully wet the wood powder; then adding light-burned magnesium oxide, aluminum chloride, sodium silicate, a cross-linking agent KH550 and semi-hydrated gypsum in sequence, and stirring for 20min to uniformly mix the components;
(3) uniformly paving the mixed materials in a mould, prepressing for forming, demoulding, and then placing on a hot press for pressing, wherein the set temperature is 35 ℃, and the multistage pressure is set to be 5MPa3600s, 10MPa 3600s and 15MPa3600 s;
(4) and (3) finishing the pressed board, and curing for 7d under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 60 +/-2 ℃ to obtain the flame-retardant wood base board.
Performance testing
The performance of the fire-retardant wood-based boards prepared in the examples and comparative examples was tested, and the test results are shown in table 1.
Table 1 performance test results of fire-retardant wood base board
As can be seen from the data in table 1, compared with the absence of the auxiliary gelling system component in comparative example 1, the addition of the auxiliary gelling system in the embodiment of the present invention improves the early mechanical properties of the wood substrate; the adhesive adopted in the comparative example 2 is free of sodium silicate, the adhesive adopted in the comparative example 3 is free of semi-hydrated gypsum, the adhesive adopted in the comparative example 4 is free of aluminum oxide, the adhesive adopted in the comparative example 5 is free of fly ash, and the semi-hydrated gypsum can shorten the setting time of a magnesium oxychloride gelling system and can react with the sodium silicate and the fly ash to generate calcium silicate and dicalcium silicate, so that the early mechanical strength of the wood substrate is improved; the active silicon dioxide component in the fly ash can react with the active magnesium oxide to generate high-temperature-resistant magnesium silicate, so that the adhesive effect is achieved, and the fire resistance of the sample plate is improved; the aluminum oxide can react with water to generate aluminum hydroxide, and plays a role in flocculent adhesion; under the condition of water, the sodium silicate can react with unreacted active magnesium oxide and semi-hydrated gypsum to respectively generate magnesium silicate and calcium silicate, so that the mechanical property and the high-temperature resistance of an inorganic gelling system are improved. Compared with the examples, it can be found that several auxiliary colloids need to be added simultaneously, and the technical effects of the invention can be achieved by the synergistic effect of the auxiliary colloids.
The addition of the coagulation regulator can improve the coagulation time of an inorganic gelling system and improve the early strength of the wood substrate; the binding capacity of an inorganic gelling system and wood fibers can be improved by adding the cross-linking agent, and the mechanical property of the wood substrate is improved; examples 8 and 9, which do not contain a set control agent and a crosslinking agent, respectively, have lower static bending strength and elastic modulus than the other examples.
Because the mechanical property of the board is related to the wood raw material, the material performance of gramineous plants such as straws is generally considered to be inferior to that of wood, so the performance of the sample board made of rice straws and wheat straws is slightly poor; therefore, the mechanical properties of examples 2, 4 and 7 are inferior with the same composition; and the density has a significant effect on the mechanical properties of the prototype.
The curing time has a large influence on the inorganic adhesive in the plate, the curing time is long, crystals grow sufficiently, and the mechanical properties of the plate are greatly improved (7d, 14d and 28 d).
Claims (12)
1. A composite adhesive is characterized in that: the raw material components comprise light calcined magnesium oxide, magnesium chloride, sodium silicate, semi-hydrated gypsum, fly ash and aluminum oxide;
the content of active magnesium oxide in the light-burned magnesium oxide is more than 60 percent;
the molar ratio of the magnesium chloride to the active magnesium oxide in the light-burned magnesium oxide is 5-8: 1;
the content of the sodium silicate is 5 to 10 percent of the mass of the active magnesium oxide in the light-burned magnesium oxide;
the content of the semi-hydrated gypsum is 10 to 20 percent of the mass of active magnesium oxide in the light calcined magnesium oxide;
the content of the fly ash is 0.5 to 2 percent of the mass of the active magnesium oxide in the light-burned magnesium oxide;
the content of the aluminum oxide is 1 to 5 percent of the mass of the active magnesium oxide in the light-burned magnesium oxide.
2. The composite adhesive according to claim 1, further comprising a set control agent, wherein the set control agent is 0.1-2% of the mass of the active magnesium oxide in the light-burned magnesium oxide.
3. The composite adhesive according to claim 1, further comprising a crosslinking agent, wherein the content of the crosslinking agent is 0.1-2% of the mass of the active magnesium oxide in the lightly calcined magnesium oxide.
4. The composite adhesive of claim 2, wherein the set control agent is a mixture of at least one of citric acid, malic acid, phosphoric acid and sodium polyphosphate.
5. The adhesive composition according to claim 3, wherein the cross-linking agent is selected from the group consisting of polyvinyl alcohol, gamma-aminopropyltriethoxysilane (KH550), gamma- (2, 3-glycidoxy) propyltrimethoxysilane (KH 560).
6. The composite adhesive according to claim 1, wherein the light calcined magnesia has a fineness of 50 to 300 mesh.
7. The flame-retardant wood substrate prepared by the composite adhesive of any one of claims 1 to 6 is characterized in that a material uniformly mixed by the composite adhesive, wood flour and water is subjected to pre-pressing forming, multi-stage mould pressing and hot pressing forming and then curing to obtain the flame-retardant wood substrate;
the mass ratio of the composite adhesive to the wood powder to the water is 30-70: 70-30: 24 to 63;
the wood powder is organic matter which has a grain size not larger than 2mm and takes wood fiber as a main component, and the water content of the wood powder is not larger than 5%.
8. The fire-retardant wood-based panel according to claim 7, wherein the wood flour is made of wood, straw, rice hull or husk powder.
9. The fire resistant wood substrate of claim 7, wherein the wood flour has a particle size of not greater than 0.5 mm.
10. The fire-retardant wood-based panel according to claim 7 wherein the multi-stage pressing is performed by pre-pressing the material in a mold, and then performing multi-stage pressure boosting.
11. The process for preparing a fire resistant wood based panel according to any one of claims 7 to 10, comprising the steps of:
(1) weighing raw material components of the composite adhesive, namely magnesium chloride, light burned magnesium oxide, sodium silicate, semi-hydrated gypsum, fly ash, alumina, a thickening time control agent and a cross-linking agent in sequence, and weighing wood flour and water;
(2) mixing magnesium chloride with water to prepare a magnesium chloride solution, and then adding a coagulation regulator to obtain a mixed solution of the coagulation regulator and the magnesium chloride;
(3) fully soaking the dried wood powder by adopting the mixed solution of the thickening time control agent and magnesium chloride, and then uniformly stirring the light-burned magnesium oxide, aluminum oxide, sodium silicate, semi-hydrated gypsum, fly ash and a cross-linking agent with the soaked wood powder;
(4) uniformly paving the uniformly stirred materials in the step (3) in a mould for prepressing molding, and then carrying out multi-stage mould pressing and hot press setting to obtain an uncured wood substrate;
(5) and (5) curing the uncured wood base plate obtained in the step (4) for a period of time under the conditions of constant temperature and constant humidity, and then curing at room temperature to obtain the flame-retardant wood composite plate.
12. The process according to claim 11, wherein the pre-press molding operation in step (3) is performed under normal temperature and pressure, and the hot press-setting process operation is performed under conditions of: the temperature is 35 +/-2 ℃, the unit pressure is 5-17 MPa, and the pressing time is 3-12 h;
the constant temperature and humidity condition in the step (4) is as follows: the temperature is 20 +/-2 ℃, the humidity is 60 +/-2% RH, and the curing time is 7-28 days.
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