CN113771168A - Fireproof flame-retardant solid wood board - Google Patents
Fireproof flame-retardant solid wood board Download PDFInfo
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- CN113771168A CN113771168A CN202111036082.1A CN202111036082A CN113771168A CN 113771168 A CN113771168 A CN 113771168A CN 202111036082 A CN202111036082 A CN 202111036082A CN 113771168 A CN113771168 A CN 113771168A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/0085—Thermal treatments, i.e. involving chemical modification of wood at temperatures well over 100°C
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/04—Combined bleaching or impregnating and drying of wood
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
- C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K2240/00—Purpose of the treatment
- B27K2240/30—Fireproofing
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention relates to the field of household building materials, in particular to a fireproof flame-retardant solid wood board which is obtained by processing a wood blank by a flame retardant twice and then by hot steam; the flame retardants used in the two flame retardant treatments are respectively a flame retardant A and a flame retardant B; the flame retardant A consists of the following components: organic phosphinates, melamine polyphosphates, zinc borate, ionic liquid, ammonium dihydrogen phosphate, triethanolamine and water; the flame retardant B is organic-inorganic hybrid SiO2The sol, the fireproof flame-retardant solid wood board of the invention has good mechanical property, flame retardance and smoke suppression, excellent fireproof performance, the limit oxygen index of 60,can be widely applied to the fields of household building materials and decoration and has excellent application prospect.
Description
Technical Field
The invention relates to the field of household building materials, in particular to a fireproof flame-retardant solid wood board.
Background
The wood has the unique characteristics of no toxicity, no harm, environmental protection, renewability and the like, is widely applied to buildings, furniture and interior decoration, and is closely related to our lives. However, wood which is not subjected to flame retardant treatment is flammable, and releases a large amount of heat energy during combustion, thereby accelerating the spread of fire and the intensity of fire. Therefore, in recent years, great attention has been paid to flame retardant treatment of wood in various countries throughout the world.
At present, the flame retardant treatment of the solid wood board is mainly carried out by coating or impregnating a flame retardant on the surface layer, in comparison, the adoption of the surface coating flame retardant layer not only can affect the decoration of the wood, but also has limited flame retardant effect and can not meet the flame retardant requirement, and the impregnation flame retardant treatment has the problem of how to keep the flame retardant inside the wood for a long time.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the technical problems, the invention provides a fireproof flame-retardant solid wood board.
The adopted technical scheme is as follows:
a fireproof flame-retardant solid wood board is obtained by performing flame retardant treatment twice on a wood blank and performing hot steam treatment;
the flame retardants used in the two flame retardant treatments are respectively a flame retardant A and a flame retardant B;
the flame retardant A consists of the following components:
organic phosphinates, melamine polyphosphates, zinc borate, ionic liquid, ammonium dihydrogen phosphate, triethanolamine and water;
the flame retardant B is organic-inorganic hybrid SiO2And (3) sol.
Further, the flame retardant A comprises the following components in parts by weight:
5-10 parts of organic phosphinate, 1-3 parts of melamine polyphosphate, 0.5-1 part of zinc borate, 2-5 parts of ionic liquid, 0.1-0.2 part of ammonium dihydrogen phosphate, 1-1.5 parts of triethanolamine and 120 parts of water.
Further, the flame retardant A consists of the following components in parts by weight:
6 parts of organic phosphinate, 3 parts of melamine polyphosphate, 0.5 part of zinc borate, 4 parts of ionic liquid, 0.2 part of ammonium dihydrogen phosphate, 1 part of triethanolamine and 100 parts of water.
Further, the organic phosphinate is any one of aluminum dimethylphosphinate, aluminum diethylphosphinate, aluminum dipropylphosphinate, or aluminum diisobutylphosphinate.
Further, the ionic liquid is imidazole ionic liquid.
Further, the preparation method of the ionic liquid comprises the following steps:
s1: adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 65-80 ℃ after adding, reacting for 10-15h, pouring a reaction product into ethyl acetate, stirring for 20-40min, performing suction filtration, and drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole;
s2: adding brominated 1-butyl-3-methylimidazole and a fluorine-containing compound into water, stirring for reacting for 25-40h, carrying out reduced pressure distillation to remove water, adding acetonitrile, stirring for 1-5h, carrying out suction filtration, carrying out reduced pressure distillation on filtrate to remove acetonitrile, and drying the obtained product.
Further, the fluorine-containing compound is any one of sodium fluoride, sodium trifluoroacetate, ammonium fluoroborate, sodium fluoroborate or potassium hexafluorophosphate.
Further, the organic-inorganic hybrid SiO2The preparation method of the sol comprises the following steps:
adding tetraethoxysilane and silane coupling agent into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 5-6 by using hydrochloric acid, and continuing stirring for 40-60 min.
Further, the silane coupling agent is any one of KH550, KH560 or KH 570.
The invention also provides a preparation method of the fireproof flame-retardant solid wood board, which comprises the following steps:
s1: putting the wood blank into impregnation equipment, vacuumizing the impregnation equipment to 0.01-0.02MPa, then injecting a flame retardant A, impregnating for 1-2h under vacuum and negative pressure, then emptying, pressurizing to 1-1.2MPa, continuously impregnating for 1-2h, emptying, repeatedly operating for 2-5 times, taking out the wood blank and drying at 70-80 ℃ to constant weight;
s2: placing the dried wood blank in impregnation equipment, vacuumizing the impregnation equipment to 0.02-0.04MPa, injecting a flame retardant B, impregnating for 2-4h under vacuum negative pressure, then emptying, pressurizing to 1.4-1.8MPa, continuously impregnating for 2-4h, then emptying, repeatedly operating for 2-5 times, taking out the wood blank, and drying at 70-80 ℃ to constant weight;
s3: finally, the wood blank is treated by superheated steam, the steam temperature is 120-140 ℃, and the treatment time is 40-60 min.
The invention has the beneficial effects that:
the invention provides a fireproof flame-retardant solid wood board, which is characterized in that a wood blank is subjected to flame retardant treatment twice and then subjected to hot steam treatment, wherein organic phosphinate, melamine polyphosphate, zinc borate and ammonium dihydrogen phosphate in a flame retardant A are common flame retardant components and have a certain synergistic effect, nitrogen and phosphorus elements in the flame retardant A have a plurality of oxidation states, and thermal decomposition products of the nitrogen and phosphorus elements have a strong dehydration effect to carbonize the covered surface to form a carbon film, so that the flame-retardant effect is achieved, and an expanded carbon layer and N can be generated in the combustion process2、CO2、NH3The flame retardant B is organic-inorganic hybrid SiO2The introduction of the sol and the silane coupling agent can improve the wettability of the sol, so that the sol can rapidly enter pore channels of wood, components in the flame retardant A are fixed, the loss of the components is avoided, the silane coupling agent has certain smoke abatement and flame retardant effects, volatile substances and dense smoke generated by combustion can be adsorbed during combustion, and meanwhile, Si-OH in the sol can be subjected to dehydration condensation with active groups in the wood to form Si-O-Si and Si-O-C bonds with higher bond energy and stronger bonding force, so that the mechanical property of the solid wood board is improved.
Detailed Description
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
a preparation method of a fireproof flame-retardant solid wood board comprises the following steps:
placing poplar blank (200mm multiplied by 10mm multiplied by 4mm) in impregnation equipment, vacuumizing the impregnation equipment to 0.01MPa, and then injecting a flame retardant A;
the flame retardant A comprises the following components in parts by weight:
6 parts of diethyl aluminum phosphinate, 3 parts of melamine polyphosphate, 0.5 part of zinc borate, 4 parts of ionic liquid, 0.2 part of ammonium dihydrogen phosphate, 1 part of triethanolamine and 100 parts of water.
The preparation method of the ionic liquid comprises the following steps:
adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 70 ℃ after adding, reacting for 15 hours, pouring a reaction product into ethyl acetate, stirring for 40min, performing suction filtration, drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole, adding the brominated 1-butyl-3-methylimidazole and sodium fluoride into water, stirring for reacting for 30 hours, performing reduced pressure distillation to remove water, adding acetonitrile, stirring for 2 hours, performing suction filtration, performing reduced pressure distillation on the filtrate to remove the acetonitrile, and drying the obtained product;
after finishing the injection of the flame retardant A, carrying out vacuum negative pressure impregnation for 2h, then emptying, then pressurizing to 1.2MPa, continuing to impregnate for 2h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying the mixture at 70 ℃ to constant weight;
placing the dried poplar blank material into impregnation equipment, vacuumizing the impregnation equipment to 0.04MPa, and then injecting a flame retardant B, wherein the flame retardant B is organic-inorganic hybrid SiO2The sol is prepared by the following steps:
adding tetraethoxysilane and KH-550 into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 5 by using hydrochloric acid, and continuing stirring for 40 min;
after finishing injecting the flame retardant B, carrying out vacuum negative pressure impregnation for 4h, then emptying, pressurizing to 1.5MPa, continuing to impregnate for 4h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying at 70 ℃ to constant weight;
and finally, treating the poplar blank by superheated steam at the steam temperature of 120 ℃ for 50 min.
Example 2:
a preparation method of a fireproof flame-retardant solid wood board comprises the following steps:
placing poplar blank (200mm multiplied by 10mm multiplied by 4mm) in impregnation equipment, vacuumizing the impregnation equipment to 0.015MPa, and then injecting a flame retardant A;
the flame retardant A comprises the following components in parts by weight:
10 parts of dipropyl aluminum phosphinate, 1 part of melamine polyphosphate, 0.5 part of zinc borate, 4 parts of ionic liquid, 0.1 part of ammonium dihydrogen phosphate, 1.5 parts of triethanolamine and 120 parts of water;
the preparation method of the ionic liquid comprises the following steps:
adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 65 ℃ after adding, reacting for 15 hours, pouring a reaction product into ethyl acetate, stirring for 30min, performing suction filtration, drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole, adding the brominated 1-butyl-3-methylimidazole and sodium fluoride into water, stirring for reacting for 35 hours, performing reduced pressure distillation to remove water, adding acetonitrile, stirring for 2 hours, performing suction filtration, performing reduced pressure distillation on the filtrate to remove the acetonitrile, and drying the obtained product;
after finishing the injection of the flame retardant A, carrying out vacuum negative pressure impregnation for 1h, then emptying, pressurizing to 1.2MPa, continuing to impregnate for 2h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying at 75 ℃ to constant weight;
placing the dried poplar blank material into impregnation equipment, vacuumizing the impregnation equipment to 0.04MPa, and then injecting a flame retardant B, wherein the flame retardant B is organic-inorganic hybrid SiO2The sol is prepared by the following steps:
adding tetraethoxysilane and KH-550 into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 6 by using hydrochloric acid, and continuously stirring for 60 min;
after finishing injecting the flame retardant B, carrying out vacuum negative pressure impregnation for 4h, then emptying, pressurizing to 1.8MPa, continuing to impregnate for 4h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying at 75 ℃ to constant weight;
and finally, treating the poplar blank by using superheated steam at the steam temperature of 130 ℃ for 40 min.
Example 3:
a preparation method of a fireproof flame-retardant solid wood board comprises the following steps:
placing poplar blank (200mm multiplied by 10mm multiplied by 4mm) in impregnation equipment, vacuumizing the impregnation equipment to 0.02MPa, and then injecting a flame retardant A;
the flame retardant A comprises the following components in parts by weight:
10 parts of diisobutylphosphinic acid aluminum, 3 parts of melamine polyphosphate, 1 part of zinc borate, 5 parts of ionic liquid, 0.2 part of ammonium dihydrogen phosphate, 1.5 parts of triethanolamine and 120 parts of water;
the preparation method of the ionic liquid comprises the following steps:
adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 80 ℃ after adding, reacting for 15 hours, pouring a reaction product into ethyl acetate, stirring for 40min, performing suction filtration, drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole, adding the brominated 1-butyl-3-methylimidazole and sodium fluoride into water, stirring for reacting for 40 hours, performing reduced pressure distillation to remove water, adding acetonitrile, stirring for 5 hours, performing suction filtration, performing reduced pressure distillation on the filtrate to remove acetonitrile, and drying the obtained product;
after finishing the injection of the flame retardant A, carrying out vacuum negative pressure impregnation for 2h, then emptying, then pressurizing to 1.2MPa, continuing to impregnate for 2h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying at 80 ℃ to constant weight;
placing the dried poplar blank material into impregnation equipment, vacuumizing the impregnation equipment to 0.04MPa, and then injecting a flame retardant B, wherein the flame retardant B is organic-inorganic hybrid SiO2The sol is prepared by the following steps:
adding tetraethoxysilane and KH-550 into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 6 by using hydrochloric acid, and continuously stirring for 60 min;
after finishing injecting the flame retardant B, carrying out vacuum negative pressure impregnation for 4h, then emptying, pressurizing to 1.8MPa, continuing to impregnate for 4h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying at 80 ℃ to constant weight;
and finally, treating the poplar blank by superheated steam at the steam temperature of 140 ℃ for 60 min.
Example 4:
a preparation method of a fireproof flame-retardant solid wood board comprises the following steps:
placing poplar blank (200mm multiplied by 10mm multiplied by 4mm) in impregnation equipment, vacuumizing the impregnation equipment to 0.01MPa, and then injecting a flame retardant A;
the flame retardant A comprises the following components in parts by weight:
10 parts of diethyl aluminum phosphinate, 1 part of melamine polyphosphate, 1 part of zinc borate, 2 parts of ionic liquid, 0.2 part of ammonium dihydrogen phosphate, 1 part of triethanolamine and 120 parts of water;
the preparation method of the ionic liquid comprises the following steps:
adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 65 ℃ after adding, reacting for 15 hours, pouring a reaction product into ethyl acetate, stirring for 20min, performing suction filtration, drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole, adding the brominated 1-butyl-3-methylimidazole and sodium fluoride into water, stirring for reacting for 40 hours, performing reduced pressure distillation to remove water, adding acetonitrile, stirring for 1 hour, performing suction filtration, performing reduced pressure distillation on the filtrate to remove the acetonitrile, and drying the obtained product;
after finishing the injection of the flame retardant A, carrying out vacuum negative pressure impregnation for 2h, then emptying, pressurizing to 1MPa, continuing to impregnate for 2h, then emptying, repeatedly operating for 2 times, taking out the mixture, and drying at 80 ℃ to constant weight;
placing the dried poplar blank material into impregnation equipment, vacuumizing the impregnation equipment to 0.02MPa, and then injecting a flame retardant B, wherein the flame retardant B is organic-inorganic hybrid SiO2The sol is prepared by the following steps:
adding tetraethoxysilane and KH-550 into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 6 by using hydrochloric acid, and continuing stirring for 40 min;
after finishing injecting the flame retardant B, carrying out vacuum negative pressure impregnation for 4h, then emptying, pressurizing to 1.4MPa, continuing to impregnate for 4h, then emptying, repeatedly operating for 2 times, taking out the mixture, and drying at 80 ℃ to constant weight;
and finally, treating the poplar blank by superheated steam at the steam temperature of 120 ℃ for 60 min.
Example 5:
a preparation method of a fireproof flame-retardant solid wood board comprises the following steps:
placing poplar blank (200mm multiplied by 10mm multiplied by 4mm) in impregnation equipment, vacuumizing the impregnation equipment to 0.02MPa, and then injecting a flame retardant A;
the flame retardant A comprises the following components in parts by weight:
5 parts of diethyl aluminum phosphinate, 3 parts of melamine polyphosphate, 0.5 part of zinc borate, 5 parts of ionic liquid, 0.1 part of ammonium dihydrogen phosphate, 1.5 parts of triethanolamine and 100 parts of water;
the preparation method of the ionic liquid comprises the following steps:
adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 80 ℃ after adding, reacting for 10 hours, pouring a reaction product into ethyl acetate, stirring for 40min, performing suction filtration, drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole, adding the brominated 1-butyl-3-methylimidazole and sodium trifluoroacetate into water, stirring for reacting for 25 hours, performing reduced pressure distillation to remove water, adding acetonitrile, stirring for 5 hours, performing suction filtration, performing reduced pressure distillation on the filtrate to remove the acetonitrile, and drying the obtained product;
after finishing injecting the flame retardant A, carrying out vacuum negative pressure impregnation for 1h, then emptying, pressurizing to 1.2MPa, continuing to impregnate for 1h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying at 70 ℃ to constant weight;
placing the dried poplar blank material into impregnation equipment, vacuumizing the impregnation equipment to 0.04MPa, and then injecting a flame retardant B, wherein the flame retardant B is organic-inorganic hybrid SiO2The sol is prepared by the following steps:
adding tetraethoxysilane and KH-550 into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 5 by using hydrochloric acid, and continuously stirring for 60 min;
after finishing injecting the flame retardant B, carrying out vacuum negative pressure impregnation for 2h, then emptying, pressurizing to 1.8MPa, continuing to impregnate for 2h, then emptying, repeatedly operating for 5 times, taking out the mixture, and drying at 70 ℃ to constant weight;
and finally, treating the poplar blank by superheated steam at the steam temperature of 140 ℃ for 40 min.
Example 6:
a preparation method of a fireproof flame-retardant solid wood board comprises the following steps:
placing poplar blank (200mm multiplied by 10mm multiplied by 4mm) in impregnation equipment, vacuumizing the impregnation equipment to 0.01MPa, and then injecting a flame retardant A;
the flame retardant A comprises the following components in parts by weight:
5 parts of diethyl aluminum phosphinate, 1 part of melamine polyphosphate, 0.5 part of zinc borate, 2 parts of ionic liquid, 0.1 part of ammonium dihydrogen phosphate, 1 part of triethanolamine and 100 parts of water;
the preparation method of the ionic liquid comprises the following steps:
adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 65 ℃ after adding, reacting for 10 hours, pouring a reaction product into ethyl acetate, stirring for 20min, performing suction filtration, drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole, adding the brominated 1-butyl-3-methylimidazole and sodium fluoborate into water, stirring for reacting for 25 hours, performing reduced pressure distillation to remove water, adding acetonitrile, stirring for 1 hour, performing suction filtration, performing reduced pressure distillation on the filtrate to remove acetonitrile, and drying the obtained product;
after finishing injecting the flame retardant A, carrying out vacuum negative pressure impregnation for 1h, then emptying, pressurizing to 1MPa, continuing to impregnate for 1h, then emptying, repeatedly operating for 2 times, taking out the mixture, and drying at 70 ℃ to constant weight;
placing the dried poplar blank material into impregnation equipment, vacuumizing the impregnation equipment to 0.02MPa, and then injecting a flame retardant B, wherein the flame retardant B is organic-inorganic hybrid SiO2The sol is prepared by the following steps:
adding tetraethoxysilane and KH-550 into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 5 by using hydrochloric acid, and continuing stirring for 40 min;
after finishing injecting the flame retardant B, vacuum negative pressure dipping for 2-4h, then emptying, pressurizing to 1.4MPa, continuing dipping for 2h, then emptying, repeatedly operating for 2 times, taking out the mixture, and drying at 70 ℃ to constant weight;
and finally, treating the poplar blank by superheated steam at the steam temperature of 120 ℃ for 40 min.
Comparative example 1:
comparative example 1 is substantially the same as example 1 except that the fire-retardant, fire-retardant solid wood board was not treated with the fire retardant a.
Comparative example 2:
comparative example 2 is substantially the same as example 1 except that the fire-retardant, fire-retardant solid wood board was not treated with the fire retardant B.
Comparative example 3:
comparative example 3 is substantially the same as example 1 except that the fire-retardant solid wood board was not subjected to the superheated steam treatment.
And (3) performance testing:
the mechanical properties of the real wood board samples and the blank samples (untreated poplar blanks) prepared according to the examples 1 to 6 and the comparative examples 1 to 3 of the invention are tested according to GB/T1936.2-2009 Wood bending elastic modulus determination method, GB/T1936.1-2009 Wood bending strength test method and GB/T1935-2009 Wood grain compression strength test method.
The test results are shown in table 1 below:
table 1:
secondly, according to ISO5660-1 part 1 of the reaction test of ignition, heat release, smoke yield and mass loss rate: heat release rate (cone calorimeter method) the solid wood board samples prepared according to examples 1 to 6 and comparative examples 1 to 3 of the present invention and the blank samples (untreated poplar wood blanks) were tested for their combustion parameters, i.e., ignition time, total heat release, total smoke generation.
Part 2 of the combustion behaviour was determined according to GB/T2406.2-2009 "oxygen index for plastics: room temperature test, the limiting oxygen index of the wood board samples prepared according to examples 1-6 and comparative examples 1-3 of the present invention and the blank (untreated poplar wood).
The test results are shown in table 2 below:
table 2:
as can be seen from the above tables 1 and 2, the fireproof and flame-retardant solid wood board disclosed by the invention is good in mechanical property, flame-retardant and smoke-suppression, excellent in fireproof performance, and high in limited oxygen index up to 60, can be widely applied to the fields of household building materials and decoration, and has an excellent application prospect.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A fireproof flame-retardant solid wood board is characterized in that the fireproof flame-retardant solid wood board is obtained by performing flame retardant treatment twice on a wood blank and performing hot steam treatment;
the flame retardants used in the two flame retardant treatments are respectively a flame retardant A and a flame retardant B;
the flame retardant A consists of the following components:
organic phosphinates, melamine polyphosphates, zinc borate, ionic liquid, ammonium dihydrogen phosphate, triethanolamine and water;
the flame retardant B is organic-inorganic hybrid SiO2And (3) sol.
2. A fireproof and flame-retardant solid wood board according to claim 1, wherein the flame retardant a comprises the following components in parts by weight:
5-10 parts of organic phosphinate, 1-3 parts of melamine polyphosphate, 0.5-1 part of zinc borate, 2-5 parts of ionic liquid, 0.1-0.2 part of ammonium dihydrogen phosphate, 1-1.5 parts of triethanolamine and 120 parts of water.
3. A fireproof and flame-retardant solid wood board according to claim 2, wherein the flame retardant a comprises the following components in parts by weight:
6 parts of organic phosphinate, 3 parts of melamine polyphosphate, 0.5 part of zinc borate, 4 parts of ionic liquid, 0.2 part of ammonium dihydrogen phosphate, 1 part of triethanolamine and 100 parts of water.
4. A fire-retardant solid wood board according to claim 1, wherein the organic phosphinate salt is any one of aluminum dimethylphosphinate, aluminum diethylphosphinate, aluminum dipropylphosphinate, or aluminum diisobutylphosphinate.
5. A fire-retardant solid wood board according to claim 1, wherein the ionic liquid is an imidazole-based ionic liquid.
6. A fireproof and flame-retardant solid wood board according to claim 1, wherein the ionic liquid is prepared by the following method:
s1: adding N-methylimidazole into trichloroethane, stirring and mixing uniformly, adding N-butyl bromide under ice bath, heating to 65-80 ℃ after adding, reacting for 10-15h, pouring a reaction product into ethyl acetate, stirring for 20-40min, performing suction filtration, and drying the obtained solid to obtain brominated 1-butyl-3-methylimidazole;
s2: adding brominated 1-butyl-3-methylimidazole and a fluorine-containing compound into water, stirring for reacting for 25-40h, carrying out reduced pressure distillation to remove water, adding acetonitrile, stirring for 1-5h, carrying out suction filtration, carrying out reduced pressure distillation on filtrate to remove acetonitrile, and drying the obtained product.
7. A fireproof and flame retardant solid wood board according to claim 6, wherein the fluorine containing compound is any one of sodium fluoride, sodium trifluoroacetate, ammonium fluoroborate, sodium fluoroborate or potassium hexafluorophosphate.
8. A fireproof flame-retardant solid wood board according to claim 1, wherein the organic-inorganic hybrid SiO is2The preparation method of the sol comprises the following steps:
adding tetraethoxysilane and silane coupling agent into absolute ethyl alcohol, stirring and mixing uniformly, adjusting the pH of the system to 5-6 by using hydrochloric acid, and continuing stirring for 40-60 min.
9. A fire-retardant solid wood board according to claim 8, wherein the silane coupling agent is any one of KH550, KH560 or KH 570.
10. A method for preparing a fireproof flame-retardant solid wood board as claimed in claims 1 to 9, which is characterized in that it comprises the following steps:
s1: putting the wood blank into impregnation equipment, vacuumizing the impregnation equipment to 0.01-0.02MPa, then injecting a flame retardant A, impregnating for 1-2h under vacuum and negative pressure, then emptying, pressurizing to 1-1.2MPa, continuously impregnating for 1-2h, emptying, repeatedly operating for 2-5 times, taking out the wood blank and drying at 70-80 ℃ to constant weight;
s2: placing the dried wood blank in impregnation equipment, vacuumizing the impregnation equipment to 0.02-0.04MPa, injecting a flame retardant B, impregnating for 2-4h under vacuum negative pressure, then emptying, pressurizing to 1.4-1.8MPa, continuously impregnating for 2-4h, then emptying, repeatedly operating for 2-5 times, taking out the wood blank, and drying at 70-80 ℃ to constant weight;
s3: finally, the wood blank is treated by superheated steam, the steam temperature is 120-140 ℃, and the treatment time is 40-60 min.
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