CN113910388A - Preparation method of efficient flame-retardant coating on wood surface based on metal ion crosslinking modification - Google Patents
Preparation method of efficient flame-retardant coating on wood surface based on metal ion crosslinking modification Download PDFInfo
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- CN113910388A CN113910388A CN202111037959.9A CN202111037959A CN113910388A CN 113910388 A CN113910388 A CN 113910388A CN 202111037959 A CN202111037959 A CN 202111037959A CN 113910388 A CN113910388 A CN 113910388A
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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
- B27K3/34—Organic impregnating agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/16—Inorganic impregnating agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/04—Combined bleaching or impregnating and drying of wood
-
- 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
Abstract
The invention discloses a preparation method of a high-efficiency flame-retardant coating on a wood surface based on metal ion crosslinking modification, and belongs to the technical field of wood flame-retardant modification. Firstly, pretreating the surface of wood to obtain wood with activated surface; preparing a polyethyleneimine solution and an ammonium polyphosphate suspension, performing layer-by-layer assembly modification on the surface of the wood by using the positive and negative charge solution/suspension, and drying; finally, the modified wood is put into a salt solution containing metal ions for soaking, washed by deionized water and dried. According to the invention, the polyethyleneimine-ammonium polyphosphate coating is crosslinked by metal ions, so that the bonding strength is enhanced, the durability of the coating is improved, the coating has the effect of promoting the catalytic formation of carbon, the air isolation is facilitated, the heat transfer is hindered, the flame retardant efficiency is improved, the efficient and lasting flame retardant of wood is further realized, and the method is simple, strong in operability and good in application prospect.
Description
Technical Field
The invention belongs to the technical field of wood flame-retardant modification, and particularly relates to a preparation method of a high-efficiency flame-retardant coating on the surface of wood based on metal ion crosslinking modification.
Background
The wood has the advantages of light weight, high strength, beautiful texture, easy processing, humidity regulation, good environmental characteristics and the like, and is a common material for furniture, interior decoration and buildings. But the wood has the defects of poor fire resistance, easy combustion and the like, and is very easy to cause fire to cause economic loss and casualties. Therefore, the flame retardant treatment of the wood can effectively avoid the fire, and the method has practical significance.
The method for constructing the flame-retardant coating on the surface of an object by adopting a layer-by-layer self-assembly method is a method for effectively endowing the flame-retardant property to a substrate, and is widely used for the flame-retardant treatment of cotton fabrics. The method has the advantages of simple operation, small dosage, low cost and the like. Thus, the technique can be applied to the construction of flame retardant coatings on wood surfaces. Ammonium polyphosphate (APP) has the advantages of low cost, wide sources and the like, the solution becomes negative charge, the APP is a common wood flame retardant, the APP is commonly used for wood impregnation treatment to improve the wood flame retardance, but the APP has the defects of large addition amount, easy loss and the like in the use process; polyethyleneimine (PEI) is a high molecular polymer with high nitrogen content, has good flame retardance and self-extinguishing property, and has positive charge in aqueous solution. The flame-retardant coating is constructed by combining the wood and the coating through a layer-by-layer self-assembly technology, and is expected to have a good flame-retardant effect. In the patent CN 111764154A, PEI and APP are utilized to construct a flame-retardant coating on the surface of a ramie plant by a layer-by-layer self-assembly method, and certain flame-retardant property is endowed to a ramie fabric; the patent CN 105755836B introduces zirconium phosphate (ZrP) on the basis of the flame retardant, and further improves the flame retardant effect. However, the flame-retardant coating constructed by only using the polyelectrolyte still has the defects of poor water resistance and durability, low flame-retardant efficiency and the like, and the application of the PEI-APP coating on the surface of wood is not seen.
The metal ions have better gridding effect on the charged high molecular compound, can obviously promote the catalytic carbon formation in the organic compound burning process, and improve the flame retardant efficiency to a certain extent. In patent CN 110065118A, ammonium polyphosphate is chelated with metal salt to form a stable solution of a polymer chelate, and wood is subjected to impregnation treatment to improve the flame retardant property of the wood, but the medicament impregnation weight gain rate is as high as 22% -35%, and the cost is high; in patent CN 102152359B, nitrogen phosphorus boron flame retardant is mixed with silicon, transition metal salt chelate or rare earth metal salt chelate in a multi-element way, and the bamboo material is modified by multi-element chelation synergistic effect, but the formula and the process are complex, the drug loading rate is still as high as 8%, and the flame retardant effect is not obviously improved.
Therefore, in conclusion, the APP and the PEI are used as raw materials to construct the flame-retardant coating on the surface of the wood through a layer-by-layer self-assembly coating method, and the metal salt ions are used for further chelating and crosslinking the constructed coating, so that the using amount of the flame retardant can be reduced, the cost is greatly saved, the flame-retardant efficiency of the wood and the durability of the flame-retardant coating can be improved, and the efficient and durable flame retardance of the wood can be realized.
Disclosure of Invention
The invention aims to provide a preparation method of a wood surface layer-by-layer self-assembled flame-retardant coating based on metal ion crosslinking modification. According to the method, firstly, a flame-retardant coating is constructed on the surface of the wood by a layer-by-layer self-assembly method through polyethyleneimine and ammonium polyphosphate polyelectrolyte solution, and then impregnation post-treatment is carried out through a metal salt solution, so that the durability and high-efficiency flame retardance of the coating are realized, the long-term high-efficiency flame retardance of the wood is further realized, and the method is simple, strong in operability and good in application prospect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a high-efficiency flame-retardant coating based on metal ion crosslinking modification on a wood surface comprises the following steps:
(1) wood surface pretreatment to obtain surface activated wood;
(2) preparing a polyethyleneimine solution with the mass fraction of 0.5% -2% and an ammonium polyphosphate suspension with the mass fraction of 0.5% -2%;
(3) layer-by-layer assembly modification of the wood surface:
sequentially immersing the activated wood into a polyethyleneimine solution with positive charges and an ammonium polyphosphate suspension with negative charges for alternate layer-by-layer assembly, and drying;
(4) and (3) soaking the modified wood in 0.5-5mol/L of a salt solution containing metal ions, washing with deionized water, and drying to obtain the ionic crosslinking type long-term efficient flame-retardant wood.
Preferably, in the step (1), the surface of the wood is subjected to impregnation pretreatment by using an alkaline solution, wherein the impregnation temperature is 70 ℃, and the impregnation time is 10-60 min; after the dipping treatment, the wood is washed until the wood is neutral and dried. Preferably, the alkaline solution is 0.1-1mol/L sodium hydroxide solution, and the wood after the impregnation pretreatment is dried at 70 ℃.
Preferably, the molecular weight of the polyethyleneimine is 1800-70000, preferably 1800, 10000, 70000.
Preferably, the polymerization degree of the ammonium polyphosphate is more than 1000.
Preferably, the pH of the ammonium polyphosphate suspension in the step (1) is adjusted to 5-10.
Preferably, the metal ions in the metal ion-containing salt solution are selected from one or more of calcium ions, magnesium ions, copper ions, barium ions, manganese ions, cobalt ions, iron ions and aluminum ions. More preferably, any of calcium ion, copper ion, cobalt ion, and manganese ion.
Preferably, when the impregnation is carried out in the step (3) layer by layer, the impregnation time is 10-60min, and the cleaning and drying are required after each impregnation. Preferably, the drying temperature is 103 ℃. More preferably, the wood after being activated and dried in the step (1) is soaked in the polyethyleneimine solution for 10-60min, the unadsorbed polyethyleneimine solution is washed away by deionized water, and the wood is dried in an oven at 70 ℃ for 5 min; secondly, soaking the wood in ammonium polyphosphate suspension for 10-60min, flushing unadsorbed polyethyleneimine solution with deionized water, and drying in a 70 ℃ oven for 5 min; and step III, repeating the step III to obtain the polyethyleneimine-ammonium polyphosphate coating, and drying in a 70 ℃ oven for 10 min.
Preferably, the number of times of the cycle assembly of the layer-by-layer assembly is 1 to 10 times.
Preferably, in step (4), the solution is soaked in a salt solution containing metal ions for 30-120min, then washed clean by deionized water, and dried in an oven at 103 ℃ to be completely dry.
Compared with the prior art, the invention has the following remarkable advantages and beneficial effects:
(1) according to the invention, through the combination of a polyethyleneimine-ammonium polyphosphate layer-by-layer self-assembly technology and a metal ion crosslinking technology, firstly, a flame-retardant coating is constructed on the surface of wood by using the negative and positive polyelectrolytes with flame retardance, and then, by utilizing the characteristic that metal ions have a chelating action on charged high molecular compounds, the negative and positive biomass electrolytes coating fibers are subjected to ion crosslinking.
(2) The polymer (ammonium polyphosphate and polyethyleneimine) and the metal salt used in the invention are environment-friendly, low in cost, non-toxic and safe, and are an environment-friendly wood surface modification method.
(3) According to the invention, the polyethyleneimine-ammonium polyphosphate coating is crosslinked by metal ions, so that the durability of the coating is improved, and the effect of promoting the coating to be catalyzed into carbon is also achieved, thereby being beneficial to isolating air, hindering heat transfer and improving flame retardant efficiency. Compared with unmodified wood, the wood oxygen index (LOI) after the ionic crosslinking modification can reach 47 to the maximum, and is improved by 27 percent compared with the unmodified wood (LOI 37), and is improved by nearly 1 time compared with the pure wood oxygen index (LOI 24); after 24 hours of soaking test, the oxygen index of the cross-linked modified wood is still as high as 42, and the cross-linked modified wood has excellent durability and flame retardant effect, so that the invention has good application prospect.
Detailed Description
The following examples are provided to more clearly illustrate the technical solutions of the present invention, but are not intended to limit the scope of the present invention.
Example 1
(1) Soaking the wood in 1mol/L sodium hydroxide solution for surface activation treatment at 70 ℃ for 60min, soaking the wood in deionized water, washing the wood until the wood is neutral, and finally drying the wood at 70 ℃ to obtain the surface-activated wood;
(2) adding a proper amount of polyethyleneimine with the molecular weight of 10000 into deionized water, and uniformly stirring to obtain a polyethyleneimine solution with the mass fraction of 1%;
(3) adding a proper amount of ammonium polyphosphate with polymerization degree of more than 1000 into deionized water, stirring, performing ultrasonic treatment for 60min, and adjusting the pH to 10 to obtain an ammonium polyphosphate suspension with mass fraction of 1%;
(4) soaking the wood subjected to activation treatment and drying in the step (1) in a 1% polyethyleneimine solution for 30min, flushing unadsorbed polyethyleneimine solution with deionized water, and drying in an oven at 70 ℃ for 5 min; secondly, soaking the wood in ammonium polyphosphate suspension for 30min, flushing unadsorbed polyethyleneimine solution by using deionized water, and drying in a 70 ℃ oven for 5 min; and thirdly, repeating the first step and the second step for 15 times to obtain 15 layers of modified wood with the polyethyleneimine-ammonium polyphosphate composite coating, and drying the modified wood in a drying oven at 103 ℃ until the flame-retardant wood is completely dried.
According to the standard of GB/T2406-2008 'determination of combustion behavior by oxygen index method for plastics', the prepared modified wood is subjected to oxygen index determination, and the LOI is 37; LOI was 28 after 24 hour run-off experiment.
Example 2
(1) Soaking the wood in 1mol/L sodium hydroxide solution for surface activation treatment at 70 ℃ for 60min, soaking the wood in deionized water, washing the wood until the wood is neutral, and finally drying the wood at 70 ℃ to obtain the surface-activated wood;
(2) adding a proper amount of polyethyleneimine with the molecular weight of 10000 into deionized water, and uniformly stirring to obtain a polyethyleneimine solution with the mass fraction of 1%;
(3) adding a proper amount of ammonium polyphosphate with polymerization degree of more than 1000 into deionized water, stirring, performing ultrasonic treatment for 60min, and adjusting the pH to 10 to obtain an ammonium polyphosphate suspension with mass fraction of 1%;
(4) weighing a proper amount of copper sulfate, adding the copper sulfate into deionized water, and stirring to completely dissolve the copper sulfate to obtain a copper ion-containing salt solution with the concentration of 1 mol/L;
(5) soaking the wood subjected to activation treatment and drying in the step (1) in a 1% polyethyleneimine solution for 30min, flushing unadsorbed polyethyleneimine solution with deionized water, and drying in an oven at 70 ℃ for 5 min; secondly, soaking the wood in ammonium polyphosphate suspension for 30min, flushing unadsorbed polyethyleneimine solution by using deionized water, and drying in a 70 ℃ oven for 5 min; thirdly, repeating the first step and the second step for 15 times to obtain 15 layers of modified wood with the polyethyleneimine-ammonium polyphosphate composite coating, and drying the modified wood in a drying oven at 70 ℃ for 10 min;
(6) and (3) soaking the modified wood in the step (5) in the prepared copper-containing ionic salt solution in the step (4) for 60min, then washing the wood clean by using deionized water, and drying the wood in a drying oven at 103 ℃ to be completely dry to obtain the ion-crosslinked long-term efficient flame-retardant wood.
According to the standard of GB/T2406-2008 'determination of combustion behavior by oxygen index method for plastics', the prepared modified wood is subjected to oxygen index determination, and the LOI is 47; LOI was 42 after 24 hour run-off experiment.
Example 3
(1) Soaking the wood in 1mol/L sodium hydroxide solution for surface activation treatment at 70 ℃ for 60min, soaking the wood in deionized water, washing the wood until the wood is neutral, and finally drying the wood at 70 ℃ to obtain the surface-activated wood;
(2) adding a proper amount of polyethyleneimine with the molecular weight of 70000 into deionized water, and uniformly stirring to obtain a polyethyleneimine solution with the mass fraction of 0.5%;
(3) adding a proper amount of ammonium polyphosphate with polymerization degree of more than 1000 into deionized water, stirring, performing ultrasonic treatment for 30min, and adjusting the pH to 10 to obtain an ammonium polyphosphate suspension with mass fraction of 0.5%;
(4) weighing a proper amount of cobalt acetate, adding the cobalt acetate into deionized water, and stirring to completely dissolve the cobalt acetate to obtain a cobalt ion-containing salt solution with the concentration of 5 mol/L;
(5) soaking the wood subjected to the activation treatment and drying in the step (1) in a 0.5% polyethyleneimine solution for 10min, flushing unadsorbed polyethyleneimine solution with deionized water, and drying in a 70 ℃ oven for 5 min; secondly, soaking the wood in ammonium polyphosphate suspension for 10min, flushing unadsorbed polyethyleneimine solution by using deionized water, and drying in a 70 ℃ oven for 15 min; repeating the first step and the second step for 10 times to obtain 10 layers of modified wood with the polyethyleneimine-ammonium polyphosphate composite coating, and drying in a 70 ℃ oven for 10 min;
(6) and (3) soaking the wood modified in the step (5) in the prepared cobalt ion salt-containing solution in the step (4) for 30min, then washing the wood with deionized water, and drying the wood in a drying oven at 103 ℃ until the wood is completely dried, so that the ion-crosslinked long-term efficient flame-retardant wood is obtained.
According to the standard of GB/T2406-2008 'determination of combustion behavior by oxygen index method for plastics', the prepared modified wood is subjected to oxygen index determination, and the LOI is 43; LOI after 24 hours run-off experiment was 39.
Example 4
(1) Soaking the wood in 2mol/L sodium hydroxide solution at 70 ℃ for 60min for surface activation treatment, soaking the wood in deionized water, washing the wood until the wood is neutral, and finally drying the wood at 70 ℃ to obtain the surface-activated wood;
(2) adding a proper amount of polyethyleneimine with the molecular weight of 1800 into deionized water, and uniformly stirring to obtain a polyethyleneimine solution with the mass fraction of 2%;
(3) adding a proper amount of ammonium polyphosphate with polymerization degree of more than 1000 into deionized water, stirring, performing ultrasonic treatment for 60min, and adjusting the pH to 10 to obtain an ammonium polyphosphate suspension with mass fraction of 2%;
(4) weighing a proper amount of manganese chloride, adding the manganese chloride into deionized water, and stirring to completely dissolve the manganese chloride to obtain a manganese ion-containing salt solution with the concentration of 2.5 mol/L;
(5) soaking the wood subjected to the activation treatment and drying in the step (1) in a 2% polyethyleneimine solution for 20min, flushing unadsorbed polyethyleneimine solution with deionized water, and drying in an oven at 70 ℃ for 5 min; secondly, soaking the wood in ammonium polyphosphate suspension for 20min, washing off unadsorbed polyethyleneimine solution by using deionized water, and drying for 15min in a 70 ℃ oven; thirdly, repeating the first step and the second step for 15 times to obtain 15 layers of modified wood with the polyethyleneimine-ammonium polyphosphate composite coating, and drying the modified wood in a drying oven at 70 ℃ for 10 min;
(6) and (3) soaking the modified wood in the step (5) in the manganese ion-containing salt solution prepared in the step (4) for 90min, then washing the wood clean by using deionized water, and drying the wood in a drying oven at 103 ℃ to be completely dry to obtain the ion-crosslinked long-term efficient flame-retardant wood.
According to the standard of GB/T2406-2008 'determination of combustion behavior by oxygen index method for plastics', the prepared modified wood is subjected to oxygen index determination, and the LOI is 35; LOI after 24 hours run-off experiment was 29.
The experimental results of the above embodiments show that the flame retardant effect of wood can be greatly improved and the durability of the coating can be obviously improved by crosslinking the polyethyleneimine-ammonium polyphosphate coating with metal ions, and the modification method is environment-friendly, simple, easy to operate, strong in practicability and good in application prospect.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a high-efficiency flame-retardant coating based on metal ion crosslinking modification on a wood surface is characterized by comprising the following steps:
(1) wood surface pretreatment to obtain surface activated wood;
(2) preparing a polyethyleneimine solution with the mass fraction of 0.5% -2% and an ammonium polyphosphate suspension with the mass fraction of 0.5% -2%;
(3) layer-by-layer assembly modification of the wood surface:
sequentially immersing the activated wood into a polyethyleneimine solution with positive charges and an ammonium polyphosphate suspension with negative charges for alternate layer-by-layer assembly, and drying;
(4) and (3) soaking the modified wood in 0.5-5mol/L of a salt solution containing metal ions, washing with deionized water, and drying to obtain the ionic crosslinking type long-term efficient flame-retardant wood.
2. The preparation method of the high-efficiency flame-retardant coating on the surface of the wood based on the metal ion crosslinking modification according to the claim 1, characterized in that in the step (1), the surface of the wood is subjected to dipping pretreatment by using an alkaline solution, wherein the dipping temperature is 70 ℃, and the dipping time is 10-60 min; after dipping treatment, washing to be neutral and drying.
3. The preparation method of the high-efficiency flame-retardant coating on the surface of the wood based on the metal ion crosslinking modification according to the claim 2, characterized in that the alkaline solution is 0.1-1mol/L sodium hydroxide solution.
4. The preparation method of the metal ion crosslinking modified wood surface efficient flame retardant coating as claimed in claim 1, wherein the molecular weight of the polyethyleneimine is 1800-70000.
5. The preparation method of the metal ion crosslinking modified wood surface efficient flame retardant coating according to claim 1, characterized in that the polymerization degree of the ammonium polyphosphate is more than 1000.
6. The preparation method of the high-efficiency flame-retardant coating on the surface of the wood based on the metal ion crosslinking modification according to the claim 1, characterized in that the pH of the ammonium polyphosphate suspension in the step (1) is adjusted to 5-10.
7. The method for preparing the efficient flame-retardant coating on the surface of the wood based on the metal ion crosslinking modification according to claim 1, wherein the metal ions in the metal ion-containing salt solution are selected from one or more of calcium ions, magnesium ions, copper ions, barium ions, manganese ions, cobalt ions, iron ions and aluminum ions.
8. The preparation method of the metal ion crosslinking modification-based high-efficiency flame-retardant coating on the surface of the wood according to the claim 1, wherein the dipping time is 10-60min during the layer-by-layer assembly dipping in the step (3), and the wood needs to be cleaned and dried after each dipping.
9. The preparation method of the metal ion crosslinking modification-based high-efficiency flame-retardant coating on the surface of the wood according to the claim 1 or 8, characterized in that the number of the layer-by-layer assembly cycles is 1-10.
10. The preparation method of the high-efficiency flame-retardant coating on the surface of the wood based on the metal ion crosslinking modification according to the claim 1, characterized in that, in the step (4), the solution containing the metal ion salt is soaked for 30-120 min.
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