CN115972328A - Preparation method of high-strength flame-retardant wood with fire early warning function - Google Patents
Preparation method of high-strength flame-retardant wood with fire early warning function Download PDFInfo
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Abstract
The invention discloses a preparation method of high-strength flame-retardant wood with a fire early warning function. The method comprises the following steps: partial delignification treatment of the wood, vacuum impregnation treatment of the treatment liquid, and densification enhancement of the impregnated wood. According to the invention, boric acid and graphene oxide are prepared into the functional mixed treatment fluid, and the boric acid is completely permeated into wood by utilizing the difference of the boric acid and the graphene oxide in the wood permeability, while the graphene oxide is mainly loaded on the surface of the wood, so that the using amount of the graphene is saved, and the cost is reduced; the flame retardant property of the wood is greatly improved by the dipping treatment of the boric acid and the graphene oxide, and the graphene oxide/boric acid layer loaded on the surface of the wood has the function of fire early warning; the mechanical strength of the wood is also obviously improved by the combined treatment of delignification and densification. The method has simple treatment process, improves the mechanical strength and the flame retardance of the wood, and has a new function of fire early warning.
Description
Technical Field
The invention relates to the field of preparation methods, in particular to a preparation method of high-strength flame-retardant wood with a fire early warning function.
Background
The wood has the characteristics of high strength-weight ratio, easiness in obtaining, easiness in processing, sustainability and the like, and is widely applied to the fields of buildings, transportation, furniture, decoration and the like. However, wood is also a flammable material, which makes it potentially fire-hazard during use. In order to reduce the fire risk, the fire retardant treatment can effectively improve the fire resistance of the wood, for example, phosphorus, halogen, nitrogen and other types of fire retardants are used. However, when a fire occurs, the requirement for safe escape is difficult to meet only by virtue of flame retardance, and an additional alarm is still needed for reminding, so that people can find the fire at the first time, and more time is provided for escape and fire extinguishment. Therefore, if the wood fire-retardant early warning function can be directly given, not only can the occurrence of fire be effectively early warned, but also the complex warning equipment can be simplified.
Graphene oxide is one of the most important derivatives of graphene, has good electrical insulation, and can be converted into highly conductive reduced graphene oxide after removing oxygen-containing groups by high-temperature treatment. Therefore, the thermal reaction characteristic of the graphene oxide is utilized, so that the graphene oxide can become an ideal material for fire early warning. However, the flame retardancy of the graphene oxide material alone is limited, and other flame retardants need to be added to improve the flame retardant performance of the wood. Therefore, the graphene oxide/boric acid mixed solution is prepared to be used as a wood flame retardant agent to endow wood with a fire early warning function and improve the flame retardance of wood. After the wood is subjected to dipping treatment by the graphene oxide/boric acid mixed solution, the boric acid with small molecular weight can completely permeate into the wood, so that the flame retardance of the wood is improved; the flake graphene oxide is large in size and mainly loaded on the surface of wood to form a graphene oxide/boric acid layer, so that the fire early warning response function can be given to the wood.
Secondly, the wood is often used as a material for building and furniture, and has certain requirements on the mechanical strength, and the mechanical property of the wood can be obviously improved through densification treatment. Therefore, the mechanical strength of the wood is improved by delignification and densification treatment, and the high-strength flame-retardant wood with the fire early warning function can be prepared. The method can effectively expand the application range of the wood, such as the fields of intelligent buildings, intelligent home furnishing and the like, and has important significance for promoting high added value utilization of the wood.
Therefore, a preparation method of the high-strength flame-retardant wood with the fire early warning function is provided for solving the problems.
Disclosure of Invention
The invention aims to provide a preparation method of high-strength flame-retardant wood with a fire early warning function, the wood with the fire early warning function realizes integration of light weight, high strength, flame retardance and fire early warning, and has important significance for expanding high added value utilization of wood.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of high-strength flame-retardant wood with a fire early warning function comprises the following steps:
(1) Wood delignification treatment: soaking the wood in a sodium chlorite solution at 60-100 ℃ for delignification treatment, wherein the treatment time is 4-24 hours (the treatment time is correspondingly adjusted according to the difference of the wood thickness). The treated wood was washed 3 times with deionized water and ethanol, respectively, to remove residual chemicals. And finally, freeze-drying for 48 hours to obtain the delignified wood.
(2) Uniformly dispersing boric acid and graphene oxide in deionized water together, wherein the mass fraction of the boric acid is 1.5-7.5%, and the concentration of the graphene oxide dispersion liquid is 4-10 mg/mL, soaking delignified wood in a graphene oxide/boric acid mixed treatment liquid in a vacuum environment, wherein only single boric acid can completely permeate into the wood in the mixed treatment liquid, and the graphene oxide/boric acid mixture is mainly loaded on the surface of the wood to form a flame-retardant early warning coating.
(3) Drying the impregnated wood in an oven at 40-80 ℃ for 4-12 hours, and evaporating the excessive water.
(4) In order to enhance the flame retardant and early warning functions of the wood, the boric acid/graphene mixed solution can be continuously coated on the surface of the dried treated material, and then the treated material is dried, so that the method can be circulated for many times.
(5) And (3) putting the wood under a hot press along the radial direction for densification hot pressing treatment, wherein the hot pressing temperature is 60-100 ℃, the pressure is 5-10 MPa, and the time is 4-8 hours, and after the hot pressing is finished, the high-strength flame-retardant wood with the fire early warning function is obtained.
Optionally, the sodium chlorite solution in the step (1) has a mass fraction of 2% -8% and a pH value of 4.4-5.0.
Optionally, the treatment temperature in the step (1) is 60-100 ℃, and the treatment time is 4-24 hours.
Optionally, in the step (2), the vacuum pressure is-0.1-0.04 MPa, and the impregnation time is 6-12 hours.
Optionally, the drying temperature of the wood after the dipping treatment in the step (3) is 40-80 ℃, and the drying time is 4-12 hours.
Optionally, the flame-retardant early warning coating in the step (4) is the same as the solution in the step (2), and is a mixed solution of 1.5-7.5% of boric acid and 4-10 mg/mL of graphene oxide.
Optionally, in the step (5), the hot pressing temperature is 60-100 ℃, the pressure is 5-10 MPa, the time is 4-8 hours, and the compression rate is controlled to be 30-60%.
The preparation method of the high-strength flame-retardant wood with the fire early warning function provided by the invention realizes the high strength, flame retardance and fire early warning multiple performances of the wood through simple treatment, expands the high added value utilization of the wood, and has the following specific advantages:
1. the method adopts the graphene oxide/boric acid mixed treatment liquid to carry out impregnation treatment on the wood, and skillfully utilizes the permeability selectivity of the pore structure of the wood to medicaments with different sizes and different molecular weights. In the vacuum impregnation treatment process, the boric acid with small molecular weight can completely permeate into the wood, so that the flame retardance of the wood is comprehensively improved; and the flake graphene oxide with larger size is mainly loaded on the surface of the wood to form a graphene oxide/boric acid layer, so that the fire disaster early warning effect is achieved, the using amount of the graphene oxide is saved, and the cost is reduced.
2. On the other hand, the method is also obviously different from other fire early warning coatings which are only coated on the surface of the material, and the micromolecule boric acid in the graphene oxide/boric acid mixed treatment liquid can completely permeate into the wood, so that the wood can obtain higher flame retardance. Meanwhile, the boric acid molecules on the surface of the wood also improve the flame retardance of the graphene oxide, and the response time of fire early warning is prolonged.
3. The method not only endows the wood with the function of fire early warning, but also improves the fire resistance of the wood; meanwhile, delignification and densification treatment are combined, so that the mechanical strength of the wood is improved; the method obviously improves the added value of the wood and greatly expands the application field of the wood.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the description of the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without inventive labor.
Fig. 1 is a photograph of a high-strength fire-retardant wood having a fire early warning function obtained in example 1.
Fig. 2 is a graph showing response time of wood having a fire early warning function prepared in example 1 of the present invention and example 6.
FIG. 3 is a graph comparing the heat release rates of example 1, comparative example 1 and comparative example 2.
Fig. 4 is a graph comparing the total heat release of example 1, comparative example 1 and comparative example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The wood used in the present invention may be hardwood or softwood, such as poplar, radiata pine, and cedar.
Example 1
A preparation method of high-strength flame-retardant wood with a fire early warning function comprises the following steps:
(1) A balsawood sample having a thickness of 8mm was treated by immersing it in a sodium chlorite solution (7.5% by mass, pH about 4.6, temperature 80 ℃) for 16 hours, and then subjected to partial delignification. Then taking out the wood, washing the wood for 3 times by using deionized water and ethanol respectively, and removing residual chemical substances. Finally, freeze-drying for 48 hours to obtain delignified wood;
(2) Soaking the delignified wood in a uniformly dispersed graphene oxide/boric acid mixed solution (the mass concentration of boric acid is 5 percent, and the concentration of graphene oxide is 5 mg/mL) for soaking treatment, vacuumizing to-0.1 MPa in a vacuum drying oven, and keeping for 12 hours to ensure that the boric acid in the solution completely permeates into the wood, and the graphene oxide is mainly loaded on the surface of the wood;
(3) Taking out a wood sample, drying in an oven at 60 ℃ for 4 hours, uniformly spraying a graphene oxide/boric acid solution on the surface of the wood, and then drying in the oven at 60 ℃ for 20 minutes; the process of coating and drying was repeated 5 times;
(4) And (3) placing the impregnated wood test under a hot press along the radial direction for densification treatment, wherein the hot pressing temperature is 80 ℃, the pressure is 5MPa, the compression rate of the wood is controlled to be 50%, and the hot pressing time is 6 hours, so that the high-strength flame-retardant wood with the fire early warning function is obtained.
The high-strength flame-retardant wood with the fire early warning function obtained in the embodiment is called G/B-wood.
And carrying out UL-94, limited oxygen index, mechanical property, cone calorimetric test and fire early warning performance test on the prepared G/B-wood test piece. And (4) performing cone calorimeter test according to ISO5660-1 standard, and measuring ignition time, peak heat release rate and total heat release amount of the test sample in the combustion process. A 4mm thick sample was connected to a warning lamp and a dc power supply (24V) by wire and then placed 20mm above the alcohol lamp, exposed to a 40mm high alcohol lamp flame all the time, and the time to trigger response of the warning lamp, and the duration of the alarm were recorded. Specific data are shown in tables 1 and 2.
Example 2
The present embodiment is different from embodiment 1 in that: the boric acid concentration in step (2) was 6%.
Example 3
The present embodiment is different from embodiment 1 in that: the boric acid concentration in step (2) was 4.5%.
Example 4
The present embodiment is different from embodiment 1 in that: the boric acid concentration in step (2) was 3%.
Example 5
The present embodiment is different from embodiment 1 in that: the boric acid concentration in step (2) was 1.5%.
Example 6
The present embodiment is different from embodiment 1 in that: the boric acid concentration in step (2) is 0%.
Comparative example 1
In order to verify that the high-strength flame-retardant wood with the flame-retardant early warning function prepared by the invention has high-efficiency flame-retardant performance and mechanical performance, wood which is not treated is used as a comparison.
The wood of this comparative example was numbered N wood.
And sawing the untreated material into test pieces with proper sizes to perform UL-94, limit oxygen index, mechanical property and cone calorimeter tests. The cone calorimeter test was carried out according to ISO5660-1 test standard to determine the ignition time, peak heat release rate and total heat release of the untreated material. Specific data are shown in tables 1 and 2.
Comparative example 2
In order to verify that the high-strength flame-retardant wood with the flame-retardant early warning function prepared by the invention has high-efficiency flame-retardant performance, the wood subjected to delignification and densification treatment is used as a comparison.
(1) A balsawood sample having a thickness of 8mm was treated by immersing it in a sodium chlorite solution (5% by mass, pH about 4.6, temperature 80 ℃) for 16 hours, and then subjected to partial delignification. Then taking out the wood, washing with deionized water and ethanol for 3 times respectively, and removing residual chemical substances. Finally, freeze-drying for 48 hours to obtain delignified wood;
(2) And (3) putting the wood under a hot press along the thickness direction for densification treatment, wherein the hot pressing temperature is 80 ℃, the pressure is 5MPa, the compression rate of the wood is controlled to be 50%, and the time is 6 hours, so that the densified wood is obtained.
The wood obtained in this comparative example was numbered D-wood.
And sawing the prepared D-wood into test pieces with proper sizes to carry out UL-94, limit oxygen index, mechanical property and cone calorimeter tests. And (4) carrying out cone calorimeter test according to ISO5660-1 standard, and measuring the ignition time, the peak value of the heat release rate and the total heat release amount of the test piece. The specific data are shown in table 1 and table 2.
In this application, THR is the total heat release amount.
In the present application, TTI is the ignition time.
In the present application, HRR is the heat release rate and refers to the amount of heat released per unit time by combustion of the material under specified test conditions. The greater the HRR, the more heat is fed back to the material surface from combustion.
In the present application, the PHRR is the peak heat release rate and is the maximum HRR of the sample during combustion, and the greater the PHRR value, the greater the probability of occurrence of a fire hazard.
TABLE 1
TABLE 2
The above examples are merely illustrative for clarity and are not intended to limit the embodiments. But any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the scope of the claims of the present invention.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (6)
1. A preparation method of high-strength flame-retardant wood with a fire early warning function is characterized by comprising the following steps: the method comprises the following steps:
s1, wood delignification treatment: soaking the wood in a sodium chlorite solution at 60-100 ℃ for delignification treatment, wherein the treatment time is 4-24 hours (the treatment time is correspondingly adjusted according to the difference of the wood thickness). The treated wood was washed 3 times with deionized water and ethanol, respectively, to remove residual chemicals. And finally, freeze-drying for 48 hours to obtain the delignified wood.
S2, uniformly dispersing boric acid and graphene oxide in deionized water together, wherein the mass fraction of the boric acid is 1.5-7.5%, the concentration of the graphene oxide dispersion liquid is 4-10 mg/mL, soaking the delignified wood in the graphene oxide/boric acid mixed treatment liquid in a vacuum environment, wherein only single boric acid can completely permeate into the wood in the mixed treatment liquid, and the graphene oxide/boric acid mixture is mainly loaded on the surface of the wood to form a flame-retardant early warning coating.
S3, drying the impregnated wood in an oven at the temperature of 40-80 ℃ for 4-12 hours, and evaporating the excessive water.
And S4, in order to enhance the flame retardant and early warning functions of the wood, continuously coating the boric acid/graphene mixed solution on the surface of the dried treated material, and drying for multiple times.
S5, placing the wood under a hot press along the radial direction for densification hot pressing treatment, wherein the hot pressing temperature is 60-100 ℃, the pressure is 5-10 MPa, and the time is 4-8 hours, and obtaining the high-strength flame-retardant wood with the fire early warning function after the hot pressing is finished.
2. The preparation method of the high-strength flame-retardant wood with the fire early warning function according to claim 1, wherein the preparation method comprises the following steps: in the step S1, the mass fraction of the sodium chlorite solution is 2-8%, the pH value is 4.4-5.0, the treatment temperature is 60-100 ℃, and the treatment time is 4-24 hours.
3. The preparation method of the high-strength flame-retardant wood with the fire early warning function according to claim 1, wherein the preparation method comprises the following steps: in the step S2, the vacuum pressure is-0.1-0.04 MPa, and the impregnation time is 6-12 hours.
4. The preparation method of the high-strength flame-retardant wood with the fire early warning function according to claim 1, wherein the preparation method comprises the following steps: the drying temperature of the wood after the dipping treatment in the step S3 is 40-80 ℃, and the drying time is 4-12 hours.
5. The preparation method of the high-strength flame-retardant wood with the fire early warning function according to claim 1, wherein the preparation method comprises the following steps: the flame-retardant early warning coating in the step S4 is the same as the solution in the step (2), and is mixed solution of 1.5-7.5% of boric acid and 4-10 mg/mL of graphene oxide.
6. The preparation method of the high-strength flame-retardant wood with the fire early warning function according to claim 1, wherein the preparation method comprises the following steps: in the step S5, the hot pressing temperature is 60-100 ℃, the pressure is 5-10 MPa, the time is 4-8 hours, and the compression rate is controlled to be 30-60%.
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