CN110127705B - Preparation method of graphene oxide modified flame-retardant silica aerogel - Google Patents
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Abstract
The invention discloses a preparation method of graphene oxide modified flame-retardant silica aerogel, which comprises the following steps: mixing a silane coupling agent, an acid catalyst, a surfactant and water, adjusting the pH to 2-5, stirring, and hydrolyzing to obtain a silica sol solution; adding an alkali catalyst into the obtained silica sol solution, stirring, adjusting the pH to 9-11, adding graphene oxide, stirring, and performing ultrasonic treatment to obtain a graphene oxide-silane mixed solution; and transferring the obtained graphene oxide-silane mixed solution into a closed container, reacting for 48-56 h at 80-90 ℃, performing solvent replacement washing, and drying at normal temperature and normal pressure to obtain the graphene oxide modified flame-retardant silica aerogel. The graphene oxide modified flame-retardant silica aerogel prepared by the preparation method disclosed by the invention is excellent in flame retardant property, and can be applied to the fields of heat insulation materials, sound absorption materials, adsorption materials and the like.
Description
Technical Field
The invention relates to the technical field of organic silicon aerogel, in particular to a preparation method of graphene oxide modified flame-retardant silicon aerogel.
Background
Since the first appearance of aerogel materials in 1931, the aerogel materials attract extensive attention in various social circles due to the unique properties of low density, high porosity, high specific surface area, low thermal conductivity and the like, and are applied to the fields of building industry, transportation, petroleum industry, aerospace, national defense and the like. Wherein, silicon aerogel is prepared into a heat insulation silica aerogel felt by scientific research personnel due to ultralow heat conductivity coefficient and excellent high and low temperature resistance, and as disclosed in the patent specification with the publication number of CN108585762A, the excellent heat insulation effect can be achieved by using a very thin material. However, the traditional preparation of silica aerogel usually requires expensive drying conditions such as supercritical drying and freeze drying, and the preparation process is complex and not suitable for large-scale production.
In order to realize preparation of silica aerogel under normal pressure, Kazuyoshi Kanamori reports an organic-inorganic polymerized silica aerogel dried under normal pressure (J.Mater.chem.,2011,21, 17077-17079), and a flexible silica aerogel with excellent mechanical properties is prepared by controlling acid and alkali to form sol-gel. In addition, the patent specification with publication number CN107523275A discloses a preparation method of a flexible silica aerogel-based phase-change composite material, in which the degree of crosslinking inside the aerogel is changed by adding trimethyl methoxysilane, so that the aerogel has flexibility, and finally a flexible aerogel with adjustable pore size is prepared. The patent specification with publication number CN108641361A discloses a preparation method of a fiber-reinforced silicone aerogel heat-insulation composite material, which comprises the steps of taking a siloxane polymer with a porous structure as a matrix, adding a flexible fiber felt, preparing a silicone solution, soaking the flexible fiber felt in the solution, and then performing sol-gel, washing and drying to finally obtain the silicone aerogel heat-insulation composite material.
However, the organic silicon aerogel and the composite material thereof prepared at normal temperature have a large amount of organic groups on silane molecules, and most of the added or modified objects are flammable materials, so that the organic silicon aerogel and the composite material thereof do not have good flame retardant property. The added or modified materials can be thermally decomposed and even burnt when meeting high temperature and flame, so that the material performance and structure of the organic silicon aerogel and the composite material thereof are seriously deteriorated, and the basic requirement on the green flame retardant performance of the materials in practical application is difficult to meet.
Disclosure of Invention
Aiming at the defects in the field, the invention provides a preparation method of graphene oxide modified flame-retardant silica aerogel, and the graphene oxide modified flame-retardant silica aerogel with the characteristics of environmental protection, light weight and high elasticity can be obtained under the normal pressure drying condition. According to the preparation method, the graphene oxide material and the micro-nano structure silicon dioxide are used for realizing synergistic flame retardance, so that the problems of flammability and the like of the traditional organic silicon aerogel and thermal insulation materials are solved. The preparation method is green and simple, can be industrialized in a large scale, and provides a new idea for developing the flame-retardant and heat-insulating organic silicon aerogel material.
A preparation method of graphene oxide modified flame-retardant silica aerogel comprises the following steps:
(1) mixing a silane coupling agent, an acid catalyst, a surfactant and water, adjusting the pH to 2-5, stirring, and hydrolyzing to obtain a silica sol solution;
(2) adding an alkali catalyst into the obtained silica sol solution, stirring, adjusting the pH to 9-11, adding graphene oxide, stirring, and performing ultrasonic treatment to obtain a graphene oxide-silane mixed solution;
(3) and transferring the obtained graphene oxide-silane mixed solution into a closed container, reacting for 48-56 h at 80-90 ℃, performing solvent replacement washing, and drying at normal temperature and normal pressure to obtain the graphene oxide modified flame-retardant silica aerogel.
According to the invention, based on the fact that the surface of graphene oxide contains a large number of hydroxyl groups, the graphene oxide can participate in silane molecule hydrolysis and condensation reaction, and a three-dimensional highly-crosslinked aerogel network structure is constructed by utilizing the chemical crosslinking effect of the graphene oxide and the silane molecule, the mechanical property of the synergistically enhanced aerogel is greatly improved, the aerogel is not easy to crack in the drying process, the skeleton can be kept complete, the powder falling phenomenon is obviously improved compared with that of pure organic silicon aerogel, and the graphene oxide bridging silane particle synergistic reinforcement structure is proved.
The assembly of the graphene oxide and the silane particles is analyzed from a microscopic angle, so that the gap diameter is reduced, the movement of gas molecules can be limited by the graphene oxide and the silane particles in a lamellar structure, the heat transfer is effectively prevented, and the heat insulation performance is further improved.
The graphene oxide cannot resist flame, the traditional organic silicon aerogel is also an inflammable material, and the graphene oxide and the traditional organic silicon aerogel are synergistically crosslinked together to construct a compact net structure, so that a good flame-retardant effect is achieved; further characterization shows that the graphene oxide can not only obstruct the transmission of air, but also effectively resist the attack of flame, and realize green flame retardance in cooperation with organic silicon molecules, thereby solving the problem that organic silicon heat-insulating aerogel can not be flame-retarded for a long time.
Preferably, in the step (1), the silane coupling agent, the acid catalyst, the surfactant and the water are added in the following amounts by weight:
more preferably, in the step (2), the addition amount of the alkali catalyst is 10-20 parts by weight, the addition amount of the graphene oxide is X parts, and X is more than 0 and less than or equal to 5. The excellent flame retardant and mechanical properties can be achieved by adding trace amount of graphene oxide under the synergistic effect.
In order to ensure the framework strength formed by the subsequent wet gel, the silane coupling agent preferably comprises trialkoxysilane and dialkoxysilane, and the mass ratio of the trialkoxysilane to the dialkoxysilane is 1.2-1.8: 1. Outside this range of content wet gels cannot be formed.
Preferably, the trialkoxysilane is selected from at least one of methyltrimethoxysilane, ethyltrimethoxysilane, methyltriethoxysilane and ethyltriethoxysilane.
Preferably, the bis-alkoxysilane is at least one selected from the group consisting of dimethyldimethoxysilane, ethyldimethoxysilane and ethyldiethoxysilane.
Preferably, the acid catalyst is at least one selected from the group consisting of acetic acid, hydrochloric acid, nitric acid and citric acid. The adding amount of the acid catalyst is measured by adjusting the pH of the silica sol solution obtained in the step (1) to 2-5.
Preferably, the surfactant is at least one selected from the group consisting of cetyltrimethylammonium bromide (CTAB), cetyltrimethylammonium chloride (CTAC), dihexadecyldimethylammonium chloride and octadecyltrimethylammonium chloride.
Preferably, the alkali catalyst is at least one selected from urea, ammonia water and tetramethylammonium hydroxide. And (3) the addition amount of the alkali catalyst is measured by adjusting the pH of the silica sol solution obtained in the step (2) to 9-11.
Preferably, the graphene oxide is micron-scale graphene oxide, and the size of the graphene oxide is 30-100 μm. The graphene oxide sheets with the size can be uniformly distributed in the gel, and the aerogel framework can be conveniently and synergistically constructed.
Preferably, in the step (2), a graphene oxide solution is added after the pH is adjusted to 9-11, and the graphene oxide solution is obtained by dissolving graphene oxide in water and then performing ultrasonic dispersion.
Preferably, in the step (3), the solvent displacement washing is carried out in two steps, the solvent used in the first step is selected from ethanol and/or isopropanol, and unreacted raw materials are washed away; and in the second step, a low-surface-tension solvent is used, at least one of n-hexane, n-heptane and n-octane is selected, the price is low, the surface energy is low, and the skeleton of the aerogel can be kept from being damaged in the normal-pressure drying process after the aerogel is washed.
In consideration of energy consumption and efficiency, it is further preferable that the solvent replacement is performed 3 to 4 times in each step of the solvent replacement washing, and the time for each solvent replacement is 6 to 10 hours. The preferred number of washes and time are such that adequate displacement can be achieved in the shortest amount of time.
The graphene oxide modified flame-retardant silica aerogel prepared by the preparation method disclosed by the invention is excellent in flame retardant property, and can be applied to the fields of heat insulation materials, sound absorption materials, adsorption materials and the like.
Compared with the prior art, the invention has the main advantages that:
(1) according to the invention, graphene oxide and organic silicon are used for flame retarding in a synergistic manner to construct a novel flame-retardant silicon aerogel material, the material is non-toxic and harmless in the preparation process, the preparation conditions are normal temperature and normal pressure, and harsh conditions such as supercritical drying and the like are not required, and the prepared material has low heat conductivity coefficient, low density, high elasticity, excellent compression performance and excellent hydrophobic performance.
(2) According to the invention, a synergetic flame-retardant system of the flaky carbon material and the silicon dioxide particles with the micro-nano structure is constructed from a microstructure, so that a new idea is provided for the silicon aerogel in the flame-retardant direction; the heat-insulating flame-retardant silica aerogel disclosed by the invention has an application prospect in the field of buildings, and can be widely used in the fields of railway traffic, petrochemical industry and the like.
Drawings
FIG. 1 is a photograph of a comparative burn experiment of a modified aerogel sample A of example 1 and an unmodified aerogel sample B of comparative example 1;
fig. 2 is a photograph showing compression recovery performance of 1.0 wt% graphene oxide-modified aerogel of example 2.
Detailed Description
The invention is further described with reference to the following drawings and specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers.
Example 1
Sequentially adding 3g of methyltrimethoxysilane, 2g of dimethyldimethoxysilane, 0.005g of acetic acid, 0.8g of CTAB (cetyl trimethyl ammonium bromide) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 5g of urea into the hydrolyzed solution, and violently stirring for 10 min; then taking 50mg of graphene oxide, adding the graphene oxide into the silica sol solution, fully stirring and carrying out ultrasonic treatment for 5 min; pouring the treated solution into a mold, sealing, placing in an oven at 80 ℃ for 48h, taking out the reacted modified silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein the replacement is carried out for 10h each time, and drying at normal temperature and normal pressure after the replacement is finished to obtain the graphene oxide modified silicon aerogel with the concentration of 2.0 wt%, which is marked as sample A. As shown in fig. 1, the alcohol burner combustion test result of sample a shows that 2.0 wt% graphene oxide modified silica aerogel can not be combusted, the alcohol burner is moved away after the graphene oxide modified silica aerogel is combusted for 5s, the sample a has a self-extinguishing effect, the framework is kept intact, the sample a is green and environment-friendly, no toxic gas is generated, and the flame retardant property is good.
Comparative example 1
Sequentially adding 3g of methyltrimethoxysilane, 2g of dimethyldimethoxysilane, 0.005g of acetic acid, 0.8g of CTAB (cetyl trimethyl ammonium bromide) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 5g of urea into the solution after hydrolysis, and stirring vigorously for 10 min; pouring the treated solution into a mold, sealing, and placing in an oven at 80 ℃ for 48 h; and then taking out the reacted silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein each solvent is replaced for 10 hours, and drying at normal temperature and normal pressure after the replacement is finished to obtain pure silicon aerogel which is marked as a sample B. As shown in FIG. 1, the alcohol burner combustion test results of sample B show that pure silica aerogel burns rapidly, the alcohol burner is removed after burning for 5s, sample B burns continuously, the skeleton is damaged, and the original appearance cannot be maintained.
Example 2
Sequentially adding 3g of methyltrimethoxysilane, 2g of dimethyldimethoxysilane, 0.005g of acetic acid, 0.8g of CTAB (cetyl trimethyl ammonium bromide) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 5g of urea into the hydrolyzed solution, and violently stirring for 10 min; then adding 25mg of graphene oxide into the silica sol solution, fully stirring and carrying out ultrasonic treatment for 5 min; pouring the treated solution into a mold, sealing, placing in an oven at 80 ℃ for 48h, taking out the reacted modified silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein each solvent is replaced for 10h each time, and drying at normal temperature and normal pressure after the replacement is finished to obtain the graphene oxide modified silicon aerogel. As shown in fig. 2, the 1.0 wt% graphene oxide modified aerogel has high elasticity and excellent compression recovery performance, so that the aerogel has a wide application prospect in the field of buildings.
Example 3
Sequentially adding 3g of methyltrimethoxysilane, 2g of dimethyldimethoxysilane, 0.005g of acetic acid, 0.6g of CTAC (cetyltrimethylammonium chloride) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 5g of urea into the hydrolyzed solution, and violently stirring for 10 min; then taking 70mg of graphene oxide, adding the graphene oxide into the silica sol solution, fully stirring and carrying out ultrasonic treatment for 5 min; pouring the treated solution into a mold, sealing, placing in an oven at 80 ℃ for 48h, taking out the reacted modified silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein each solvent is replaced for 8h, and drying at normal temperature and normal pressure after replacement is finished to obtain the graphene oxide modified silicon aerogel. Compared with the method without modified aerogel, the flame retardant effect of the graphene oxide modified aerogel is obviously improved, the structure of the graphene oxide modified aerogel can not be damaged under the flame condition, the sample is green and environment-friendly, and no toxic gas is generated.
Example 4
Sequentially adding 3g of methyltrimethoxysilane, 2g of dimethyldimethoxysilane, 0.005g of hydrochloric acid, 0.6g of CTAC (cetyltrimethylammonium chloride) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 5g of urea into the hydrolyzed solution, and violently stirring for 10 min; then taking 20mg of graphene oxide, adding the graphene oxide into the silica sol solution, fully stirring and carrying out ultrasonic treatment for 5 min; pouring the treated solution into a mold, sealing, placing in an oven at 80 ℃ for 48h, taking out the reacted modified silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein each solvent is replaced for 8h, and drying at normal temperature and normal pressure after the replacement is finished to obtain the graphene oxide modified silicon aerogel. Compared with the method without modified aerogel, the flame retardant effect of the graphene oxide modified aerogel is obviously improved, the structure of the graphene oxide modified aerogel can not be damaged under the flame condition, the sample is green and environment-friendly, and no toxic gas is generated.
Example 5
Sequentially adding 3g of ethyl trimethoxy silane, 2g of dimethyl diethoxy silane, 0.005g of nitric acid, 0.8g of CTAB (cetyl trimethyl ammonium bromide) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 3g of urea into the hydrolyzed solution, and violently stirring for 10 min; then adding 25mg of graphene oxide into the silica sol solution, fully stirring and carrying out ultrasonic treatment for 5 min; pouring the treated solution into a mold, sealing, placing in an oven at 80 ℃ for 48h, taking out the reacted modified silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein each solvent is replaced for 8h, and drying at normal temperature and normal pressure after the replacement is finished to obtain the graphene oxide modified silicon aerogel. Compared with the method without modified aerogel, the flame retardant effect of the graphene oxide modified aerogel is obviously improved, the structure of the graphene oxide modified aerogel can not be damaged under the flame condition, the sample is green and environment-friendly, and no toxic gas is generated.
Example 6
Sequentially adding 3g of methyltriethoxysilane, 2g of dimethyldiethoxysilane, 0.005g of acetic acid, 0.8g of CTAB (cetyl trimethyl ammonium bromide) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 4g of urea into the hydrolyzed solution, and violently stirring for 10 min; then taking 20mg of graphene oxide, adding the graphene oxide into the silica sol solution, fully stirring and carrying out ultrasonic treatment for 5 min; pouring the treated solution into a mold, sealing, placing in a 90 ℃ oven for 56h, taking out the reacted modified silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein each solvent is replaced for 8h each time, and drying at normal temperature and normal pressure after the replacement is finished to obtain the graphene oxide modified flame-retardant silicon aerogel. Compared with the method without modified aerogel, the flame retardant effect of the graphene oxide modified aerogel is obviously improved, the structure of the graphene oxide modified aerogel can not be damaged under the flame condition, the sample is green and environment-friendly, and no toxic gas is generated.
Example 7
Sequentially adding 3g of methyltriethoxysilane, 2g of diethyldiethoxysilane, 0.005g of acetic acid, 0.6g of CTAB (cetyl trimethyl ammonium bromide) and 15g of water into a beaker, and magnetically stirring for 30min to fully hydrolyze the silane; then adding 5g of urea into the hydrolyzed solution, and violently stirring for 10 min; then taking 20mg of graphene oxide, adding the graphene oxide into the silica sol solution, fully stirring and carrying out ultrasonic treatment for 5 min; pouring the treated solution into a mold, sealing, placing in a 90 ℃ oven for 56h, taking out the reacted modified silicon wet gel, sequentially carrying out solvent replacement in isopropanol and n-hexane for three times, wherein each solvent is replaced for 8h each time, and drying at normal temperature and normal pressure after the replacement is finished to obtain the graphene oxide modified flame-retardant silicon aerogel. Compared with the method without modified aerogel, the flame retardant effect of the graphene oxide modified aerogel is obviously improved, the structure of the graphene oxide modified aerogel can not be damaged under the flame condition, the sample is green and environment-friendly, and no toxic gas is generated.
Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the above description of the present invention, and equivalents also fall within the scope of the invention as defined by the appended claims.
Claims (6)
1. A preparation method of graphene oxide modified flame-retardant silica aerogel comprises the following steps:
(1) mixing a silane coupling agent, an acid catalyst, a surfactant and water, adjusting the pH to 2-5, stirring, and hydrolyzing to obtain a silica sol solution; the silane coupling agent comprises trialkoxysilane and dialkoxysilane in a mass ratio of 1.2-1.8: 1;
the silane coupling agent, the acid catalyst, the surfactant and the water are added in parts by weight as follows:
(2) adding an alkali catalyst into the obtained silica sol solution, stirring, adjusting the pH to 9-11, adding graphene oxide, stirring, and performing ultrasonic treatment to obtain a graphene oxide-silane mixed solution; the size of the graphene oxide is 30-100 mu m; the graphene oxide is added in X parts by weight, wherein X is more than 0 and less than or equal to 5;
(3) and transferring the obtained graphene oxide-silane mixed solution into a closed container, reacting for 48-56 h at 80-90 ℃, performing solvent replacement washing, and drying at normal temperature and normal pressure to obtain the graphene oxide modified flame-retardant silica aerogel.
2. The preparation method of the graphene oxide modified flame-retardant silica aerogel according to claim 1, wherein in the step (2), the addition amount of the alkali catalyst is 10-20 parts by weight.
3. The method of claim 1, wherein the acid catalyst is at least one selected from the group consisting of acetic acid, hydrochloric acid, nitric acid, and citric acid.
4. The method of claim 1, wherein the surfactant is at least one selected from the group consisting of cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, dihexadecyldimethylammonium chloride and octadecyltrimethylammonium chloride.
5. The method of claim 1, wherein the base catalyst is at least one selected from the group consisting of urea, ammonia, and tetramethylammonium hydroxide.
6. The method for preparing graphene oxide modified flame-retardant silica aerogel according to claim 1, wherein the solvent displacement washing is performed in two steps, and the solvent used in the first step is selected from ethanol and/or isopropanol; the second step uses a low surface tension solvent selected from at least one of n-hexane, n-heptane and n-octane.
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| CN111253615B (en) * | 2020-02-24 | 2022-06-10 | 杭州师范大学 | Super-hydrophobic organic silicon aerogel and normal-temperature normal-pressure drying preparation method and application thereof |
| CN112138612A (en) * | 2020-09-16 | 2020-12-29 | 复旦大学 | Preparation method of graphene-organic silicon composite aerogel |
| CN112744820A (en) * | 2021-01-21 | 2021-05-04 | 江苏泛亚微透科技股份有限公司 | Green preparation method of methylsilsesquioxane aerogel |
| CN112876195A (en) * | 2021-02-05 | 2021-06-01 | 东莞市道睿石墨烯研究院 | Preparation method of graphene composite silicon aerogel thermal insulation material |
| CN114050273B (en) * | 2021-10-09 | 2022-11-01 | 东风汽车集团股份有限公司 | Modified graphene oxide, composite material, GDL and preparation method thereof |
| CN114436620A (en) * | 2022-01-18 | 2022-05-06 | 东莞市鹏威能源科技有限公司 | Graphene-based aerogel and preparation method thereof |
| CN115028883B (en) * | 2022-06-10 | 2023-11-10 | 山东蓝森新材料有限责任公司 | Preparation method of flame-retardant silicon aerogel |
| CN116199522A (en) * | 2023-01-17 | 2023-06-02 | 武汉中科先进材料科技有限公司 | PU sponge-based silicon aerogel felt and preparation method thereof |
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