CN113045792A - Preparation method of starch/agar composite base flame-retardant aerogel - Google Patents
Preparation method of starch/agar composite base flame-retardant aerogel Download PDFInfo
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- CN113045792A CN113045792A CN202110295203.8A CN202110295203A CN113045792A CN 113045792 A CN113045792 A CN 113045792A CN 202110295203 A CN202110295203 A CN 202110295203A CN 113045792 A CN113045792 A CN 113045792A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/12—Agar-agar; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a preparation method of a starch/agar composite base flame-retardant aerogel, which comprises the steps of stirring and heating starch and agar powder in a water bath kettle, and dissolving to obtain starch/agar mixed sol; and ultrasonically dispersing the mixed suspension of the magnesium oxide powder and the attapulgite clay, adding the mixture into the mixed sol, continuously heating and stirring, cooling and condensing to obtain the composite hydrogel, freezing the obtained composite hydrogel in a refrigerator, and freeze-drying the composite hydrogel in a vacuum freeze dryer. According to the invention, the starch/agar composite aerogel is used as a carrier framework, the flame retardant magnesium hydroxide is introduced into the polymer aerogel in a simple and economic in-situ generation manner, the problem of poor compatibility of magnesium hydroxide and a polymer matrix is solved, the high addition of magnesium hydroxide is reduced by adding mineral clay with abundant reserves and flame retardant property, the prepared composite aerogel has a good flame retardant effect, the mechanical property is also improved, and the composite aerogel has a certain application prospect in the field of building heat preservation.
Description
Technical Field
The invention relates to a method for modifying starch-based aerogel by utilizing an in-situ generated flame retardant and a clay adding mode, and relates to the technical field of composite material preparation.
Background
The polymer aerogel has wide application prospect in the field of building heat preservation due to the special structure of light weight and porosity. Compared with the traditional inorganic aerogel material, the plant polysaccharide aerogel also has the advantages of biodegradability, biocompatibility and environmental friendliness; however, the poor mechanical properties and easy combustion of the starch/agar based composite aerogel material are important reasons for limiting the application of the starch/agar based composite aerogel material in the field of building thermal insulation and heat preservation.
The flame retardant is introduced into the aerogel matrix, so that the flame retardant performance is improved simply and efficiently. Magnesium hydroxide is an environment-friendly flame retardant widely applied in the polymer industry, but the magnesium hydroxide has large specific surface area and is easy to agglomerate among crystal grains, so that the problem of poor compatibility with polymers exists; on the other hand, magnesium hydroxide has low flame retardant efficiency, and researches show that the sufficient flame retardant effect can be achieved only by the loading amount of magnesium hydroxide of more than 50 wt%, which can further damage the compatibility of the filler and the polymer matrix, lead to the reduction of the mechanical properties of the aerogel and bring cost burden. Patent CN110128698A discloses a method for preparing an environment-friendly flame-retardant smoke suppressant, which is prepared by performing surface treatment on an environment-friendly inorganic flame retardant (magnesium hydroxide, aluminum hydroxide, brucite or hydrotalcite) by adopting a molybdenum-containing borate ester active agent, wherein the active agent is uniformly coated on the surface of flame retardant powder, so that the compatibility of the flame retardant powder and a polymer matrix is improved, and the flame retardant powder can be applied to high polymer materials such as polyvinyl chloride, butadiene acrylonitrile rubber, polystyrene, unsaturated resin and the like. Patent CN112225945A discloses a magnesium hydroxide-microcapsule flame retardant and a preparation method thereof, wherein magnesium hydroxide is used as a flame retardant core, and a surface modification layer, a DOPO layer and a polymerization layer are sequentially coated on the outer layer of the flame retardant core, so that the problems of low flame retardant efficiency and poor dispersibility and compatibility in a polymer matrix of the flame retardant are effectively solved. Some of the inventions adopt the surfactant, the saturated or unsaturated high fatty acid salt, the silane coupling agent and the like to modify the magnesium hydroxide flame retardant, so that the compatibility problem of the flame retardant and a polymer matrix is solved to a certain extent, but the introduction of the modifier is undoubtedly accompanied with the problems of new process cost and environmental protection, and the high addition of the magnesium hydroxide is still difficult to solve.
The attapulgite is a water-containing magnesium-rich aluminosilicate clay mineral with a chain layered structure, has good length-diameter ratio and abundant inner pore channels, generates water vapor by the loss of structure water of the attapulgite clay at high temperature, can block oxygen, and can generate MgO and Al with good stability2O3The oxide interlayer is a better reinforcing material and has a flame-retardant effect. The attapulgite has abundant reserves in northwest areas of China and completely meets the requirements of industrial production. The development and utilization of the clay mineral are effectively widened, the resource value of the clay mineral is changed into economic value, and the clay mineral is particularly important for serving national economic development.
Disclosure of Invention
The purpose of the invention is: provides a simple, economic and environment-friendly method for successfully loading magnesium hydroxide in a starch/agar composite aerogel matrix, and solves the problem of poor compatibility of magnesium hydroxide and other high polymer materials. And the attapulgite clay mineral with rich reserves is introduced to solve the problem of high addition of magnesium hydroxide, and meanwhile, a new way is opened up for the development and utilization of the attapulgite clay mineral with rich resources.
The technical solution of the invention is as follows: stirring and heating starch and agar powder in a water bath kettle to completely dissolve the starch and the agar powder to obtain starch/agar mixed sol; then ultrasonically dispersing the mixed suspension of the magnesium oxide powder and the attapulgite clay, adding the mixture into the mixed sol, and continuously heating and stirring to hydrate the magnesium oxide to generate magnesium hydroxide; and then cooling and condensing to obtain the composite hydrogel, and freezing in a refrigerator and carrying out vacuum freeze drying to obtain the composite aerogel.
Preferably, in the preparation method of the starch/agar composite base flame-retardant aerogel, which is simple and economical in process, the flame retardant magnesium hydroxide is generated in situ through magnesium oxide.
Preferably, said starch belongs to the group of potato starches.
Preferably, the starch and agar concentrations are 2% and 1%, respectively.
Preferably, the addition amount of the magnesium oxide powder and the clay is as follows: the mass of the magnesium hydroxide generated in situ by the magnesium oxide and the mass of the attapulgite respectively account for (0%, 60%, 0%, 50% and 10%) of the total mass of the starch/agar/magnesium hydroxide/attapulgite.
Preferably, the water bath heating and stirring temperature is 99 ℃, the rotating speed is 500rpm, and the time is 4 h.
Preferably, the sol condensation is carried out rapidly by placing the mold in a cold water environment.
Preferably, the refrigerator temperature is-40 ℃, the freezing time is 24h, the vacuum freeze dryer temperature is-60 ℃, the vacuum degree is 1Pa, and the time is not less than 60 h.
Compared with the prior art, the invention has the following advantages:
1. the potato starch and agar are used as raw materials, and the potato starch and agar biodegradable natural non-toxic food has the advantages of wide sources and biodegradability.
2. The magnesium hydroxide fire retardant is introduced into the polymer matrix in an in-situ generation mode, the process is simple and economic, the problem of poor compatibility of the fire retardant and the polymer matrix can be effectively avoided, and meanwhile, the framework strength of the aerogel matrix can be improved.
3. The attapulgite clay which is abundant and cheap in reserves in China is used as a flame retardant to replace magnesium hydroxide, so that the high addition amount of the magnesium hydroxide is reduced, the cost is reduced, and the application approaches of the attapulgite clay are widened.
Drawings
FIG. 1 is an optical photograph of (a) several starch/agar based composite aerogels and (b) starch/agar aerogel burn for 5s, (c) starch/agar/magnesium hydroxide aerogel burn for 5s, and (d) starch/agar/magnesium hydroxide/attapulgite aerogel burn for 5 s.
Figure 2 is a composite aerogel compressive stress-strain curve.
Detailed Description
The technical solution of the invention is further illustrated below with reference to examples, which are not to be construed as limiting the technical solution.
Example 1
Dissolving 20g of potato starch and 10g of agar powder in 1000ml of distilled water, stirring in a water bath heating stirring pot at 99 ℃ until the potato starch and the agar powder are completely dissolved, pouring the dissolved mixed sol into a mold placed in cold water for condensation molding, freezing the molded hydrogel sample in a refrigerator at-40 ℃, and then transferring the frozen hydrogel sample into a vacuum freeze dryer for drying for 60 hours to sublimate frozen water to prepare the starch/agar composite aerogel.
Example 2
Dissolving 6.20g of magnesium oxide powder in a small amount of distilled water, uniformly stirring by magnetic force, performing ultrasonic dispersion for 20min, adding the obtained magnesium oxide suspension into 200ml of the mixed sol obtained in the embodiment 1, continuously heating and stirring for 4h in a water bath kettle at 99 ℃, then condensing and molding in a mold, freezing the obtained composite hydrogel in a refrigerator at-40 ℃, and drying in a vacuum freeze dryer for 60h to sublimate frozen water to obtain the starch/agar/magnesium hydroxide composite aerogel.
Example 3
Dissolving 5.17g of magnesium oxide powder and 1.5g of attapulgite clay in a small amount of distilled water, performing magnetic stirring uniformly, performing ultrasonic dispersion for 20min, adding the obtained magnesium oxide suspension into 200ml of the mixed sol obtained in the example 1, continuously heating and stirring in a 99 ℃ water bath kettle for 4h, then performing condensation molding in a mold, freezing the obtained composite hydrogel in a-40 ℃ refrigerator, and drying in a vacuum freeze-drying machine for 60h to sublimate the frozen water to obtain the starch/agar/magnesium hydroxide/attapulgite composite aerogel.
The invention discloses a preparation method of a starch/agar composite base flame-retardant aerogel, which utilizes a method of in-situ generation and clay addition to carry out flame-retardant modification on a polymer aerogel. Stirring and heating starch and agar powder in a water bath kettle to completely dissolve the starch and the agar powder to obtain starch/agar mixed sol; then ultrasonically dispersing the mixed suspension of the magnesium oxide powder and the attapulgite clay, adding the mixture into the mixed sol, and continuously heating and stirring to hydrate the magnesium oxide to generate magnesium hydroxide; and then cooling and condensing to obtain the composite hydrogel, and freezing in a refrigerator at-40 ℃ and freeze-drying in vacuum to obtain the magnesium hydroxide and attapulgite clay loaded starch/agar-based composite aerogel. According to the invention, the starch/agar composite aerogel which is rich in resources and biodegradable is used as a carrier framework, the flame retardant magnesium hydroxide is introduced into the polymer aerogel through a simple and economic in-situ generation mode, the problem of poor compatibility of the magnesium hydroxide and a polymer matrix is solved, the high addition of the magnesium hydroxide is reduced by adding the mineral clay which is rich in reserves and has flame retardant characteristics, the prepared composite aerogel has a good flame retardant effect, the mechanical property is also improved, and the composite aerogel has a certain application prospect in the field of building heat preservation.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. 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. The preparation method of the starch/agar composite base flame-retardant aerogel is characterized by comprising the following steps:
step 1): dispersing potato starch and agar powder in distilled water, dissolving in a water bath heating stirring pot to obtain starch/agar mixed sol, sealing, and placing in an oven for use;
step 2): dispersing magnesium oxide powder and attapulgite clay in distilled water, and performing ultrasonic dispersion after uniform magnetic stirring;
step 3): adding the suspension obtained in the step 2) into the mixed sol prepared in the step 1), and heating and stirring in a water bath;
step 4): condensing and molding the composite sol obtained in the step 3) in a mold to obtain starch/agar/magnesium hydroxide/attapulgite composite hydrogel;
step 5): freezing the composite hydrogel obtained in the step 4) in a refrigerator, and then placing the frozen composite hydrogel in a vacuum freeze dryer for freeze drying to obtain the starch/agar/magnesium hydroxide/attapulgite composite aerogel.
2. The method of claim 1, wherein the concentrations of potato starch and agar in step 1) are 2% and 1%, respectively.
3. The preparation method according to claim 1, wherein the heating temperature of the water bath in the step 1) is 99 ℃, the stirring speed is 500rpm, and the oven temperature is not lower than 70 ℃.
4. The method according to claim 1, wherein the sonication time in step 2) is 20 min.
5. The method according to claim 1, wherein the amount of the magnesium oxide powder and the clay added in step 2) is: the mass of the magnesium hydroxide generated in situ by the magnesium oxide and the mass of the attapulgite respectively account for (0 percent and 0 percent) of the total mass of the starch/agar/magnesium hydroxide/attapulgite.
6. The method according to claim 1, wherein the amount of the magnesium oxide powder and the clay added in step 2) is: the mass of the magnesium hydroxide generated in situ by the magnesium oxide and the mass of the attapulgite respectively account for 60 percent and 0 percent of the total mass of the starch/agar/magnesium hydroxide/attapulgite.
7. The method according to claim 1, wherein the amount of the magnesium oxide powder and the clay added in step 2) is: the mass of the magnesium hydroxide generated in situ by the magnesium oxide and the mass of the attapulgite respectively account for 50 percent and 10 percent of the total mass of the starch/agar/magnesium hydroxide/attapulgite.
8. The method according to claim 1, wherein the heating temperature of the water bath in the step 3) is 99 ℃, the stirring speed is 500rpm, and the stirring time is 4 hours.
9. The method according to claim 1, wherein the condensation molding in step 4) is performed by immersing the mold in cold water.
10. The method according to claim 1, wherein in the step 5), the temperature of the refrigerator is-40 ℃, the freezing time is 24 hours, the temperature of the freeze dryer is-60 ℃, the vacuum degree is 1Pa, and the time is not less than 60 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114292446A (en) * | 2021-12-27 | 2022-04-08 | 重庆大学 | Glucomannan composite flame-retardant aerogel and preparation method thereof |
| CN116515329A (en) * | 2023-05-22 | 2023-08-01 | 兰州交通大学 | Preparation method of air purification inorganic coating based on in-situ growth method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114292446A (en) * | 2021-12-27 | 2022-04-08 | 重庆大学 | Glucomannan composite flame-retardant aerogel and preparation method thereof |
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| CN116515329A (en) * | 2023-05-22 | 2023-08-01 | 兰州交通大学 | Preparation method of air purification inorganic coating based on in-situ growth method |
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