CN111454386A - Preparation method of aerogel organic glass - Google Patents
Preparation method of aerogel organic glass Download PDFInfo
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- CN111454386A CN111454386A CN202010410464.5A CN202010410464A CN111454386A CN 111454386 A CN111454386 A CN 111454386A CN 202010410464 A CN202010410464 A CN 202010410464A CN 111454386 A CN111454386 A CN 111454386A
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- aerogel
- prepolymer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
Abstract
The invention discloses a preparation method of aerogel glass, which comprises the following steps of weighing raw material aerogel powder and a methyl methacrylate matrix according to weight; adding the prepared methyl methacrylate substrate into a reaction kettle, stirring and converting into a prepolymer, and enabling the conversion rate of the prepolymer to reach 25-35%; adding the weighed aerogel powder into a prepolymer with the conversion rate of 25-35%, continuously stirring and uniformly mixing to form a mixed prepolymer, wherein the conversion rate of the mixed prepolymer reaches 50%; filtering the mixed prepolymer, adding the filtered mixed prepolymer into a mold, and performing vibration exhaust and promotion of final polymerization until the mixed prepolymer in the mold is in a gel state; and continuously heating and maintaining the temperature, so that the mixed prepolymer in the gel state forms the formed aerogel organic glass. According to the invention, aerogel particles with various specifications are uniformly mixed with the organic glass prepolymer, so that the aerogel organic glass with low heat conductivity coefficient, high mechanical strength, good sound absorption and noise reduction effects and convenience in installation and use is obtained.
Description
Technical Field
The invention relates to the technical field of glass preparation, in particular to a preparation method of aerogel glass.
Background
The aerogel is a light nano porous amorphous solid material formed by mutually clustering primary particles with the diameter of about 3-8nm, has low density and vacuum thermal conductivity of 0.001W/m.K, and is a very good thermal insulation material. Wherein the variable acoustic impedance range of the silicon dioxide aerogel powder is about 103-107kg/m2 & S, the average sound absorption coefficient is more than 0.8 in the frequency range of 125-4000Hz, the sound absorption performance is not changed after water spraying and ash spraying, and the silicon dioxide aerogel powder has excellent sound absorption performance. Since the porosity of the aerogel is more than 98%, and the specific surface area is 1000m2/g, the aerogel is a solid with the lowest density in the world at present and is also a high-brittleness solid, the high-brittleness application of the aerogel product has to be combined with other toughness materials, such as aerogel glass fiber composite materials, aerogel ceramic fiber composite materials, aerogel pre-oxidized fiber composite materials and the like which are industrialized at present.
The assembly of organic/inorganic nano-hybrid materials and related nanotechnology are currently the focus of research for the preparation of new nanocomposites. Organic glass (PMMA) is one of the best transparent polymer materials, and has excellent toughness, optical properties, electrical insulation properties, and processability. The glass has wide application in the aspects of bulletproof glass, aircraft cabin window glass, optical appliances, building materials and the like. The application range is limited due to the disadvantages in heat resistance, toughness, and the like. Chemical crosslinking and nano-compounding are important ways to improve the heat resistance, mechanical property and other properties of the organic glass. By organically combining the rigidity and thermal stability of the inorganic particles, the toughness of the organic material, the processing type, and the like, a composite material having excellent properties can be obtained.
Disclosure of Invention
The invention aims to provide a preparation method of aerogel organic glass, which is characterized in that aerogel particles with various specifications are uniformly mixed with organic glass prepolymer to obtain the aerogel organic glass with low heat conductivity coefficient, high mechanical strength, good sound absorption and noise reduction effects and convenient installation and use.
The invention provides a preparation method of aerogel organic glass, which comprises the following steps:
(1) weighing raw material aerogel powder and methyl methacrylate matrix according to the weight ratio of 0.2-200: 100;
(2) adding the prepared methyl methacrylate substrate into a reaction kettle, stirring and converting into a prepolymer, and enabling the conversion rate of the prepolymer to reach 25-35%;
(3) adding the weighed aerogel powder into a prepolymer with the conversion rate of 25-35%, continuously stirring and uniformly mixing to form a mixed prepolymer, wherein the conversion rate of the mixed prepolymer reaches 50%;
(4) filtering the mixed prepolymer, adding the filtered mixed prepolymer into a mold, and placing the mold in a constant-temperature shaking table or constant-temperature ultrasonic equipment for vibration exhaust and promotion of final polymerization until the mixed prepolymer in the mold is in a gel state;
(5) and continuously heating and maintaining the temperature, so that the mixed prepolymer in the gel state forms the formed aerogel organic glass.
Preferably, in the step (1), the aerogel powder is silicon aerogel powder, silicon aerogel particles or carbon aerogel powder subjected to hydrophobic treatment, and the particle size of the aerogel powder is 200-1000-mesh uniform powder.
Preferably, in the step (1), the methyl methacrylate matrix comprises 90.1-94.79% of methyl methacrylate, 0.06-0.2% of initiator, 4.8-9% of plasticizer and 0.35-0.7% of release agent according to parts by weight.
Preferably, the initiator is selected from one of benzoyl peroxide, azobisisobutyronitrile and diisopropyl peroxycarbonate.
Preferably, the plasticizer is one of dibutyl phthalate, dioctyl ester, dibutyl sebacate and di-n-butyl adipate.
Preferably, the release agent is stearic acid or silicone oil.
Preferably, in the step (2), the reaction kettle comprises a jacket, a stirrer and a feeding port, the temperature of the jacket is set to be 60-90 ℃, and the stirring time of the reaction kettle is 30-60 min.
Preferably, in the step (3), the heating temperature for stirring is 80 to 90 ℃.
Preferably, in the step (4), a 100-mesh 200-mesh stainless steel wire net is used for filtering, the temperature of a constant-temperature shaking table or constant-temperature ultrasonic equipment is set to be 50-100 ℃, the oscillation amplitude is less than or equal to 25mm, and the ultrasonic frequency is less than or equal to 4 KHz.
Preferably, in the step (5), the temperature is raised to 95 ℃, and the holding time is 2 h.
The embodiment of the invention provides a preparation method of aerogel organic glass, wherein the dried aerogel powder is used for preparing the aerogel organic glass, so that the influence of moisture introduction on the prepolymerization process of an organic glass body methyl methacrylate matrix is avoided, and the physical properties of the organic glass are improved; the aerogel uniform powder with the granularity of 200 meshes to 1000 meshes is selected, so that the structural characteristics of the aerogel can be maintained to the maximum extent, and the sound absorption effect of the prepared aerogel organic glass can be greatly improved; the aerogel powder is added in the prepolymerization process of the methyl methacrylate matrix, so that the prepared aerogel glass material is more uniform, and the heat insulation performance is improved; the organic glass prepared by mixing the hydrophobic silica aerogel and the methyl methacrylate polymer matrix maintains the high hydrophobicity of the aerogel, improves the self water absorption performance and prolongs the aging time.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts, based on the embodiments of the present invention, belong to the scope of protection of the present invention, and in the context of the present invention the terms "oil well drilling, production and storage system" and "gas well drilling, production and storage system" comprise all corrosion-prone pipes and equipment for drilling, producing and storing oil and gas from underground formations.
Example 1
The embodiment 1 of the invention provides a preparation method of aerogel organic glass, which comprises the following steps:
(1) weighing 100g of raw material gas gel powder and 5kg of methyl methacrylate matrix according to the weight; wherein the aerogel powder is silicon aerogel powder subjected to hydrophobic treatment, and the particle size of the aerogel powder is 600-mesh uniform powder; the methyl methacrylate matrix comprises 90.1 percent of methyl methacrylate, 0.2 percent of benzoyl peroxide, 9 percent of dibutyl phthalate and 0.7 percent of stearic acid according to parts by weight;
(2) adding the prepared methyl methacrylate substrate into a reaction kettle provided with a jacket, a stirrer and a feeding port, and stirring to convert the methyl methacrylate substrate into a prepolymer, wherein the temperature of the jacket is set to be 80 ℃, and the stirring time is 35min, so that the conversion rate of the prepolymer reaches 25%;
(3) drying, grinding and sieving the weighed aerogel powder, adding the aerogel powder into a prepolymer with a conversion rate of 25%, continuously stirring and uniformly mixing, controlling the polymerization temperature to be 85 ℃ to form a mixed prepolymer, and enabling the conversion rate of the mixed prepolymer to reach 50%;
(4) filtering the mixed prepolymer through a 200-mesh stainless steel wire net, adding the filtered mixed prepolymer into a mold, placing the mold in a constant-temperature shaking table or constant-temperature ultrasonic equipment for vibration exhaust and promotion of final polymerization, setting the temperature at 60 ℃, the vibration amplitude at 25mm, the ultrasonic frequency at 4KHz and the time at 2h, and stopping ultrasonic treatment until the mixed prepolymer in the mold is in a gel state;
(5) and continuously heating to 90 ℃ and keeping for 2 hours to enable the gel-state mixed prepolymer to form the formed aerogel organic glass, and cooling and demolding to obtain the aerogel organic glass with uniformly dispersed aerogel powder.
Example 2
The embodiment 2 of the invention provides a preparation method of aerogel organic glass, which comprises the following steps:
(1) weighing 500g of raw material aerogel powder and 5kg of methyl methacrylate matrix according to the weight; wherein the aerogel powder is silicon aerogel powder subjected to hydrophobic treatment, and the particle size of the aerogel powder is 600-mesh uniform powder; the methyl methacrylate matrix comprises 93 percent of methyl methacrylate, 0.1 percent of azobisisobutyronitrile, 6.4 percent of dioctyl and 0.5 percent of silicone oil according to the weight portion;
(2) adding the prepared methyl methacrylate substrate into a reaction kettle provided with a jacket, a stirrer and a feeding port, and stirring to convert the methyl methacrylate substrate into a prepolymer, wherein the temperature of the jacket is set to be 85 ℃, and the stirring time is 30min, so that the conversion rate of the prepolymer reaches 25%;
(3) drying, grinding and sieving the weighed aerogel powder, adding the aerogel powder into a prepolymer with a conversion rate of 25%, continuously stirring and uniformly mixing, controlling the polymerization temperature to be 85 ℃ to form a mixed prepolymer, and enabling the conversion rate of the mixed prepolymer to reach 50%;
(4) filtering the mixed prepolymer through a 100-mesh stainless steel wire net, adding the filtered mixed prepolymer into a mold, placing the mold in a constant-temperature shaking table or constant-temperature ultrasonic equipment for vibration exhaust and promotion of final polymerization, setting the temperature at 65 ℃, the vibration amplitude at 25mm, the ultrasonic frequency at 2KHz and the time at 1.5h, and stopping ultrasonic treatment until the mixed prepolymer in the mold is in a gel state;
(5) and continuously heating to 90 ℃ and keeping for 2 hours to enable the gel-state mixed prepolymer to form the formed aerogel organic glass, and cooling and demolding to obtain the aerogel organic glass with uniformly dispersed aerogel powder.
Example 3
The embodiment 3 of the invention provides a preparation method of aerogel organic glass, which comprises the following steps:
(1) weighing 800g of raw material aerogel powder and 5kg of methyl methacrylate matrix according to the weight; wherein the aerogel powder is silicon aerogel powder subjected to hydrophobic treatment, and the particle size of the aerogel powder is uniform powder of 1000 meshes; the methyl methacrylate matrix comprises 94.7 percent of methyl methacrylate, 0.06 percent of diisopropyl peroxycarbonate, 4.89 percent of dibutyl sebacate and 0.35 percent of silicone oil according to the weight portion;
(2) adding the prepared methyl methacrylate substrate into a reaction kettle provided with a jacket, a stirrer and a feeding port, and stirring to convert the methyl methacrylate substrate into a prepolymer, wherein the temperature of the jacket is set to be 85 ℃, and the stirring time is 40min, so that the conversion rate of the prepolymer reaches 30%;
(3) drying, grinding and sieving the weighed aerogel powder, adding the aerogel powder into a prepolymer with the conversion rate of 30%, continuously stirring and uniformly mixing, controlling the polymerization temperature to be 85 ℃ to form a mixed prepolymer, and enabling the conversion rate of the mixed prepolymer to reach 50%;
(4) filtering the mixed prepolymer through a 200-mesh stainless steel wire net, adding the filtered mixed prepolymer into a mold, placing the mold in a constant-temperature shaking table or constant-temperature ultrasonic equipment for vibration exhaust and promotion of final polymerization, setting the temperature at 65 ℃, the vibration amplitude at 25mm, the ultrasonic frequency at 4KHz and the time at 1h, and stopping ultrasonic treatment until the mixed prepolymer in the mold is in a gel state;
(5) and continuously heating to 90 ℃ and keeping for 2 hours to enable the gel-state mixed prepolymer to form the formed aerogel organic glass, and cooling and demolding to obtain the aerogel organic glass with uniformly dispersed aerogel powder.
Example 4
The embodiment 4 of the invention provides a preparation method of aerogel organic glass, which comprises the following steps:
(1) weighing 2kg of raw material aerogel powder and 5kg of methyl methacrylate matrix according to the weight; wherein the aerogel powder is silicon aerogel powder subjected to hydrophobic treatment, and the particle size of the aerogel powder is uniform powder with 500 meshes; the methyl methacrylate matrix comprises 93.5 percent of methyl methacrylate, 0.2 percent of benzoyl peroxide, 9 percent of dibutyl phthalate and 0.6 percent of stearic acid according to parts by weight;
(2) adding the prepared methyl methacrylate substrate into a reaction kettle provided with a jacket, a stirrer and a feeding port, and stirring to convert the methyl methacrylate substrate into a prepolymer, wherein the temperature of the jacket is set to be 70 ℃, and the stirring time is 45min, so that the conversion rate of the prepolymer reaches 25%;
(3) drying, grinding and sieving the weighed aerogel powder, adding the aerogel powder into a prepolymer with a conversion rate of 25%, continuously stirring and uniformly mixing, controlling the polymerization temperature to be 85 ℃ to form a mixed prepolymer, and enabling the conversion rate of the mixed prepolymer to reach 50%;
(4) filtering the mixed prepolymer through a 200-mesh stainless steel wire net, adding the filtered mixed prepolymer into a mold, placing the mold in a constant-temperature shaking table or constant-temperature ultrasonic equipment for vibration exhaust and promotion of final polymerization, setting the temperature at 60 ℃, the vibration amplitude at 25mm, the ultrasonic frequency at 4KHz and the time at 2h, and stopping ultrasonic treatment until the mixed prepolymer in the mold is in a gel state;
(5) and continuously heating to 90 ℃ and keeping for 2.5 hours to enable the gel-state mixed prepolymer to form the formed aerogel organic glass, and cooling and demolding to obtain the aerogel organic glass with uniformly dispersed aerogel powder.
Example 5
The embodiment 5 of the invention provides a preparation method of aerogel organic glass, which comprises the following steps:
(1) weighing 10kg of raw material aerogel powder and 5kg of methyl methacrylate matrix according to the weight; wherein the aerogel powder is silicon aerogel powder subjected to hydrophobic treatment, and the particle size of the aerogel powder is 200-mesh uniform powder; the methyl methacrylate matrix comprises 94 percent of methyl methacrylate, 0.2 percent of benzoyl peroxide, 9 percent of dibutyl phthalate and 0.7 percent of silicone oil according to the weight portion;
(2) adding the prepared methyl methacrylate substrate into a reaction kettle provided with a jacket, a stirrer and a feeding port, and stirring to convert the methyl methacrylate substrate into a prepolymer, wherein the temperature of the jacket is set to be 70 ℃, and the stirring time is 45min, so that the conversion rate of the prepolymer reaches 25%;
(3) drying, grinding and sieving the weighed aerogel powder, adding the aerogel powder into a prepolymer with a conversion rate of 25%, continuously stirring and uniformly mixing, controlling the polymerization temperature to be 85 ℃ to form a mixed prepolymer, and enabling the conversion rate of the mixed prepolymer to reach 50%;
(4) filtering the mixed prepolymer through a 100-mesh stainless steel wire net, adding the filtered mixed prepolymer into a mold, placing the mold in a constant-temperature shaking table or constant-temperature ultrasonic equipment for vibration exhaust and promotion of final polymerization, setting the temperature at 60 ℃, the vibration amplitude at 20mm, the ultrasonic frequency at 2KHz and the time at 2h, and stopping ultrasonic treatment until the mixed prepolymer in the mold is in a gel state;
(5) and continuously heating to 90 ℃ and keeping for 2 hours to enable the gel-state mixed prepolymer to form the formed aerogel organic glass, and cooling and demolding to obtain the aerogel organic glass with uniformly dispersed aerogel powder.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. The preparation method of the aerogel organic glass is characterized by comprising the following steps of:
(1) weighing raw material aerogel powder and a methyl methacrylate matrix according to weight, wherein the weight ratio of the aerogel powder to the methyl methacrylate matrix is 0.2-200: 100;
(2) adding the prepared methyl methacrylate substrate into a reaction kettle, stirring and converting into a prepolymer, and enabling the conversion rate of the prepolymer to reach 25-35%;
(3) adding the weighed aerogel powder into a prepolymer with the conversion rate of 25-35%, continuously stirring and uniformly mixing to form a mixed prepolymer, wherein the conversion rate of the mixed prepolymer reaches 50%;
(4) filtering the mixed prepolymer, adding the filtered mixed prepolymer into a mold, and placing the mold in a constant-temperature shaking table or constant-temperature ultrasonic equipment for vibration exhaust and promotion of final polymerization until the mixed prepolymer in the mold is in a gel state;
(5) and continuously heating and maintaining the temperature, so that the mixed prepolymer in the gel state forms the formed aerogel organic glass.
2. The method for preparing aerogel organic glass according to claim 1, wherein in the step (1), the aerogel powder is hydrophobic-treated silica aerogel powder, silica aerogel particles or carbon aerogel powder, and the particle size of the aerogel powder is 200-1000 mesh uniform powder.
3. The method for preparing aerogel organic glass according to claim 1, wherein in step (1), the methyl methacrylate matrix comprises 90.1-94.79% of methyl methacrylate, 0.06-0.2% of initiator, 4.8-9% of plasticizer and 0.35-0.7% of release agent in parts by weight.
4. The method of claim 3, wherein the initiator is selected from the group consisting of benzoyl peroxide, azobisisobutyronitrile, and diisopropyl peroxycarbonate.
5. The method of claim 3, wherein said plasticizer is selected from the group consisting of dibutyl phthalate, dioctyl phthalate, dibutyl sebacate, and di-n-butyl adipate.
6. The method of claim 3, wherein the release agent is stearic acid or silicone oil.
7. The method for preparing aerogel organic glass according to claim 1, wherein in step (2), the reaction kettle comprises a jacket, a stirrer and a feeding port, the temperature of the jacket is set to be 60-90 ℃, and the stirring time of the reaction kettle is 30-60 min.
8. The method of preparing aerogel organic glass as in claim 1, wherein in step (3), the temperature of stirring and heating is 80-90 ℃.
9. The method for preparing aerogel organic glass as in claim 1, wherein in the step (4), 100-mesh 200-mesh stainless steel wire mesh is used for filtering, the temperature of the constant temperature shaking table or constant temperature ultrasonic equipment is set to be 50-100 ℃, the oscillation amplitude is less than or equal to 25mm, and the ultrasonic frequency is less than or equal to 4 KHz.
10. The method for preparing aerogel organic glass as in claim 1, wherein in step (5), the temperature is raised to 95 ℃ and the holding time is 2 h.
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| CN202010410464.5A CN111454386B (en) | 2020-05-15 | 2020-05-15 | Preparation method of aerogel organic glass |
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| CN202010410464.5A CN111454386B (en) | 2020-05-15 | 2020-05-15 | Preparation method of aerogel organic glass |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114702774A (en) * | 2022-02-15 | 2022-07-05 | 上海耀江建设工程有限公司 | Flame-retardant heat-insulation organic material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566583A (en) * | 2015-06-09 | 2016-05-11 | 天津城建大学 | Highly-impact-resistant highly-light-transmitting highly-heat-insulating polymethylmethacrylate composite material and preparation method thereof |
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2020
- 2020-05-15 CN CN202010410464.5A patent/CN111454386B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566583A (en) * | 2015-06-09 | 2016-05-11 | 天津城建大学 | Highly-impact-resistant highly-light-transmitting highly-heat-insulating polymethylmethacrylate composite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114702774A (en) * | 2022-02-15 | 2022-07-05 | 上海耀江建设工程有限公司 | Flame-retardant heat-insulation organic material and preparation method and application thereof |
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