CN107868190A - A kind of silica polymethyl methacrylate compound insulating material and preparation method thereof - Google Patents

A kind of silica polymethyl methacrylate compound insulating material and preparation method thereof Download PDF

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Publication number
CN107868190A
CN107868190A CN201610856368.7A CN201610856368A CN107868190A CN 107868190 A CN107868190 A CN 107868190A CN 201610856368 A CN201610856368 A CN 201610856368A CN 107868190 A CN107868190 A CN 107868190A
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weight
parts
insulating material
compound insulating
methyl methacrylate
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李洪彦
刘洪丽
宋礼猛
魏玉峰
李如意
付永强
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Tianjin Chengjian University
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Tianjin Chengjian University
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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
    • C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
    • 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
    • C08F6/00—Post-polymerisation treatments
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Silicon Compounds (AREA)
  • Silicon Polymers (AREA)

Abstract

The present invention discloses a kind of silica polymethyl methacrylate compound insulating material and preparation method thereof, use aerosil small molecule presoma and polymethyl methacrylate monomer for raw material, mixed under liquid phase environment small molecular state, pass through the reaction respectively of mixture supercritical technology together, realize the preparation with uniform three dimensional network structure compound insulating material, obtained aerogel material has uniform three-dimensional net structure, higher heat-proof quality and boundary thermal resistance, possesses excellent heat-insulating property.

Description

A kind of silicon dioxide-poly methyl methacrylate compound insulating material and its preparation Method
Technical field
The invention belongs to green construction material technical field, more particularly to a kind of silicon dioxide-poly methyl methacrylate Compound insulating material and preparation method thereof.
Background technology
The thermal loss of transparent enclosure structure accounts for very big proportion in building energy consumption, and its reason is largely derived from building The low thermal insulation of thing glass component.Particularly in the sternness increasingly of environment and energy problem instantly, building transparent enclosure knot is improved The insulation of structure is horizontal, makes great efforts to promote building energy conservation, for improving building thermal environments, mitigating environmental pollution, money of preserving our planet Source and ecological environment are respectively provided with more deep meaning.People recognize that building transparent enclosure structure heat dissipation capacity is big very early in fact This problem, it is proposed that some improve glass component thermal insulations method, such as hollow or vacuum glass, heat-reflecting glass, Low-E glass and pad pasting glass etc..But these methods do not solve the problems, such as the radiating of transparent enclosure structure fundamentally, or Say it is that the heat preservation and insulation methods of these glass components also reaches far away our expection.Polymethyl methacrylate (Polymethylmethacrylate, abbreviation PMMA, English Acrylic), also known as does acryl or lucite, its cast panel The number-average molecular weight of polymer is generally 2.2 × 104, relative density 1.19-1.20, refractive index 1.482-1.521, moisture absorption For degree below 0.5%, glass transition temperature is 105 DEG C.Low price, it is usual the advantages that being easy to be machined with the high grade of transparency The glass alternative materials being commonly used.PMMA thermal conductivity factor is about 0.2W/m.K, is mutually gone very apart from building heat preservation insulation requirement Far, at the same time, PMMA mechanical strengths, shock resistance etc. still have the space that can be lifted.Chemical silica airsetting Glue is a kind of novel low density, transparent, structure-controllable nano-porous materials, compared with traditional silicon dioxide particle, titanium dioxide Silica aerogel has continuous tridimensional network, has the design features such as low-density, high voidage, high-specific surface area.Simultaneously With excellent thermal and insulating performance, thermal conductivity is extremely low under normal temperature and pressure, is the minimum solid material of the thermal conductivity being currently known, Had broad application prospects in the heat-insulated field of building heat preservation.
The content of the invention
It is an object of the invention to provide a kind of silicon dioxide-poly methyl methacrylate compound insulating material and its preparation Method, use aerosil small molecule presoma and polymethyl methacrylate monomer for raw material, in liquid phase ring Mixed under the small molecular state of border, by the reaction respectively of mixture, supercritical technology, realization have uniform three dimensional network together The preparation of structure composite insulation material, obtained aerogel material have higher heat-proof quality and boundary thermal resistance.
The technical purpose of the present invention is achieved by following technical proposals：
A kind of silicon dioxide-poly methyl methacrylate compound insulating material and preparation method thereof, enters as steps described below OK：
Added in 80-150 parts by weight tetraethyl orthosilicates in the aqueous solution of 0.1-1 parts by weight 12mol/L hydrogen chloride (i.e. Hydrochloric acid), 30-180min is stood after stirring 5-30min at 20-25 DEG C of room temperature, then adds 0.01-0.2 parts by weight of sodium hydroxide Solid, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2-6h, 100 parts by weight are added in wet gel Methyl methacrylate, supernatant liquor is removed after soaking 12-24h, repeats immersion process 2-3 times, continues to add in wet gel The dibenzoyl peroxide of 0.02-0.2 parts by weight, being warming up to after ultrasonic disperse is uniform will be polymerize on initiation temperature with triggering, After standing 2-6h, product is placed in CO2In supercritical high-pressure extraction device, with CO2It is medium in 30-50 DEG C of temperature and air pressure 7- Supercritical drying 10-20h is carried out under 10MPa, you can obtain silicon dioxide-poly methyl methacrylate compound insulating material.
In the step, the progress supercritical drying time is 2-3h.
In the step, with CO2Supercritical drying is carried out for medium, temperature is 35-40 DEG C, air pressure 8-9MPa.
In the step, tetraethyl orthosilicate is 100-120 parts by weight, and the aqueous solution of 12mol/L hydrogen chloride is 0.3- 0.8 parts by weight, sodium hydrate solid are 0.05-0.1 parts by weight, and dibenzoyl peroxide is 0.07-0.15 parts by weight.
In the step, after adding the aqueous solution of hydrogen chloride in tetraethyl orthosilicate, 10- is stirred at 20-25 DEG C of room temperature 60-120min is stood after 20min, mixing speed turns for 100-150 per minute；Sodium hydrate solid is then added, is stirred to it It is completely dissolved, mixing speed turns for 100-150 per minute, wet gel will be obtained after above-mentioned solution left standstill 3-5h, in wet gel Methyl methacrylate is added, soaks 15-20h, dibenzoyl peroxide is added in wet gel, stands 3-5h.
Silicon dioxide-poly methyl-prop is observed using Dutch Philips Nanosem430 field emission scanning electron microscopes E pioic acid methyl ester compound insulating material, such as Fig. 1.Silicon dioxide-poly methyl methacrylate compound insulating material has three-dimensional network Structure, nano level hole distribution are more uniform.N2 adsorption specific surface area through scientific and technological (Beijing) Co., Ltd of Bei Shide instruments Analyzer determines, and the porosity of silicon dioxide-poly methyl methacrylate compound insulating material is 93.37%, pore-size distribution compared with To be uniform, 20-25nm is concentrated in porosity average out to 93-95%, aperture on the whole.
In the infrared spectrum of polymethyl methacrylate, in 1734cm-1The peak of appearance is C=O vibration absorption peak, 1458cm-1The peak nearby occurred is CH2Vibration absorption peak, in 1396cm-1Neighbouring peak is CH3Vibration absorption peak, 1241cm-1And 1149cm-1The peak nearby occurred is C-O-C vibration absorption peak.In the spectrogram of aerosil, 3523cm-1The peak nearby occurred is constitution water H-O-H vibration absorption peak, in 1650cm-1The peak nearby occurred is H-O-H Vibration absorption peak, in 1088cm-1The absworption peak nearby occurred is Si-O-Si vibration absorption peak, in 848cm-1And 472cm-1Go out Existing peak is Si-O-Si symmetrical stretching vibrations and flexural vibrations.Aerosil-polymethyl selects methyl esters complex heat-preservation In the infrared spectrum of material, in 1735cm-1The peak of appearance is C=O stretching vibrations, in 1145cm-1And 843cm-1The peak of appearance is Si-O-Si vibration absorption peak.The infrared spectrum of aerosil, more functions on the infrared curve of compound insulating material Group C=O, the composition of compound insulating material is illustrated, at the same time, on curve not having C=C is present, and illustrates that polymerization process is anti- Should be complete.
Bibliography (Effects of chemical bonding on heat transport across Interfaces, Nature Materials, 2012,11,502) it is described, use German Linseis TF-LFA types time domain heat Reflective probe determines silicon dioxide-poly methyl methacrylate compound insulating material boundary thermal resistance, the results are shown in Table 1.Using west An Xia small streams Electronic Science and Technology Co., Ltd. TC3000E types thermal conductivity factor instrument is to silicon dioxide-poly methyl methacrylate complex heat-preservation The thermal conductivity factor of material is measured, and the results are shown in Table 1, the silicon dioxide-poly methyl methacrylate complex heat-preservation finally prepared Material has higher boundary thermal resistance and relatively low thermal conductivity factor, boundary thermal resistance average out to 30-34MWm-2K-1, thermal conductivity factor Average out to 0.02-0.03Wm-1K-1。
Therefore, a kind of silicon dioxide-poly methyl methacrylate compound insulating material of the present invention and preparation method thereof, Use aerosil small molecule presoma and polymethyl methacrylate monomer for raw material, it is small in liquid phase environment Mixed under molecular state, by the reaction respectively of mixture, there is uniform three dimensional network structure to answer for supercritical technology, realization together The preparation of insulation material is closed, obtained aerogel material has uniform three-dimensional net structure, higher heat-proof quality and phase boundary Face thermal resistance, possess excellent heat-insulating property, i.e. silicon dioxide-poly methyl methacrylate compound insulating material of the invention is being built Build the application in insulation.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of silicon dioxide-poly methyl methacrylate compound insulating material.
Fig. 2 is that polymethyl methacrylate, aerosil and aerosil-polymethyl select methyl esters The infrared spectrum of compound insulating material.
Embodiment
Technical scheme is further illustrated with reference to specific embodiment, reagent and raw material therein are purchased from day Ke Miou chemical reagent Co., Ltd of Jinshi City, supercritical drying equipment is using Haian Oil Scientific Research Apparatus Co., Ltd. CO2Supercritical high-pressure extraction device.
Embodiment 1
0.5g12mol/L hydrochloric acid is added in 90g tetraethyl orthosilicates, 120min is stood after 22min is stirred at room temperature, is then added Enter 0.07g sodium hydroxides, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 5h, add 100g wherein Methyl methacrylate, supernatant liquor is removed after soaking 16h, repeats immersion process 2 times, adds 0.1g diphenyl peroxide first Acyl, be warming up to after ultrasonic disperse is uniform, to trigger polymerization, after standing 5h, CO will be placed in by product on initiation temperature2It is overcritical In high-pressure extraction device, with CO2Supercritical drying 13h is carried out under temperature 45 C and air pressure 7.2MPa for medium, you can obtain Silicon dioxide-poly methyl methacrylate compound insulating material.
Embodiment 2
1g12mol/L hydrochloric acid is added in 95g tetraethyl orthosilicates, 170min is stood after 5min is stirred at room temperature, is then added 0.14g sodium hydroxides, stir to it and are completely dissolved, and will obtain wet gel after above-mentioned solution left standstill 2.5h, add 100g wherein Methyl methacrylate, supernatant liquor is removed after soaking 24h, repeats immersion process 3 times, adds 0.17g diphenyl peroxide first Acyl, be warming up to after ultrasonic disperse is uniform, to trigger polymerization, after standing 5h, CO will be placed in by product on initiation temperature2It is overcritical In high-pressure extraction device, with CO2Supercritical drying 10h is carried out under temperature 50 C and air pressure 10MPa for medium, you can obtain two Silica-polymethyl methacrylate compound insulating material.
Embodiment 3
0.7g12mol/L hydrochloric acid is added in 110g tetraethyl orthosilicates, 90min is stood after 23min is stirred at room temperature, is then added Enter 0.13g sodium hydroxides, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2.7h, added wherein 100g methyl methacrylates, supernatant liquor is removed after soaking 12.5h, repeats immersion process 2 times, adds 0.12g peroxidating Dibenzoyl, be warming up to after ultrasonic disperse is uniform, to trigger polymerization, after standing 6h, CO will be placed in by product on initiation temperature2 In supercritical high-pressure extraction device, with CO2Supercritical drying 20h is carried out at 34 DEG C of temperature and air pressure 7MPa for medium, you can Obtain silicon dioxide-poly methyl methacrylate compound insulating material.
Embodiment 4
0.9g12mol/L hydrochloric acid is added in 150g tetraethyl orthosilicates, 55min is stood after 29min is stirred at room temperature, is then added Enter 0.2g sodium hydroxides, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2.5h, add 100g wherein Methyl methacrylate, supernatant liquor is removed after soaking 17h, repeats immersion process 3 times, adds 0.02g diphenyl peroxide first Acyl, be warming up to after ultrasonic disperse is uniform, to trigger polymerization, after standing 3h, CO will be placed in by product on initiation temperature2It is overcritical In high-pressure extraction device, with CO2Supercritical drying 13h is carried out at 49 DEG C of temperature and air pressure 7.1MPa for medium, you can obtain Silicon dioxide-poly methyl methacrylate compound insulating material.
Embodiment 5
0.5g12mol/L hydrochloric acid is added in 80g tetraethyl orthosilicates, 179min is stood after 27min is stirred at room temperature, is then added Enter 0.11g sodium hydroxides, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2h, add 100g wherein Methyl methacrylate, supernatant liquor is removed after soaking 12h, repeats immersion process 3 times, adds 0.06g diphenyl peroxide first Acyl, be warming up to after ultrasonic disperse is uniform, to trigger polymerization, after standing 3h, CO will be placed in by product on initiation temperature2It is overcritical In high-pressure extraction device, with CO2Supercritical drying 18h is carried out at 42 DEG C of temperature and air pressure 9.7MPa for medium, you can obtain Silicon dioxide-poly methyl methacrylate compound insulating material.
The impermeability of table 1 and thermal conductivity factor
According to the technical scheme of present invention, the system that corresponding technological parameter in preparation process carries out different materials is adjusted Material that is standby, finally preparing, the material base table prepared with above-described embodiment reveal identical property.The present invention is done above Exemplary description, it should explanation, in the case where not departing from the core of the present invention, any simple deformation, modification or Person other skilled in the art can not spend the equivalent substitution of creative work to each fall within protection scope of the present invention.

Claims (10)

  1. A kind of 1. silicon dioxide-poly methyl methacrylate compound insulating material, it is characterised in that porosity average out on the whole 93-95%, pore-size distribution is more uniform, and in 20-25nm, boundary thermal resistance is 30-34MWm-2K-1, thermal conductivity factor 0.02- 0.03Wm-1K-1, carry out as steps described below：
    (i.e. salt in the aqueous solution of 0.1-1 parts by weight 12mol/L hydrogen chloride is added in 80-150 parts by weight tetraethyl orthosilicates Acid), 30-180min is stood after stirring 5-30min at 20-25 DEG C of room temperature, 0.01-0.2 parts by weight of sodium hydroxide is then added and consolidates Body, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2-6h, 100 parts by weight first are added in wet gel Base methyl acrylate, supernatant liquor is removed after soaking 12-24h, repeats immersion process 2-3 times, continues to add in wet gel The dibenzoyl peroxide of 0.02-0.2 parts by weight, after standing 2-6h, product is placed in CO2In supercritical high-pressure extraction device, With CO2Supercritical drying 10-20h is carried out at 30-50 DEG C of temperature and air pressure 7-10MPa for medium, you can obtain silica- Polymethyl methacrylate compound insulating material.
  2. 2. a kind of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 1, its feature exist In in the step, the progress supercritical drying time is 2-3h.
  3. 3. a kind of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 1, its feature exist In in the step, with CO2Supercritical drying is carried out for medium, temperature is 35-40 DEG C, air pressure 8-9MPa.
  4. 4. a kind of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 1, its feature exist In in the step, tetraethyl orthosilicate is 100-120 parts by weight, and the aqueous solution of 12mol/L hydrogen chloride is 0.3-0.8 weights Part is measured, sodium hydrate solid is 0.05-0.1 parts by weight, and dibenzoyl peroxide is 0.07-0.15 parts by weight.
  5. 5. a kind of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 1, its feature exist In, in the step, in tetraethyl orthosilicate add hydrogen chloride the aqueous solution after, stir 10-20min at 20-25 DEG C of room temperature After stand 60-120min, mixing speed is that 100-150 per minute turns；Sodium hydrate solid is then added, is stirred completely molten to it Solution, mixing speed turn for 100-150 per minute, will obtain wet gel after above-mentioned solution left standstill 3-5h, first is added in wet gel Base methyl acrylate, 15-20h is soaked, dibenzoyl peroxide is added in wet gel, stand 3-5h.
  6. 6. a kind of preparation method of silicon dioxide-poly methyl methacrylate compound insulating material, it is characterised in that according to following Step is carried out：
    (i.e. salt in the aqueous solution of 0.1-1 parts by weight 12mol/L hydrogen chloride is added in 80-150 parts by weight tetraethyl orthosilicates Acid), 30-180min is stood after stirring 5-30min at 20-25 DEG C of room temperature, 0.01-0.2 parts by weight of sodium hydroxide is then added and consolidates Body, stir to it and be completely dissolved, wet gel will be obtained after above-mentioned solution left standstill 2-6h, 100 parts by weight first are added in wet gel Base methyl acrylate, supernatant liquor is removed after soaking 12-24h, repeats immersion process 2-3 times, continues to add in wet gel The dibenzoyl peroxide of 0.02-0.2 parts by weight, after standing 2-6h, product is placed in CO2In supercritical high-pressure extraction device, With CO2Supercritical drying 10-20h is carried out at 30-50 DEG C of temperature and air pressure 7-10MPa for medium, you can obtain silica- Polymethyl methacrylate compound insulating material.
  7. 7. a kind of preparation method of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 6, Characterized in that, in the step, the progress supercritical drying time is 2-3h.
  8. 8. a kind of preparation method of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 6, Characterized in that, in the step, with CO2Supercritical drying is carried out for medium, temperature is 35-40 DEG C, air pressure 8-9MPa.
  9. 9. a kind of preparation method of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 6, Characterized in that, in the step, tetraethyl orthosilicate is 100-120 parts by weight, and the aqueous solution of 12mol/L hydrogen chloride is 0.3-0.8 parts by weight, sodium hydrate solid are 0.05-0.1 parts by weight, and dibenzoyl peroxide is 0.07-0.15 parts by weight.
  10. A kind of 10. preparation side of silicon dioxide-poly methyl methacrylate compound insulating material according to claim 6 Method, it is characterised in that in the step, after adding the aqueous solution of hydrogen chloride in tetraethyl orthosilicate, stirred at 20-25 DEG C of room temperature 60-120min is stood after mixing 10-20min, mixing speed turns for 100-150 per minute；Then add sodium hydrate solid, stirring It is completely dissolved to it, mixing speed turns for 100-150 per minute, will obtain wet gel after above-mentioned solution left standstill 3-5h, wet solidifying Methyl methacrylate is added in glue, soaks 15-20h, dibenzoyl peroxide is added in wet gel, stands 3-5h.
CN201610856368.7A 2016-09-27 2016-09-27 A kind of silica polymethyl methacrylate compound insulating material and preparation method thereof Pending CN107868190A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105566585A (en) * 2015-06-09 2016-05-11 天津城建大学 Highly-impact-resistant highly-heat-insulating highly-light-transmitting high-strength polymethylmethacrylate composite material and preparation method thereof
CN105600795A (en) * 2016-01-16 2016-05-25 天津城建大学 SiO2 based composite aerogel material and preparation method thereof
CN105693958A (en) * 2016-01-16 2016-06-22 天津城建大学 Silicon dioxide-methyl methacrylate composite aerogel material based on surface modification and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105566585A (en) * 2015-06-09 2016-05-11 天津城建大学 Highly-impact-resistant highly-heat-insulating highly-light-transmitting high-strength polymethylmethacrylate composite material and preparation method thereof
CN105600795A (en) * 2016-01-16 2016-05-25 天津城建大学 SiO2 based composite aerogel material and preparation method thereof
CN105693958A (en) * 2016-01-16 2016-06-22 天津城建大学 Silicon dioxide-methyl methacrylate composite aerogel material based on surface modification and preparation method thereof

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