CN105968789B - A kind of lightweight Organic-inorganic composite insulating foam and preparation method - Google Patents
A kind of lightweight Organic-inorganic composite insulating foam and preparation method Download PDFInfo
- Publication number
- CN105968789B CN105968789B CN201610290386.3A CN201610290386A CN105968789B CN 105968789 B CN105968789 B CN 105968789B CN 201610290386 A CN201610290386 A CN 201610290386A CN 105968789 B CN105968789 B CN 105968789B
- Authority
- CN
- China
- Prior art keywords
- added
- solution
- sio
- nanosphere
- foam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/04—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2101/00—Manufacture of cellular products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of lightweight organo-mineral complexing insulating foam and preparation method thereof, the complex heat-preservation foamed material is by polyurethane foam, nano zeolite porous fibre composite aerogel, modified mesoporous C SiO2Nanosphere is compound to be prepared；Wherein, the mass fraction of complex heat-preservation foamed material is 60 70%, and the mass fraction of nano zeolite porous fibre composite aerogel is 10 20%, remaining is modified mesoporous C SiO2Nanosphere；By after above-mentioned three kinds of material mixings through injection molding, swollen fixed, demoulding and after cure, obtain organo-mineral complexing insulating foam.The present invention not only increases the tensile strength of polyurethane foam using novel porous fiber composite aeroge as the modifying agent of polyurethane foam, while ensuring that polyurethane foamed material has preferable heat-insulating property；Pass through the mesoporous C SiO of modification2Nanosphere is filled the modified heat-insulating property for further improving polyurethane foam to polyurethane.
Description
Technical field
The present invention relates to a kind of lightweight Organic-inorganic composite insulating foam and preparation methods, belong to complex function material
Expect technical field, is suitable for the thermal insulation material of refrigerator.
Background technology
In recent years, energy consumption of refrigerator occupies 10% or more of family's total energy consumption, and for domestic refrigerator, the heat preservation of babinet plays
Important role.The refrigerator of early stage is used as thermal insulation material usually using sponge, asbestos etc., but this kind of material heat-insulating capability is not
Height easily causes heat losses, causes energy consumption of refrigerator higher, and due to non-watertight, heat-insulating property is gradually lost in use
It loses.
Currently, the thermal insulation material of domestic refrigerator is mainly hard polyurethane foam material, thermal coefficient is about 0.03~
0.037W/(m·K).In order to keep the temperature, traditional method is to increase tank thickness, increases the thermal resistance of unit area, reduce refrigerator with it is outer
The effect of heat preservation energy-saving is played in the heat conduction of boundary's air.Meanwhile that there is also compressive strengths is low for pure polyurethane foam material, brittleness is big
Defect.Although in recent years, there is research to be modified enhancing to polyurethane foamed material to improve its compressive strength performance.But
It is after modified material is added, although improving the compressive strength of polyurethane foam, to reduce the porosity of polyurethane simultaneously, make
The heat-insulating property for obtaining polyurethane foam declines.
Therefore, a kind of Organic-inorganic composite heat preservation bubble of the refrigerator with high compression-strength and high insulating power is developed
Foam material is of great practical significance.
Invention content
In order to solve the problems, such as that refrigerator heat insulation material exists in the prior art, the invention discloses one kind to have highly resistance crisp
The refrigerator of performance and high insulating power lightweight Organic-inorganic composite insulating foam and preparation method.
To achieve the above objectives, the technical solution adopted by the present invention is：
A kind of lightweight Organic-inorganic composite insulating foam, the complex heat-preservation foamed material be by polyurethane foam,
Nano zeolite-porous fibre composite aerogel, modified mesoporous C-SiO2Nanosphere is compound to be prepared, the complex heat-preservation bubble
The compressive strength of foam material is not less than 250kPa, and thermal coefficient is not more than 0.02W/ (mK)；Wherein, the complex heat-preservation foam
The mass fraction of polyurethane foam is 60-70% in material, and the mass fraction of nano zeolite-porous fibre composite aerogel is
10-20%, surplus are modified mesoporous C-SiO2Nanosphere.
Preferably, the mass fraction of nano zeolite is 40-60% in the nano zeolite-porous fibre composite aerogel,
The grain size of nano zeolite is 70-90nm.
Preferably, the mesoporous C-SiO of the modification2SiO in nano material2Mass fraction is 12%, and the grain size of nanosphere is
100nm, specific surface area 548m2/g。
A kind of preparation method of above-mentioned complex heat-preservation foamed material, including：
(1) molecular sieve of Nano zeolite is prepared
After water and organic amine are mixed evenly, ethyl orthosilicate is added at room temperature with the speed of 300-500r/min
20-28h is stirred, after being aged 22-26h, addition aluminium isopropoxide continues stirring 22-26h with the speed of 500-700r/min and contained
Have the colloidal sol of silicon and aluminium, ethyl orthosilicate in the colloidal sol, organic amine, water and aluminium isopropoxide molal weight ratio be 1: 0.3~
0.35: 17.5~18.5: 0.003~0.004, the colloidal sol is carried out to microwave radiation technology aging reaction, the segmentation hydro-thermal of 48h successively
Crystallization, vacuum filtration, washing, 110 DEG C of drying obtain the molecular sieve of Nano zeolite that grain size is 80~100nm；Wherein, first
80 DEG C of section hydrothermal crystallizing temperature, crystallization time 90min；120 DEG C of second segment hydrothermal crystallizing temperature, crystallization time 30min；
(2) oxycellulose suspension is prepared
Lint cellulose is added in distilled water after ultrasonic disperse 5min, be added catalytic oxidant and sodium bromide stir to
Two substances dissolve, and the hypochlorite solutions of 0.1mol/L are then added dropwise, and can use hydrochloric acid or sodium hydroxide solution will be above-mentioned
Suspension pH value is adjusted to 10.0, and oxidation reaction is occurred with the speed of 500r/min stirring 2h at 4 DEG C, adds methanol, and
The pH value of suspension is adjusted to 7.0 formation suspensions, it is spare that suspension is disperseed suspension of the acquisition containing 5% oxycellulose；Wherein, cotton
The mass volume ratio of Down Fiber element and distilled water be 0.01g/mL, lint cellulose, catalytic oxidant, sodium bromide mass ratio be
125: 2: 40, distilled water, hypochlorite solutions, methanol volume ratio be 40: (8-9): 1；
(3) nano zeolite-porous fibre composite aerogel is prepared
Molecular sieve of Nano zeolite is uniformly dispersed in water to obtain zeolite suspension, zeolite suspension is added dropwise to
In the suspension of 5% oxycellulose, coupling and reaction that coupling agent carries out 4h is then added, after reaction, be centrifuged ,-
20 DEG C of vacuum freeze dryings obtain nano zeolite-porous fibre composite aerogel；Wherein, molecular sieve of Nano zeolite and 5% oxidation
The suspension of cellulose is 7: 200 in mass ratio, and the mass volume ratio of molecular sieve of Nano zeolite and water is 0.07g/mL, water and idol
The volume ratio for joining agent is 25: 1；
(4) mesoporous C-SiO is prepared2Nanosphere
It, will by the template triblock copolymer F127 F127 solution for standby soluble in water for forming a concentration of 0.064g/mL
Silicon source prehydrolysis 2h soluble in water forms the silicon source solution for standby of a concentration of 0.0076g/mL；Phenol is melted completely at 50 DEG C
After move into round-bottomed flask, sodium hydroxide solution is then added into round-bottomed flask, under 400r/min speed stir 10min mixing
Uniformly；37% formalin is added into round-bottomed flask again, and is warming up to 70 DEG C, thermotonus 30min is kept to obtain instead
Then the phenolic resin (Mw ＜ 500) of the low molecular weight of application is cooled to 66 DEG C, F127 solution is added, in 66 DEG C, 400r/min
Under the conditions of stir 2h, silicon source solution is added and continues to stir 12h under the conditions of 50 DEG C, 500r/min, be added toluene 60 DEG C,
Continue to stir 1h under the conditions of 600r/min, stand until the temperature of solution is down to room temperature in round-bottomed flask, then by round-bottomed flask
In solution be transferred to hydrothermal reaction kettle at a temperature of 110-140 DEG C hydro-thermal reaction for 24 hours, after the completion of reaction solution through cooling, take out
Obtained synthetic product, is then put into tube furnace, calcines 3h in a nitrogen atmosphere by filter, washing, dry acquisition synthetic product
It removes template and is carbonized, obtain orderly mesoporous C-SiO2Nanosphere；Wherein, phenol, triblock copolymer F127, silicon source
Mass ratio is 30: 48: 19, F127 solution, silicon source solution, sodium hydroxide solution, 37% formalin, the volume ratio of toluene are
150∶500∶150∶21∶10；
(5) modified mesoporous C-SiO is prepared2Nanosphere
The ethyl alcohol of 50mL and water are configured to alcohol solution by 1: 1 volume ratio, with the hydrochloric acid of 1mol/L by alcohol solution
PH value be adjusted to 5.0 to obtain mixed solution spare；By the mesoporous C-SiO of 5g2Nanosphere adds in the mixed solution, then will
It is transferred to 20min is handled in 50 DEG C of water-baths of ultrasonic wave and stirring, and the wherein power of ultrasonic wave is 10W, and stirring turns
Speed is 400r/min, and the surface modifier of 0.05g is then added dropwise, and continuation is stirred 2h, finally taken out under the same conditions
After filter, washing, dry, grinding, obtain being modified mesoporous C-SiO2Nanosphere；
(6) polyurethane foam is prepared
By 100 parts of multi-hydroxy polyethers, 6305,2 parts of foam stabilizers, 2.5 parts of catalyst 33LV, 12 parts of foaming agent F11,2 part 1,3-
Butanediol toughener is adjusted to 18 DEG C after mixing, by system temperature, 105 parts of polyisocyanate 44v20 is added together with
The speed of 800r/min is stirred 4h, obtains polyurethane foam；
(7) Organic-inorganic composite insulating foam is prepared
By the nano zeolite of corresponding parts by weight-porous fibre composite aerogel and modified mesoporous C-SiO2Nanosphere is added to
It is stirred 2h under the speed of 1000r/min in polyurethane foam, when having observed that bubble is emerged and foam whitens, immediately
Foam in injection aluminium-making mould, through swollen fixed, demoulding and after cure, obtain Organic-inorganic composite insulating foam, apparent density
For 0.42~0.45g/cm3；
Wherein, the step of preparation method be (1), (2), (3), (4), (5), (6), (7) or (1), (2), (3), (6),
(4), (5), (7) or (4), (5), (1), (2), (3), (6), (7) or (4), (5), (6), (1), (2), (3), (7) or (6),
(1), (2), (3), (4), (5), (7) or (6), (4), (5), (1), (2), (3), (7)；.(1), (2), (3) are nano zeolite-
The related preparation process of porous fibre composite aerogel, (4) and (5) are modified mesoporous C-SiO2The related of nanosphere prepares step
Suddenly, (6) are the related preparation process of polyurethane foam；
Preferably, organic amine described in (1) is tetraethyl amine or tetrapropyl amine.
Preferably, catalytic oxidant described in (2) is 2,2,6,6- tetramethyl piperidine -1- oxygroup free radicals, the secondary chlorine
Hydrochlorate is sodium hypochlorite.
Preferably, coupling agent described in (3) is (3- propyl mercaptan) trimethoxy silane.
Preferably, silicon source described in (4) is gamma-aminopropyl-triethoxy-silane, and the hydrothermal temperature is 130 DEG C,
The calcination temperature is 450 DEG C.
Preferably, surface modifier described in (4) and (5) is γ-(methacryloxypropyl) propyl trimethoxy silicane.
The present invention has following good effect compared with prior art：
(1), using novel porous fiber composite aeroge as the modifying agent of polyurethane foam, polyurethane foam is not only increased
Tensile strength, while ensure polyurethane foamed material have preferable heat-insulating property.
(2), pass through the mesoporous C-SiO of modification2Nanosphere is filled modification to polyurethane and further improves polyurethane foam
The heat-insulating property of foam.
Specific implementation mode
It is described below for disclosing the present invention so that those skilled in the art can realize the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Embodiment 1
A kind of preparation method of Organic-inorganic composite insulating foam, including：
(1) molecular sieve of Nano zeolite is prepared
After water and tetrapropyl amine are mixed evenly, ethyl orthosilicate is added and is stirred at room temperature with the speed of 400r/min
It mixes for 24 hours, after ageing for 24 hours, addition aluminium isopropoxide continues stirring with the speed of 600r/min and obtains the colloidal sol containing silicon and aluminium for 24 hours,
Ethyl orthosilicate in the colloidal sol, tetrapropyl amine, water and aluminium isopropoxide molal weight ratio be 1: 0.31: 17.5: 0.003, will
The colloidal sol carries out the microwave radiation technology aging reaction of 48h, the reaction of segmentation hydrothermal crystallizing, vacuum filtration, washing, 110 DEG C of bakings successively
It is dry to obtain the molecular sieve of Nano zeolite that grain size is 80-85nm；Wherein, 80 DEG C of first segment hydrothermal crystallizing temperature, crystallization time
90min；120 DEG C of second segment hydrothermal crystallizing temperature, crystallization time 30min；
(2) oxycellulose suspension is prepared
2g lint celluloses are added in 200mL distilled water after ultrasonic disperse 5min, are added the 2 of 32mg, 2,6,6- tetra-
The sodium bromide of methyl piperidine -1- oxygroups free radical and 0.64g stir the 0.1mol/L's that 40.5mL is then added dropwise to dissolving
The pH value of above-mentioned suspension is adjusted to 10.0 by liquor natrii hypochloritis with 0.1mol/L hydrochloric acid and sodium hydroxide solution, and at 4 DEG C with
Oxidation reaction occurs for the speed stirring 2h of 500r/min, adds 5mL methanol, and the hydrochloric acid and sodium hydroxide solution of 0.1mol/L
The pH value of suspension is adjusted to 7.0 formation suspensions, it is spare that suspension is disperseed suspension of the acquisition containing 5% oxycellulose；
(3) nano zeolite-porous fibre composite aerogel is prepared
3.5g molecular sieve of Nano zeolite is uniformly dispersed in 50mL water to obtain zeolite suspension, dropwise by zeolite suspension
It is added in the suspension for containing 5% oxycellulose to 100g, (3- propyl mercaptan) trimethoxy silane that 2mL is then added carries out
The coupling of 4h and reaction are centrifuged, that -20 DEG C of vacuum freeze dryings obtain nano zeolite-porous fibres is compound after reaction
Aeroge；
(4) mesoporous C-SiO is prepared2Nanosphere
0.96g template triblock copolymers F127 is dissolved in formed in 15mL water a concentration of 0.064g/mL F127 it is molten
Liquid is spare, and by the gamma-aminopropyl-triethoxy-silane of 0.38g, prehydrolysis 2h forms a concentration of 0.0076g/mL's in 50mL water
Silicon source solution for standby；Round-bottomed flask is moved into after 0.6g phenol is melted completely at 50 DEG C, is then added into round-bottomed flask
It is uniformly mixed to stir 10min under 400r/min speed for the sodium hydroxide solution of 15ml 0.1mol/L；Again into round-bottomed flask
37% formalin is added, and is warming up to 70 DEG C, thermotonus 30min is kept to obtain the phenolic aldehyde of the low molecular weight of reaction
Resin (Mw ＜ 500) is then cooled to 66 DEG C, and F127 solution is added, and 2h is stirred under the conditions of 66 DEG C, 400r/min, and silicon is added
Source solution continues to stir 12h under the conditions of 50 DEG C, 500r/min, and toluene is added and continues to stir under the conditions of 60 DEG C, 600r/min
1h, standing are down to room temperature up to the temperature of solution in round-bottomed flask, the solution in round-bottomed flask are then transferred to hydro-thermal reaction
For 24 hours, solution obtains synthetic product to hydro-thermal reaction to kettle through cooling, suction filtration, washing, drying after the completion of reaction, so at a temperature of 110 DEG C
Obtained synthetic product is put into tube furnace afterwards, 3h is calcined in a nitrogen atmosphere and removes surfactant and be carbonized, had
The mesoporous C-SiO of sequence2Nanosphere；Wherein, phenol, triblock copolymer F127, the mass ratio of silicon source are molten for 30: 48: 19, F127
Liquid, silicon source solution, sodium hydroxide solution, 37% formalin, the volume ratio of toluene are 150: 500: 150: 21: 10；Synthesis
Mixing speed in the process is particularly important to preparing uniform meso-porous nano ball, and the round-bottomed flask, hydro-thermal in certain step are anti-
Answer kettle, tube furnace etc. can be by instrument or equipment equivalent substitute with phase same-action；
(5) modified mesoporous C-SiO is prepared2Nanosphere
The ethyl alcohol of 50mL and water are configured to alcohol solution by 1: 1 volume ratio, with the hydrochloric acid of 1mol/L by alcohol solution
PH value be adjusted to 5.0 to obtain mixed solution spare；By the mesoporous C-SiO of 5g2Nanosphere adds in the mixed solution, then will
It is transferred to 20min is handled in 50 DEG C of water-baths of ultrasonic wave and stirring, and the wherein power of ultrasonic wave is 10W, and stirring turns
Speed is 400r/min, and the surface modifier of 0.05g is then added dropwise, and continuation is stirred 2h, finally taken out under the same conditions
After filter, washing, dry, grinding, obtain being modified mesoporous C-SiO2Nanosphere；
(6) polyurethane foam is prepared
By 100 parts of multi-hydroxy polyethers, 6305,2 parts of foam stabilizers, 2.5 parts of catalyst 33LV, 12 parts of foaming agent F11,2 part 1,3-
Butanediol toughener is adjusted to 18 DEG C after mixing, by system temperature, 105 parts of polyisocyanate 44v20 is added together with
The speed of 800r/min is stirred 4h, obtains polyurethane foam；
(7) Organic-inorganic composite insulating foam is prepared
By the mesoporous C-SiO of modification of the nano zeolite of 20 mass parts-porous fibre composite aerogel and 20 mass parts2Nanometer
Ball is added in the polyurethane foam of 60 mass parts and is stirred 2h under the speed of 1000r/min, when having observed that bubble emits
Go out and when foam whitens, inject in 200 × 200 × 100 aluminium-making mould and foam immediately, through swollen fixed, demoulding and after cure, obtain
Organic-inorganic composite insulating foam.In complex heat-preservation foamed material, shared by nano zeolite-porous fibre composite aerogel
Mass ratio score is 20%, modified mesoporous C-SiO2Mass ratio score shared by nanosphere is 20%, shared by polyurethane foam
Mass ratio score is 60%, and the apparent density of complex heat-preservation foamed material is 0.34g/cm3。
Embodiment 2
A kind of preparation method of Organic-inorganic composite insulating foam, including：
(1) molecular sieve of Nano zeolite is prepared
After water and tetrapropyl amine are mixed evenly, ethyl orthosilicate is added and is stirred at room temperature with the speed of 300r/min
20h is mixed, after being aged 26h, addition aluminium isopropoxide continues stirring 25h with the speed of 500r/min and obtains the colloidal sol containing silicon and aluminium,
Ethyl orthosilicate in the colloidal sol, tetrapropyl amine, water and aluminium isopropoxide molal weight ratio be 1: 0.35: 18.5: 0.003, will
The colloidal sol carries out the microwave radiation technology aging reaction of 48h, the reaction of segmentation hydrothermal crystallizing, vacuum filtration, washing, 110 DEG C of bakings successively
It is dry to obtain the molecular sieve of Nano zeolite that grain size is 85-90nm；Wherein, 80 DEG C of first segment hydrothermal crystallizing temperature, crystallization time
90min；120 DEG C of second segment hydrothermal crystallizing temperature, crystallization time 30min；
(2) oxycellulose suspension is prepared
2g lint celluloses are added in 200mL distilled water after ultrasonic disperse 5min, are added the 2 of 32mg, 2,6,6- tetra-
The sodium bromide of methyl piperidine -1- oxygroups free radical and 0.64g stir the 0.1mol/L's that 40.5mL is then added dropwise to dissolving
The pH value of above-mentioned suspension is adjusted to 10.0 by liquor natrii hypochloritis with 0.1mol/L hydrochloric acid and sodium hydroxide solution, and at 4 DEG C with
Oxidation reaction occurs for the speed stirring 2h of 500r/min, adds 5mL methanol, and the hydrochloric acid and sodium hydroxide solution of 0.1mol/L
The pH value of suspension is adjusted to 7.0 formation suspensions, it is spare that suspension is disperseed suspension of the acquisition containing 5% oxycellulose；
(3) nano zeolite-porous fibre composite aerogel is prepared
3.5g molecular sieve of Nano zeolite is uniformly dispersed in 50mL water to obtain zeolite suspension, dropwise by zeolite suspension
It is added in the suspension for containing 5% oxycellulose to 100g, (3- propyl mercaptan) trimethoxy silane that 2mL is then added carries out
The coupling of 4h and reaction are centrifuged, that -20 DEG C of vacuum freeze dryings obtain nano zeolite-porous fibres is compound after reaction
Aeroge；
(4) mesoporous C-SiO is prepared2Nanosphere
0.96g template triblock copolymers F127 is dissolved in formed in 15mL water a concentration of 0.064g/mL F127 it is molten
Liquid is spare, and by the gamma-aminopropyl-triethoxy-silane of 0.38g, prehydrolysis 2h forms a concentration of 0.0076g/mL's in 50mL water
Silicon source solution for standby；Round-bottomed flask is moved into after 0.6g phenol is melted completely at 50 DEG C, is then added into round-bottomed flask
It is uniformly mixed to stir 10min under 400r/min speed for the sodium hydroxide solution of 15ml 0.1mol/L；Again into round-bottomed flask
37% formalin is added, and is warming up to 70 DEG C, thermotonus 30min is kept to obtain the phenolic aldehyde of the low molecular weight of reaction
Resin (Mw ＜ 500) is then cooled to 66 DEG C, and F127 solution is added, and 2h is stirred under the conditions of 66 DEG C, 400r/min, and silicon is added
Source solution continues to stir 12h under the conditions of 50 DEG C, 500r/min, and toluene is added and continues to stir under the conditions of 60 DEG C, 600r/min
1h, standing are down to room temperature up to the temperature of solution in round-bottomed flask, the solution in round-bottomed flask are then transferred to hydro-thermal reaction
For 24 hours, solution obtains synthetic product to hydro-thermal reaction to kettle through cooling, suction filtration, washing, drying after the completion of reaction, so at a temperature of 120 DEG C
Obtained synthetic product is put into tube furnace afterwards, 3h is calcined in a nitrogen atmosphere and removes surfactant and be carbonized, had
The mesoporous C-SiO of sequence2Nanosphere；Wherein, phenol, triblock copolymer F127, the mass ratio of silicon source are molten for 30: 48: 19, F127
Liquid, silicon source solution, sodium hydroxide solution, 37% formalin, the volume ratio of toluene are 150: 500: 150: 21: 10；Synthesis
Mixing speed in the process is particularly important to preparing uniform meso-porous nano ball, and the round-bottomed flask, hydro-thermal in certain step are anti-
Answer kettle, tube furnace etc. can be by instrument or equipment equivalent substitute with phase same-action；
(5) modified mesoporous C-SiO is prepared2Nanosphere
The ethyl alcohol of 50mL and water are configured to alcohol solution by 1: 1 volume ratio, with the hydrochloric acid of 1mol/L by alcohol solution
PH value be adjusted to 5.0 to obtain mixed solution spare；By the mesoporous C-SiO of 5g2Nanosphere adds in the mixed solution, then will
It is transferred to 20min is handled in 50 DEG C of water-baths of ultrasonic wave and stirring, and the wherein power of ultrasonic wave is 10W, and stirring turns
Speed is 400r/min, and the surface modifier of 0.05g is then added dropwise, and continuation is stirred 2h, finally taken out under the same conditions
After filter, washing, dry, grinding, obtain being modified mesoporous C-SiO2Nanosphere；
(6) polyurethane foam is prepared
By 100 parts of multi-hydroxy polyethers, 6305,2 parts of foam stabilizers, 2.5 parts of catalyst 33LV, 12 parts of foaming agent F11,2 part 1,3-
Butanediol toughener is adjusted to 18 DEG C after mixing, by system temperature, 105 parts of polyisocyanate 44v20 is added together with
The speed of 800r/min is stirred 4h, obtains polyurethane foam；
(7) Organic-inorganic composite insulating foam is prepared
By the mesoporous C-SiO of modification of the nano zeolite of 10 mass parts-porous fibre composite aerogel and 30 mass parts2Nanometer
Ball is added in the polyurethane foam of 60 mass parts and is stirred 2h under the speed of 1000r/min, when having observed that bubble emits
Go out and when foam whitens, inject in 200 × 200 × 100 aluminium-making mould and foam immediately, through swollen fixed, demoulding and after cure, obtain
Organic-inorganic composite insulating foam.In complex heat-preservation foamed material, shared by nano zeolite-porous fibre composite aerogel
Mass ratio score is 10%, modified mesoporous C-SiO2Mass ratio score shared by nanosphere is 30%, shared by polyurethane foam
Mass ratio score is 60%, and the apparent density of complex heat-preservation foamed material is 0.33g/cm3。
Embodiment 3
A kind of preparation method of Organic-inorganic composite insulating foam, including：
(1) molecular sieve of Nano zeolite is prepared
After water and tetrapropyl amine are mixed evenly, ethyl orthosilicate is added and is stirred at room temperature with the speed of 500r/min
28h is mixed, after being aged 22h, addition aluminium isopropoxide continues stirring 26h with the speed of 700r/min and obtains the colloidal sol containing silicon and aluminium,
Ethyl orthosilicate in the colloidal sol, tetrapropyl amine, water and aluminium isopropoxide molal weight ratio be 1: 0.3: 17.5: 0.004, by institute
It states colloidal sol and carries out the microwave radiation technology aging reaction of 48h, the reaction of segmentation hydrothermal crystallizing, vacuum filtration, washing, 110 DEG C of drying successively
Obtain the molecular sieve of Nano zeolite that grain size is 90-95nm；Wherein, 80 DEG C of first segment hydrothermal crystallizing temperature, crystallization time 90min；
120 DEG C of second segment hydrothermal crystallizing temperature, crystallization time 30min；
(2) oxycellulose suspension is prepared
2g lint celluloses are added in 200mL distilled water after ultrasonic disperse 5min, are added the 2 of 32mg, 2,6,6- tetra-
The sodium bromide of methyl piperidine -1- oxygroups free radical and 0.64g stir the 0.1mol/L's that 40.5mL is then added dropwise to dissolving
The pH value of above-mentioned suspension is adjusted to 10.0 by liquor natrii hypochloritis with 0.1mol/L hydrochloric acid and sodium hydroxide solution, and at 4 DEG C with
Oxidation reaction occurs for the speed stirring 2h of 500r/min, adds 5mL methanol, and the hydrochloric acid and sodium hydroxide solution of 0.1mol/L
The pH value of suspension is adjusted to 7.0 formation suspensions, it is spare that suspension is disperseed suspension of the acquisition containing 5% oxycellulose；
(3) nano zeolite-porous fibre composite aerogel is prepared
3.5g molecular sieve of Nano zeolite is uniformly dispersed in 50mL water to obtain zeolite suspension, dropwise by zeolite suspension
It is added in the suspension for containing 5% oxycellulose to 100g, (3- propyl mercaptan) trimethoxy silane that 2mL is then added carries out
The coupling of 4h and reaction are centrifuged, that -20 DEG C of vacuum freeze dryings obtain nano zeolite-porous fibres is compound after reaction
Aeroge；
(4) mesoporous C-SiO is prepared2Nanosphere
0.96g template triblock copolymers F127 is dissolved in formed in 15mL water a concentration of 0.064g/mL F127 it is molten
Liquid is spare, and by the gamma-aminopropyl-triethoxy-silane of 0.38g, prehydrolysis 2h forms a concentration of 0.0076g/mL's in 50mL water
Silicon source solution for standby；Round-bottomed flask is moved into after 0.6g phenol is melted completely at 50 DEG C, is then added into round-bottomed flask
It is uniformly mixed to stir 10min under 400r/min speed for the sodium hydroxide solution of 15ml 0.1mol/L；Again into round-bottomed flask
37% formalin is added, and is warming up to 70 DEG C, thermotonus 30min is kept to obtain the phenolic aldehyde of the low molecular weight of reaction
Resin (Mw ＜ 500) is then cooled to 66 DEG C, and F127 solution is added, and 2h is stirred under the conditions of 66 DEG C, 400r/min, and silicon is added
Source solution continues to stir 12h under the conditions of 50 DEG C, 500r/min, and toluene is added and continues to stir under the conditions of 60 DEG C, 600r/min
1h, standing are down to room temperature up to the temperature of solution in round-bottomed flask, the solution in round-bottomed flask are then transferred to hydro-thermal reaction
For 24 hours, solution obtains synthetic product to hydro-thermal reaction to kettle through cooling, suction filtration, washing, drying after the completion of reaction, so at a temperature of 130 DEG C
Obtained synthetic product is put into tube furnace afterwards, 3h is calcined in a nitrogen atmosphere and removes surfactant and be carbonized, had
The mesoporous C-SiO of sequence2Nanosphere；Wherein, phenol, triblock copolymer F127, the mass ratio of silicon source are molten for 30: 48: 19, F127
Liquid, silicon source solution, sodium hydroxide solution, 37% formalin, the volume ratio of toluene are 150: 500: 150: 21: 10；Synthesis
Mixing speed in the process is particularly important to preparing uniform meso-porous nano ball, and the round-bottomed flask, hydro-thermal in certain step are anti-
Answer kettle, tube furnace etc. can be by instrument or equipment equivalent substitute with phase same-action；
(5) modified mesoporous C-SiO is prepared2Nanosphere
The ethyl alcohol of 50mL and water are configured to alcohol solution by 1: 1 volume ratio, with the hydrochloric acid of 1mol/L by alcohol solution
PH value be adjusted to 5.0 to obtain mixed solution spare；By the mesoporous C-SiO of 5g2Nanosphere adds in the mixed solution, then will
It is transferred to 20min is handled in 50 DEG C of water-baths of ultrasonic wave and stirring, and the wherein power of ultrasonic wave is 10W, and stirring turns
Speed is 400r/min, and the surface modifier of 0.05g is then added dropwise, and continuation is stirred 2h, finally taken out under the same conditions
After filter, washing, dry, grinding, obtain being modified mesoporous C-SiO2Nanosphere；
(6) polyurethane foam is prepared
By 100 parts of multi-hydroxy polyethers, 6305,2 parts of foam stabilizers, 2.5 parts of catalyst 33LV, 12 parts of foaming agent F11,2 part 1,3-
Butanediol toughener is adjusted to 18 DEG C after mixing, by system temperature, 105 parts of polyisocyanate 44v20 is added together with
The speed of 800r/min is stirred 4h, obtains polyurethane foam；
(7) Organic-inorganic composite insulating foam is prepared
By the mesoporous C-SiO of modification of the nano zeolite of 10 mass parts-porous fibre composite aerogel and 20 mass parts2Nanometer
Ball is added in the polyurethane foam of 70 mass parts and is stirred 2h under the speed of 1000r/min, when having observed that bubble emits
Go out and when foam whitens, inject in 200 × 200 × 100 aluminium-making mould and foam immediately, through swollen fixed, demoulding and after cure, obtain
Organic-inorganic composite insulating foam.In complex heat-preservation foamed material, shared by nano zeolite-porous fibre composite aerogel
Mass ratio score is 10%, modified mesoporous C-SiO2Mass ratio score shared by nanosphere is 20%, shared by polyurethane foam
Mass ratio score is 70%, and the apparent density of complex heat-preservation foamed material is 0.32g/cm3。
Embodiment 4
A kind of preparation method of Organic-inorganic composite insulating foam, including：
(1) molecular sieve of Nano zeolite is prepared
After water and tetrapropyl amine are mixed evenly, ethyl orthosilicate is added and is stirred at room temperature with the speed of 400r/min
26h is mixed, after being aged 26h, addition aluminium isopropoxide continues stirring 22h with the speed of 650r/min and obtains the colloidal sol containing silicon and aluminium,
Ethyl orthosilicate in the colloidal sol, tetrapropyl amine, water and aluminium isopropoxide molal weight ratio be 1: 0.33: 18: 0.004, by institute
It states colloidal sol and carries out the microwave radiation technology aging reaction of 48h, the reaction of segmentation hydrothermal crystallizing, vacuum filtration, washing, 110 DEG C of drying successively
Obtain the molecular sieve of Nano zeolite that grain size is 95-100nm；Wherein, 80 DEG C of first segment hydrothermal crystallizing temperature, crystallization time 90min；
120 DEG C of second segment hydrothermal crystallizing temperature, crystallization time 30min；
(2) oxycellulose suspension is prepared
2g lint celluloses are added in 200mL distilled water after ultrasonic disperse 5min, are added the 2 of 32mg, 2,6,6- tetra-
The sodium bromide of methyl piperidine -1- oxygroups free radical and 0.64g stir the 0.1mol/L's that 40.5mL is then added dropwise to dissolving
The pH value of above-mentioned suspension is adjusted to 10.0 by liquor natrii hypochloritis with 0.1mol/L hydrochloric acid and sodium hydroxide solution, and at 4 DEG C with
Oxidation reaction occurs for the speed stirring 2h of 500r/min, adds 5mL methanol, and the hydrochloric acid and sodium hydroxide solution of 0.1mol/L
The pH value of suspension is adjusted to 7.0 formation suspensions, it is spare that suspension is disperseed suspension of the acquisition containing 5% oxycellulose；
(3) nano zeolite-porous fibre composite aerogel is prepared
3.5g molecular sieve of Nano zeolite is uniformly dispersed in 50mL water to obtain zeolite suspension, dropwise by zeolite suspension
It is added in the suspension for containing 5% oxycellulose to 100g, (3- propyl mercaptan) trimethoxy silane that 2mL is then added carries out
The coupling of 4h and reaction are centrifuged, that -20 DEG C of vacuum freeze dryings obtain nano zeolite-porous fibres is compound after reaction
Aeroge；
(4) mesoporous C-SiO is prepared2Nanosphere
0.96g template triblock copolymers F127 is dissolved in formed in 15mL water a concentration of 0.064g/mL F127 it is molten
Liquid is spare, and by the gamma-aminopropyl-triethoxy-silane of 0.38g, prehydrolysis 2h forms a concentration of 0.0076g/mL's in 50mL water
Silicon source solution for standby；Round-bottomed flask is moved into after 0.6g phenol is melted completely at 50 DEG C, is then added into round-bottomed flask
It is uniformly mixed to stir 10min under 400r/min speed for the sodium hydroxide solution of 15ml 0.1mol/L；Again into round-bottomed flask
37% formalin is added, and is warming up to 70 DEG C, thermotonus 30min is kept to obtain the phenolic aldehyde of the low molecular weight of reaction
Resin (Mw ＜ 500) is then cooled to 66 DEG C, and F127 solution is added, and 2h is stirred under the conditions of 66 DEG C, 400r/min, and silicon is added
Source solution continues to stir 12h under the conditions of 50 DEG C, 500r/min, and toluene is added and continues to stir under the conditions of 60 DEG C, 600r/min
1h, standing are down to room temperature up to the temperature of solution in round-bottomed flask, the solution in round-bottomed flask are then transferred to hydro-thermal reaction
For 24 hours, solution obtains synthetic product to hydro-thermal reaction to kettle through cooling, suction filtration, washing, drying after the completion of reaction, so at a temperature of 140 DEG C
Obtained synthetic product is put into tube furnace afterwards, 3h is calcined in a nitrogen atmosphere and removes surfactant and be carbonized, had
The mesoporous C-SiO of sequence2Nanosphere；Wherein, phenol, triblock copolymer F127, the mass ratio of silicon source are molten for 30: 48: 19, F127
Liquid, silicon source solution, sodium hydroxide solution, 37% formalin, the volume ratio of toluene are 150: 500: 150: 21: 10；Synthesis
Mixing speed in the process is particularly important to preparing uniform meso-porous nano ball, and the round-bottomed flask, hydro-thermal in certain step are anti-
Answer kettle, tube furnace etc. can be by instrument or equipment equivalent substitute with phase same-action；
(5) modified mesoporous C-SiO is prepared2Nanosphere
The ethyl alcohol of 50mL and water are configured to alcohol solution by 1: 1 volume ratio, with the hydrochloric acid of 1mol/L by alcohol solution
PH value be adjusted to 5.0 to obtain mixed solution spare；By the mesoporous C-SiO of 5g2Nanosphere adds in the mixed solution, then will
It is transferred to 20min is handled in 50 DEG C of water-baths of ultrasonic wave and stirring, and the wherein power of ultrasonic wave is 10W, and stirring turns
Speed is 400r/min, and the surface modifier of 0.05g is then added dropwise, and continuation is stirred 2h, finally taken out under the same conditions
After filter, washing, dry, grinding, obtain being modified mesoporous C-SiO2Nanosphere；
(6) polyurethane foam is prepared
By 100 parts of multi-hydroxy polyethers, 6305,2 parts of foam stabilizers, 2.5 parts of catalyst 33LV, 12 parts of foaming agent F11,2 part 1,3-
Butanediol toughener is adjusted to 18 DEG C after mixing, by system temperature, 105 parts of polyisocyanate 44v20 is added together with
The speed of 800r/min is stirred 4h, obtains polyurethane foam；
(7) Organic-inorganic composite insulating foam is prepared
By the mesoporous C-SiO of modification of the nano zeolite of 15 mass parts-porous fibre composite aerogel and 25 mass parts2Nanometer
Ball is added in the polyurethane foam of 60 mass parts and is stirred 2h under the speed of 1000r/min, when having observed that bubble emits
Go out and when foam whitens, inject in 200 × 200 × 100 aluminium-making mould and foam immediately, through swollen fixed, demoulding and after cure, obtain
Organic-inorganic composite insulating foam.In complex heat-preservation foamed material, shared by nano zeolite-porous fibre composite aerogel
Mass ratio score is 15%, modified mesoporous C-SiO2Mass ratio score shared by nanosphere is 25%, shared by polyurethane foam
Mass ratio score is 60%, and the apparent density of complex heat-preservation foamed material is 0.35g/cm3。
Masters of the establishing criteria QB/T 2081-1995 to the Organic-inorganic composite insulating foam obtained by embodiment 1-4
Performance is wanted to be tested, the results are shown in Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Apparent density (g/cm3) | 0.34 | 0.33 | 0.32 | 0.35 |
| Compressive strength (kPa) | 256 | 252 | 259 | 263 |
| Thermal coefficient (W/ (mK)) | 0.019 | 0.018 | 0.017 | 0.019 |
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection domain by appended claims and its
Equivalent defines.
Claims (8)
1. a kind of lightweight Organic-inorganic composite insulating foam, it is characterised in that：The complex heat-preservation foamed material is by gathering
Urethane foam, nano zeolite-porous fibre composite aerogel, modified mesoporous C-SiO2Nanosphere is compound to be prepared, described
The compressive strength of complex heat-preservation foamed material is not less than 250kPa, and thermal coefficient is not more than 0.02W/ (mK)；Wherein, described multiple
The mass fraction for closing polyurethane foam in insulating foam is 60-70%, the matter of nano zeolite-porous fibre composite aerogel
Amount score is 10-20%；
Wherein, the preparation method of the complex heat-preservation foamed material, including：
(1) molecular sieve of Nano zeolite is prepared
After water and organic amine are mixed evenly, ethyl orthosilicate is added and is stirred at room temperature with the speed of 300-500r/min
20-28h, after being aged 22-26h, addition aluminium isopropoxide continues stirring 22-26h with the speed of 500-700r/min and obtains containing silicon
With the colloidal sol of aluminium, ethyl orthosilicate in the colloidal sol, organic amine, water and aluminium isopropoxide molal weight ratio be 1:0.3-0.35:
17.5-18.5:0.003-0.004, microwave radiation technology aging reaction, the segmentation hydrothermal crystallizing that the colloidal sol is carried out to 48h successively are anti-
It answers, be filtered by vacuum, washing, 110 DEG C of drying obtain the molecular sieve of Nano zeolite that grain size is 80-100nm；Wherein, first segment hydro-thermal
80 DEG C of crystallization temperature, crystallization time 90min；120 DEG C of second segment hydrothermal crystallizing temperature, crystallization time 30min；
(2) oxycellulose suspension is prepared
Lint cellulose is added in distilled water after ultrasonic disperse 5min, catalytic oxidant is added and sodium bromide is stirred to molten
Solution, is then added dropwise the hypochlorite solutions of 0.1mol/L, suspension pH value is adjusted to 10.0, and with 500r/min at 4 DEG C
Speed stirring 2h occur oxidation reaction, add methanol, and the pH value of suspension is adjusted to 7.0 formation suspensions, suspension disperseed
It is spare to obtain the suspension containing 5% oxycellulose；Wherein, the mass volume ratio of lint cellulose and distilled water is 0.01g/
ML, lint cellulose, catalytic oxidant, sodium bromide mass ratio be 125:2:40, distilled water, hypochlorite solutions, methanol
Volume ratio is 40：(8-9)：1；
(3) nano zeolite-porous fibre composite aerogel is prepared
Molecular sieve of Nano zeolite is uniformly dispersed in water to obtain zeolite suspension, zeolite suspension is added dropwise to 5% oxygen
In the suspension of cellulose, coupling and reaction that coupling agent carries out 4h is then added, after reaction, be centrifuged, -20 DEG C it is true
Vacuum freecing-dry obtains nano zeolite-porous fibre composite aerogel；Wherein, molecular sieve of Nano zeolite and 5% oxycellulose
Suspension mass ratio be 7:200, the mass volume ratio of molecular sieve of Nano zeolite and water is 0.07g/mL, the body of water and coupling agent
Product is than being 25:1；
(4) mesoporous C-SiO is prepared2Nanosphere
By the template triblock copolymer F127 F127 solution for standby soluble in water for forming a concentration of 0.064g/mL, by silicon source
Prehydrolysis 2h soluble in water forms the silicon source solution for standby of a concentration of 0.0076g/mL；It is moved after phenol is melted completely at 50 DEG C
Enter round-bottomed flask, sodium hydroxide solution is then added into round-bottomed flask, it is equal that 10min mixing is stirred under 400r/min speed
It is even；37% formalin is added into round-bottomed flask again, and is warming up to 70 DEG C, thermotonus 30min is kept to be reacted
The phenolic resin of low molecular weight, wherein then the Mw ＜ 500 of phenolic resin are cooled to 66 DEG C, F127 solution is added,
66 DEG C, 2h is stirred under the conditions of 400r/min, silicon source solution is added and continues to stir 12h under the conditions of 50 DEG C, 500r/min, first is added
Benzene continues to stir 1h under the conditions of 60 DEG C, 600r/min, and standing is down to room temperature up to the temperature of solution in round-bottomed flask, then will
Solution in round-bottomed flask is transferred to hydrothermal reaction kettle, and for 24 hours, solution passes through hydro-thermal reaction after the completion of reaction at a temperature of 110-140 DEG C
Obtained synthetic product, is then put into tube furnace, in a nitrogen atmosphere by cooling, suction filtration, washing, dry acquisition synthetic product
Calcining 3h removes template and is carbonized, and obtains orderly mesoporous C-SiO2Nanosphere；Wherein, phenol, triblock copolymer F127,
The mass ratio of silicon source is 30:48:The body of 19, F127 solution, silicon source solution, sodium hydroxide solution, 37% formalin, toluene
Product is than being 150:500:150:21:10；
(5) modified mesoporous C-SiO is prepared2Nanosphere
The ethyl alcohol of 50mL and water are pressed 1:1 volume ratio is configured to alcohol solution, with the hydrochloric acid of 1mol/L by the pH of alcohol solution
Value is adjusted to 5.0, and to obtain mixed solution spare；By the mesoporous C-SiO of 5g2Nanosphere adds in the mixed solution, then by its turn
It moves to 20min is handled in 50 DEG C of water-baths of ultrasonic wave and stirring, the wherein power of ultrasonic wave is 10W, and the rotating speed of stirring is
400r/min, is then added dropwise the surface modifier of 0.05g, and continuation stirs 2h, finally filtered, washed under the same conditions
After washing, dry, grinding, obtain being modified mesoporous C-SiO2Nanosphere；
(6) polyurethane foam is prepared
By 100 parts of multi-hydroxy polyethers, 6305,2 parts of foam stabilizers, 2.5 parts of catalyst 33LV, 12 parts of foaming agent F11,2 parts of 1,3- fourths two
Alcohol toughener is adjusted to 18 DEG C after mixing, by system temperature, and 105 parts of polyisocyanate 44v20 is added together with 800r/
The speed of min is stirred 4h, obtains polyurethane foam；
(7) Organic-inorganic composite insulating foam is prepared
By the nano zeolite of corresponding parts by weight-porous fibre composite aerogel and modified mesoporous C-SiO2Nanosphere is added to poly- ammonia
It is stirred 2h under the speed of 1000r/min in ester foam, when having observed that bubble is emerged and foam whitens, is injected immediately
Foam in aluminium-making mould, through swollen fixed, demoulding and after cure, obtain Organic-inorganic composite insulating foam, apparent density is
0.42~0.45g/cm3；
Wherein, the step of preparation method be (1), (2), (3), (4), (5), (6), (7) or (1), (2), (3), (6), (4),
(5), (7) or (4), (5), (1), (2), (3), (6), (7) or (4), (5), (6), (1), (2), (3), (7) or (6), (1),
(2), (3), (4), (5), (7) or (6), (4), (5), (1), (2), (3), (7).
2. complex heat-preservation foamed material as described in claim 1, it is characterised in that：The compound gas of nano zeolite-porous fibre
The mass fraction of nano zeolite is 40-60% in gel, and the grain size of nano zeolite is 70-90nm.
3. complex heat-preservation foamed material as described in claim 1, it is characterised in that：The mesoporous C-SiO of modification2In nanosphere
SiO2Mass fraction is 12%, and the grain size of nanosphere is 100nm, specific surface area 548m2/g。
4. complex heat-preservation foamed material as described in claim 1, it is characterised in that：Organic amine described in step (1) is tetraethyl
Amine or tetrapropyl amine.
5. complex heat-preservation foamed material as described in claim 1, it is characterised in that：Catalytic oxidant described in step (2) is 2,
2,6,6- tetramethyl piperidine -1- oxygroup free radicals, the hypochlorite are sodium hypochlorite.
6. complex heat-preservation foamed material as described in claim 1, it is characterised in that：Coupling agent described in step (3) is (3- propyl
Mercaptan) trimethoxy silane.
7. complex heat-preservation foamed material as described in claim 1, it is characterised in that：Silicon source described in step (4) is γ-aminopropyl
Triethoxysilane, the hydrothermal temperature are 130 DEG C, and the calcination temperature is 450 DEG C.
8. complex heat-preservation foamed material as described in claim 1, it is characterised in that：Surface modifier described in step (5) is γ-
(methacryloxypropyl) propyl trimethoxy silicane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610290386.3A CN105968789B (en) | 2016-04-27 | 2016-04-27 | A kind of lightweight Organic-inorganic composite insulating foam and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610290386.3A CN105968789B (en) | 2016-04-27 | 2016-04-27 | A kind of lightweight Organic-inorganic composite insulating foam and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105968789A CN105968789A (en) | 2016-09-28 |
| CN105968789B true CN105968789B (en) | 2018-07-24 |
Family
ID=56994450
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610290386.3A Expired - Fee Related CN105968789B (en) | 2016-04-27 | 2016-04-27 | A kind of lightweight Organic-inorganic composite insulating foam and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105968789B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135547A (en) * | 2018-07-12 | 2019-01-04 | 田秋珍 | A kind of insulation and fire-proof paint |
| CN111591612A (en) * | 2020-05-25 | 2020-08-28 | 湖北三江航天万峰科技发展有限公司 | For military use wave prevention heat preservation fortune water pitcher |
| CN111793187A (en) * | 2020-08-04 | 2020-10-20 | 湖南省普瑞达内装材料有限公司 | High-density high-thermal conductivity polyurethane foam and preparation method thereof |
| CN116102779A (en) * | 2023-01-10 | 2023-05-12 | 南京大毛牛环保科技有限公司 | Low-heat-conductivity flexible heat-insulating foam and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422965A (en) * | 2007-10-29 | 2009-05-06 | 成都思摩纳米技术有限公司 | Composite incubation material |
| CN102219460A (en) * | 2011-03-16 | 2011-10-19 | 广西大学 | Organic and inorganic composite insulation material |
| CN104629080A (en) * | 2015-03-06 | 2015-05-20 | 武汉理工大学 | Method for synthesizing ZIF-8 aerogel on basis of cellulose hard template |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03239753A (en) * | 1990-02-19 | 1991-10-25 | Kao Corp | Water-absorbing polyurethane foam and production thereof |
-
2016
- 2016-04-27 CN CN201610290386.3A patent/CN105968789B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422965A (en) * | 2007-10-29 | 2009-05-06 | 成都思摩纳米技术有限公司 | Composite incubation material |
| CN102219460A (en) * | 2011-03-16 | 2011-10-19 | 广西大学 | Organic and inorganic composite insulation material |
| CN104629080A (en) * | 2015-03-06 | 2015-05-20 | 武汉理工大学 | Method for synthesizing ZIF-8 aerogel on basis of cellulose hard template |
Non-Patent Citations (2)
| Title |
|---|
| "C/SiO2复合微纳米粒增强环氧树脂";吕文晏等，;《化工新型材料》;20121215;第40卷(第12期);第126-128页 * |
| "块状低密度C/SiO2复合气凝胶的制备";孔勇等，;《南京工业大学学报》;20120731;第34卷(第4期);第6-10页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105968789A (en) | 2016-09-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105968789B (en) | A kind of lightweight Organic-inorganic composite insulating foam and preparation method | |
| CN107312166B (en) | A kind of modified PET polyester and its preparation method and application | |
| CN107263948B (en) | A kind of fire-proof thermal-insulation decoration and preparation method thereof | |
| CN107325328A (en) | A kind of preparation method of graphene/silicon dioxide compound particle | |
| CN115259828A (en) | Method for preparing carbon fiber and carbon nanotube composite silicon aerogel through freeze drying | |
| CN106810139A (en) | A kind of method that ultrasonic wave added prepares hydrophobic silica aerogel composite | |
| CN105367032A (en) | Preparation method of nano heat preservation board | |
| CN103553487B (en) | A kind of Composite lightweight thermal insulation material and preparation method thereof | |
| CN106084771A (en) | A kind of automobile plastic lightweight modified nylon materials | |
| CN108546031A (en) | A kind of preparation method of foam concrete | |
| CN102219930B (en) | Calcium sulfate whisker surface modification technology | |
| CN111560172A (en) | Biomass fiber reinforced organic silicon aerogel composite material and preparation method and application thereof | |
| CN108484097B (en) | Preparation method of lignin-enhanced silicon dioxide aerogel felt | |
| CN106046675B (en) | A kind of vacuum heat-insulating plate composite core material and preparation method | |
| CN114105674B (en) | Composite board with heat preservation function and preparation method thereof | |
| CN111807808B (en) | Preparation method of high-temperature-resistant heat-insulation composite material | |
| CN114538956B (en) | Perlite mixed flame-retardant thermal-insulation material and production process thereof | |
| CN106517893A (en) | Heat-insulation concrete additive material containing hollow glass beads filled with nitrogen | |
| CN106588078A (en) | Foam concrete heat insulation board with air purifying function for roof and preparation method thereof | |
| CN113292283A (en) | Activated wet tuff particle thermal insulation wall material and manufacturing method thereof | |
| CN115353700B (en) | High-strength nano aerogel building material and preparation method thereof | |
| CN115626837B (en) | Heat-insulating energy-saving material for building and preparation method thereof | |
| CN104944864A (en) | Thermal insulation glazed hollow bead mortar with good construction performance and manufacturing method thereof | |
| CN115651160B (en) | Thermal insulation polyurethane sandwich template and preparation method thereof | |
| CN115477318B (en) | Method for preparing complete block-shaped pure alumina aerogel by freeze drying |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180614 Address after: 528427 Nantou Town, Zhongshan, Guangdong, min an industrial zone Applicant after: Zhongshan Taiyuan packing material Co.,Ltd. Address before: 315040 B3 building, R & D Park, Ningbo hi tech Development Zone, Zhejiang 509-512 Applicant before: NINGBO XIAYUAN TECHNOLOGY Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Lightweight organic inorganic composite thermal insulation foam material and preparation method thereof Effective date of registration: 20211130 Granted publication date: 20180724 Pledgee: China Co. truction Bank Corp Zhongshan branch Pledgor: Zhongshan Taiyuan packing material Co.,Ltd. Registration number: Y2021980013622 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180724 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |