CN113800808A - Preparation method of aerogel dispersible particles, prepared aerogel particles and application - Google Patents
Preparation method of aerogel dispersible particles, prepared aerogel particles and application Download PDFInfo
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- CN113800808A CN113800808A CN202110857613.7A CN202110857613A CN113800808A CN 113800808 A CN113800808 A CN 113800808A CN 202110857613 A CN202110857613 A CN 202110857613A CN 113800808 A CN113800808 A CN 113800808A
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- aerogel
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- 239000004964 aerogel Substances 0.000 title claims abstract description 146
- 239000002245 particle Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 27
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000008187 granular material Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000005453 pelletization Methods 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 17
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 239000010949 copper Substances 0.000 claims description 17
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 16
- 229920000570 polyether Polymers 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 9
- 230000003179 granulation Effects 0.000 claims description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 9
- 235000011152 sodium sulphate Nutrition 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 6
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 150000002191 fatty alcohols Chemical class 0.000 claims description 6
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 6
- 229920005646 polycarboxylate Polymers 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 230000002093 peripheral effect Effects 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- 125000002877 alkyl aryl group Chemical group 0.000 claims description 2
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 2
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 239000000230 xanthan gum Substances 0.000 claims description 2
- 229920001285 xanthan gum Polymers 0.000 claims description 2
- 235000010493 xanthan gum Nutrition 0.000 claims description 2
- 229940082509 xanthan gum Drugs 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000000428 dust Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 39
- 239000004965 Silica aerogel Substances 0.000 description 33
- 230000002209 hydrophobic effect Effects 0.000 description 15
- 239000000654 additive Substances 0.000 description 6
- 125000001165 hydrophobic group Chemical group 0.000 description 6
- 239000000741 silica gel Substances 0.000 description 6
- 229910002027 silica gel Inorganic materials 0.000 description 6
- 230000009471 action Effects 0.000 description 3
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- 239000010451 perlite Substances 0.000 description 2
- 235000019362 perlite Nutrition 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 210000002249 digestive system Anatomy 0.000 description 1
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- 229910003472 fullerene Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 231100000563 toxic property Toxicity 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a preparation method of aerogel dispersible granules, which is characterized in that firstly, aerogel powder is made into a master batch, and the preparation method comprises the following steps: firstly, slowly adding a filler 1 into deionized water, and uniformly mixing in a stirrer; secondly, adding a filler 2 into the step one; thirdly, slowly adding the filler 3 into the mixed step two, uniformly mixing in a stirrer, and sealing for later use; fourthly, taking aerogel powder, adding the aerogel powder into the solution obtained in the second step for a small number of times, stirring, stopping when the intermediate temperature rises, continuing to add the aerogel after cooling, stirring, and finally completely mixing the aerogel powder with the components obtained in the third step to obtain a master batch; and (3) feeding the master batch prepared according to the formula into a mixer through a feeder, mixing, and drying. The invention also provides the aerogel dispersible particles and application. The invention has the advantages that: the process is simple and convenient to popularize; the high-content aerogel prepared by the method has good dispersion particle dispersibility, uniform particle size, low probability of breakage and no dust in use.
Description
Technical Field
The present invention relates to a method for preparing aerogels, in particular to a method for preparing dispersible particles of aerogels.
Background
Aerogel is the best solid heat insulation material (thermal conductivity coefficient is 0.013W/m.k) in the known world, is invented by U.S. Kistler.S. in 1931, creates 15 guines records because of light and thin fog and bluish color, also called as 'blue smoke' and 'frozen smoke', is known as one of ten new materials for changing the world together with graphene, fullerene and the like, is also the lightest solid material in the world, has outstanding performance in the fields of thermal, optical, electrical, mechanical, acoustic and the like, is one of 10 hot scientific technologies listed in the 90 s of the 20 th century, and is a military and civil dual-purpose technology with great application value. At present, the aerogel taking silicon as a basic material has no carcinogenic or toxic properties. However, silicone aerogels can irritate the eyes, skin, respiratory tract, and digestive system of humans and can cause dryness of the skin mucosa upon contact.
Disclosure of Invention
The technical problem to be solved by the invention is how to avoid dust pollution when the aerogel particles are used.
The invention solves the technical problems through the following technical means: a method for preparing aerogel dispersible granules, firstly preparing aerogel powder into a master batch, comprising the following steps:
step one, slowly adding a filler 1 into deionized water, wherein the filler 1 is one or a mixture of fatty alcohol polyether, polycarboxylate compound and EO/PO block polyether, and uniformly mixing in a stirrer;
step two, adding a filler 2 into the step one, wherein the filler 2 is one or a mixture of sodium chloride and sodium sulfate;
step three, slowly adding a filler 3 into the mixed step two, wherein the filler 3 is one or more of alkyl sulfate, a naphthalene sulfonic acid formaldehyde condensate, alkylaryl polyoxyethylene polyoxypropylene ether, an alkyl sulfonate anionic surfactant, polyvinyl alcohol, starch ether, xanthan gum, polyvinylpyrrolidone, a poly (alkenyl polyether) crosslinked acrylic acid polymer and cellulose polyether, uniformly mixing in a stirrer, and sealing for later use;
step four, taking aerogel powder, adding the aerogel powder into the solution obtained in the step two for a small number of times, stirring, stopping when the intermediate temperature rises, continuing to add the aerogel after cooling, stirring, and finally completely mixing all the aerogel powder with the components obtained in the step three to obtain a master batch;
the process for the aerogel dispersible granules is as follows:
and (3) feeding the prepared master batch into a mixer through a feeder to mix, and then putting the mixture into an oven to be dried at the temperature of 100-150 ℃ to obtain the aerogel dispersible particles.
The aerogel used in the invention is silica gel, and as a plurality of hydrophobic groups are introduced into the molecules of the silica aerogel, the hydrophobicity of the silica aerogel is particularly strong, the powdery aerogel is difficult to be mixed with water by a common method to prepare aerogel dispersible particles, and the invention provides a method for fully mixing the hydrophobic silica aerogel with water and other additives. Most of the silica aerogel products on the market today are aerogel powders, and the present invention makes hydrophobic silica aerogel powders into high content aerogel dispersible particles for the first time. According to the invention, the aerogel powder is processed into aerogel particles, so that the situation that dust floats everywhere is avoided, and the stimulation and the damage to a human body are avoided.
The cellulose polyether in the third step is any one of hydroxyethyl cellulose, hydroxymethyl cellulose, carboxymethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose and lignocellulose.
As an optimized technical scheme, in the first step, the temperature of the stirrer is controlled to be 20-30 ℃, the rotating speed is 1000rpm/min, in the third step, the temperature of the stirrer is controlled to be 20-30 ℃, the rotating speed is 2500rpm/min, and in the fourth step, the temperature of the stirrer is always controlled to be 20-30 ℃, and the rotating speed is 3000 rpm/min.
As an optimized technical scheme, the mass ratio of the raw materials used for preparation is as follows:
silicon aerogel: 5 to 98 percent of the total weight of the steel,
packing 1: 0.2 to 10 percent of the total weight of the composition,
and (3) filler 2: 0.02 to 1 percent of the total weight of the alloy,
and (3) filler: 0.2 to 10 percent of the total weight of the composition,
water is added to make up to 100%.
As the technical scheme who optimizes, the cell type blendor includes the blendor main part, the control panel, the charge door, the eccentric swage, the pelletization sword, the pelletization net circle, the dispersion impeller, the discharge gate, the baffle, the copper pipe, the electrical control part is located the blendor main part, the control panel sets up in one side of blendor main part top, the charge door is located the opposite side of blendor main part top, the charge door is with the peripheral fixed connection who is located the pelletization net circle of its below, and charge door and the inside intercommunication of pelletization net circle, the pelletization sword sets up inside the pelletization net circle, the dispersion impeller encircles the outside that sets up at the pelletization net circle, one side of dispersion impeller is provided with the discharge gate, the baffle of slope is installed to the discharge gate, the copper pipe that has a lot of holes has been designed on the upper portion of baffle.
As an optimized technical scheme, the process of mixing materials in the groove-type mixer is as follows:
the diameter size of the dispersible granule of size regulation aerogel through the different pelletization net ring particle diameters of adjustment is through the eccentric swage, presses the masterbatch to the pelletization edge of a knife, extrudees the granulation through the effort between pelletization sword and the pelletization net, and on the material fell into rotatory dispersion impeller after the granulation, through rotatory, conveyed the material to the discharge gate.
As an optimized technical scheme, the inclined baffle is arranged at the discharge port, a copper pipe with a plurality of holes is designed at the upper part of the baffle, the copper pipe is connected with compressed air, and materials at the discharge port are blown under the action of air pressure, so that the materials at the discharge port are prevented from being accumulated.
As an optimized technical scheme, a rotatable rotating cage is arranged below a discharge port, and materials passing through the rotating cage enter a tray from the discharge port.
The invention also provides aerogel dispersible particles prepared by the preparation method of the aerogel dispersible particles according to any one of the above schemes.
The invention also provides application of the aerogel dispersible particles prepared by the preparation method of the aerogel dispersible particles in the scheme to a heat insulation plate.
The invention also provides application of the aerogel dispersible particles prepared by the preparation method of the aerogel dispersible particles in a coating.
The invention has the advantages that: the granulation method of the high-content aerogel dispersed particles provided by the invention has the advantages of simple process, less equipment investment and convenience for popularization; in addition, the high-content aerogel dispersed particles prepared by the method have the advantages of good dispersibility, uniform particle size, low possibility of being broken, no dust in use and the like.
Drawings
FIG. 1 is a front view of a trough mixer according to an embodiment of the present invention;
FIG. 2 is a top view of a trough mixer according to an embodiment of the present invention;
FIG. 3 is a side view of a trough mixer according to an embodiment of the present invention;
FIG. 4 is a diagram showing the copper pipe and baffle plate of the trough type mixer in accordance with the present invention;
FIG. 5 is a schematic view of a rotating cage of a trough mixer according to an embodiment of the present invention;
fig. 6 is a schematic view illustrating that the aerogel dispersible particles prepared according to the embodiment of the present invention are applied to an insulation board.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the aerogel particles prepared in this example required the following ingredients:
1000g of water, 5g of fatty alcohol polyether, 0.5g of sodium chloride, 5g of lignocellulose and 690g of aerogel powder.
The preparation method of the aerogel particles provided in this example is as follows:
firstly, aerogel powder is made into a master batch, and the method comprises the following steps:
step one, slowly adding 5g of fatty alcohol polyether into 1000g of deionized water, controlling the temperature of a stirrer at 20 ℃, rotating at 1000rpm/min, and uniformly mixing;
step two, adding 0.5g of sodium chloride into the step one;
step three, slowly adding 5g of lignocellulose into the mixed step two, controlling the temperature of a stirrer at 30 ℃, rotating speed at 2500rpm/min, uniformly mixing, and sealing for later use;
and step four, controlling the temperature to be 20 ℃ all the time, taking 690g of aerogel powder, rotating the stirrer at 3000rpm/min, adding the aerogel powder into the solution in the step two for a small number of times, stopping the temperature rise in the middle, continuing to add the aerogel powder after the temperature is reduced, stirring, and finally completely mixing 690g of aerogel powder with the components in the step three to form the master batch.
The aerogel used in the invention is silica gel, and as a plurality of hydrophobic groups are introduced into the molecules of the silica aerogel, the hydrophobicity of the silica aerogel is particularly strong, the powdery aerogel is difficult to be mixed with water by a common method to prepare aerogel dispersible particles, and the invention provides a method for fully mixing the hydrophobic silica aerogel with water and other additives.
Most of the currently marketed silica aerogel products are aerogel powders, and the hydrophobic silica aerogel powders are first prepared into high-content aerogel dispersible particles according to the present invention, and referring to fig. 1 to 5, the preparation method of the aerogel dispersible particles is as follows:
the masterbatch prepared by the fourth step is fed into a groove type mixer shown in fig. 1 through a feeder, wherein the groove type mixer comprises a mixer main body 1, a control screen 2, a feed inlet 3, a material pressing device (not shown), a granulating knife (not shown), a granulating mesh ring 5, a dispersion disc 6, a discharge port 7, a baffle 8, a copper pipe 9, a rotating cage 10 and a tray (not shown). The electrical control part is located blendor main part 1, the control panel sets up in one side of 1 top of blendor main part, charge door 3 is located the opposite side of 1 top of blendor main part, charge door 3 and the peripheral fixed connection of the pelletization net circle 5 that is located its below, and charge door 3 and the inside intercommunication of pelletization net circle 5, the pelletization sword sets up inside pelletization net circle 5, dispersion impeller 6 encircles and sets up in the outside of pelletization net circle 5, one side of dispersion impeller 6 is provided with discharge gate 7, baffle 8 of slope is installed to discharge gate 7, baffle 8 can be fixed on dispersion impeller 6, also can fix on the support frame that externally establishes in addition, baffle 8's upper portion has designed a copper pipe 9 that has a lot of holes, the lower extreme of copper pipe 9 can be fixed on baffle 8, rotatable rotor cage 10 is installed to discharge gate 7's below, the exit of rotor cage 10 sets up the tray.
The masterbatch of doing passes through, the charge door 3 gets into pelletization net circle 5, through the eccentric swage, presses the masterbatch to the pelletization edge of a knife, extrudes the granulation through the effort of pelletization sword between 5 with the pelletization net circle, and through the diameter size of the adjustable aerogel dispersible granule of the size of the particle diameter of the pelletization net circle 5 of adjustment difference, on the granulation back material can fall into rotatory dispersion impeller 6, through rotatory, conveys the material discharge gate 7. The inclined baffle plate 8 is arranged at the discharge port 7, the copper pipe 9 with a plurality of holes is designed at the upper part of the baffle plate 8, the copper pipe 9 is connected with compressed air, and the material at the discharge port 7 is blown under the action of air pressure, so that the material at the discharge port 7 can be effectively prevented from being accumulated (because the material contains water, the accumulation can be realized). A rotary cage 10 which can rotate is arranged below the discharge hole 7, so that the problem of overlong materials can be well avoided. The materials passing through the rotating cage 10 enter the tray from the discharge port 7 and are placed in an oven to be dried at the temperature of 100 ℃. The completely dried material is aerogel dispersible granules, wherein the content of aerogel powder is 98.5%.
Example 2:
1000g of water, 8g of polycarboxylate compound, 0.3g of sodium sulfate, 3g of hydroxyethyl cellulose and 700g of aerogel powder.
The preparation method of the aerogel particles provided in this example is as follows:
firstly, aerogel powder is made into a master batch, and the method comprises the following steps:
step one, slowly adding 8g of polycarboxylate compound into 1000g of deionized water, controlling the temperature of a stirrer at 30 ℃, rotating at 1000rpm/min, and uniformly mixing;
step two, adding 0.3g of sodium sulfate into the step one;
step three, slowly adding 3g of hydroxyethyl cellulose into the mixed step two, controlling the temperature of a stirrer at 20 ℃, rotating speed at 2500rpm/min, uniformly mixing, and sealing for later use;
and step four, controlling the temperature to be 30 ℃ all the time, taking 7000g of aerogel powder, rotating the stirrer at 3000rpm/min, adding the aerogel powder into the solution in the step two a little for multiple times, stopping the temperature rise in the middle, continuing to add the aerogel powder after cooling, stirring, and finally completely mixing 700g of aerogel powder with the components in the step three to form the master batch.
The aerogel used in the invention is silica gel, and as a plurality of hydrophobic groups are introduced into the molecules of the silica aerogel, the hydrophobicity of the silica aerogel is particularly strong, the powdery aerogel is difficult to be mixed with water by a common method to prepare aerogel dispersible particles, and the invention provides a method for fully mixing the hydrophobic silica aerogel with water and other additives.
Most of the currently marketed silica aerogel products are aerogel powders, and the hydrophobic silica aerogel powders are first prepared into high-content aerogel dispersible particles according to the present invention, and referring to fig. 1 to 5, the preparation method of the aerogel dispersible particles is as follows:
the masterbatch prepared by the fourth step is fed into a groove type mixer shown in fig. 1 through a feeder, wherein the groove type mixer comprises a mixer main body 1, a control screen 2, a feed inlet 3, a material pressing device (not shown), a granulating knife (not shown), a granulating mesh ring 5, a dispersion disc 6, a discharge port 7, a baffle 8, a copper pipe 9, a rotating cage 10 and a tray (not shown). The electrical control part is located blendor main part 1, the control panel sets up in one side of 1 top of blendor main part, charge door 3 is located the opposite side of 1 top of blendor main part, charge door 3 and the peripheral fixed connection of the pelletization net circle 5 that is located its below, and charge door 3 and the inside intercommunication of pelletization net circle 5, the pelletization sword sets up inside pelletization net circle 5, dispersion impeller 6 encircles and sets up in the outside of pelletization net circle 5, one side of dispersion impeller 6 is provided with discharge gate 7, baffle 8 of slope is installed to discharge gate 7, baffle 8 can be fixed on dispersion impeller 6, also can fix on the support frame that externally establishes in addition, baffle 8's upper portion has designed a copper pipe 9 that has a lot of holes, the lower extreme of copper pipe 9 can be fixed on baffle 8, rotatable rotor cage 10 is installed to discharge gate 7's below, the exit of rotor cage 10 sets up the tray.
The masterbatch of doing passes through, the charge door 3 gets into pelletization net circle 5, through the eccentric swage, presses the masterbatch to the pelletization edge of a knife, extrudes the granulation through the effort of pelletization sword between 5 with the pelletization net circle, and through the diameter size of the adjustable aerogel dispersible granule of the size of the particle diameter of the pelletization net circle 5 of adjustment difference, on the granulation back material can fall into rotatory dispersion impeller 6, through rotatory, conveys the material discharge gate 7. The inclined baffle plate 8 is arranged at the discharge port 7, the copper pipe 9 with a plurality of holes is designed at the upper part of the baffle plate 8, the copper pipe 9 is connected with compressed air, and the material at the discharge port 7 is blown under the action of air pressure, so that the material at the discharge port 7 can be effectively prevented from being accumulated (because the material contains water, the accumulation can be realized). A rotary cage 10 which can rotate is arranged below the discharge hole 7, so that the problem of overlong materials can be well avoided. The materials passing through the rotating cage 10 enter the tray from the discharge port 7 and are placed in an oven to be dried at the temperature of 120 ℃. The completely dried material is aerogel dispersible granules, wherein the content of aerogel powder is 98.4%.
Example 3:
1000g of water, 10g of EO/PO block polyether, 0.2g of sodium sulfate, 2g of polyvinylpyrrolidone and 700g of aerogel powder.
The preparation method of the aerogel particles provided in this example is as follows:
firstly, aerogel powder is made into a master batch, and the method comprises the following steps:
step one, slowly adding 10g of EO/PO block polyether into 1000g of deionized water, controlling the temperature of a stirrer at 25 ℃, rotating speed at 1000rpm/min, and uniformly mixing;
step two, adding 0.2g of sodium sulfate into the step one;
step three, slowly adding 2g of polyvinylpyrrolidone into the mixed step two, controlling the temperature of a stirrer at 25 ℃, rotating speed at 2500rpm/min, uniformly mixing, and sealing for later use;
and step four, controlling the temperature to be 25 ℃ all the time, taking 7000g of aerogel powder, rotating the stirrer at 3000rpm/min, adding the aerogel powder into the solution in the step two a little for multiple times, stopping the temperature rise in the middle, continuing to add the aerogel powder after cooling, stirring, and finally completely mixing 700g of aerogel powder with the components in the step three to form the master batch.
The aerogel used in the invention is silica gel, and as a plurality of hydrophobic groups are introduced into the molecules of the silica aerogel, the hydrophobicity of the silica aerogel is particularly strong, the powdery aerogel is difficult to be mixed with water by a common method to prepare aerogel dispersible particles, and the invention provides a method for fully mixing the hydrophobic silica aerogel with water and other additives.
Most of the silica aerogel products on the market at present are aerogel powder, the hydrophobic silica aerogel powder is prepared into high-content aerogel dispersible particles for the first time by the method disclosed by the invention, the preparation method of the aerogel dispersible particles is as in example 1, and the difference is that the hydrophobic silica aerogel powder is placed into an oven to be dried at the temperature of 150 ℃, and the completely dried material is the aerogel dispersible particles, wherein the content of aerogel powder is 98.3%.
Example 4:
1000g of water, 4g of fatty alcohol polyether, 0.2g of sodium sulfate, 6g of hydroxyethyl cellulose and 690g of aerogel powder.
The preparation method of the aerogel particles provided in this example is as follows:
firstly, aerogel powder is made into a master batch, and the method comprises the following steps:
step one, slowly adding 4g of fatty alcohol polyether into 1000g of deionized water, controlling the temperature of a stirrer at 25 ℃, rotating at 1000rpm/min, and uniformly mixing;
step two, adding 0.2g of sodium sulfate into the step one;
step three, slowly adding 6g of hydroxyethyl cellulose into the mixed step two, controlling the temperature of a stirrer at 25 ℃, rotating speed at 2500rpm/min, uniformly mixing, and sealing for later use;
and step four, controlling the temperature to be 25 ℃ all the time, taking 690g of aerogel powder, rotating the stirrer at 3000rpm/min, adding the aerogel powder into the solution in the step two for a small number of times, stopping the temperature rise in the middle, continuing to add the aerogel powder after the temperature is reduced, stirring, and finally completely mixing 690g of aerogel powder with the components in the step three to form the master batch.
The aerogel used in the invention is silica gel, and as a plurality of hydrophobic groups are introduced into the molecules of the silica aerogel, the hydrophobicity of the silica aerogel is particularly strong, the powdery aerogel is difficult to be mixed with water by a common method to prepare aerogel dispersible particles, and the invention provides a method for fully mixing the hydrophobic silica aerogel with water and other additives.
Most of the silica aerogel products in the market at present are aerogel powder, the hydrophobic silica aerogel powder is prepared into high-content aerogel dispersible particles for the first time, and the difference is that the hydrophobic silica aerogel powder is placed into an oven to be dried at the temperature of 150 ℃ as in example 1, the completely dried material is the aerogel dispersible particles, and the content of aerogel powder is 98.5%.
Example 5:
1000g of water, 4g of polycarboxylate compound, 0.3g of sodium chloride, 6g of polyvinyl alcohol and 690g of aerogel powder.
The preparation method of the aerogel particles provided in this example is as follows:
firstly, aerogel powder is made into a master batch, and the method comprises the following steps:
step one, slowly adding 4g of polycarboxylate compound into 1000g of deionized water, controlling the temperature of a stirrer at 25 ℃, rotating speed at 1000rpm/min, and uniformly mixing;
step two, adding 0.3g of sodium sulfate into the step one;
step three, slowly adding 6g of polyvinyl alcohol into the mixed step two, controlling the temperature of a stirrer at 25 ℃, rotating speed at 2500rpm/min, uniformly mixing, and sealing for later use;
and step four, controlling the temperature to be 25 ℃ all the time, taking 690g of aerogel powder, rotating the stirrer at 3000rpm/min, adding the aerogel powder into the solution in the step two for a small number of times, stopping the temperature rise in the middle, continuing to add the aerogel powder after the temperature is reduced, stirring, and finally completely mixing 690g of aerogel powder with the components in the step three to form the master batch.
The aerogel used in the invention is silica gel, and as a plurality of hydrophobic groups are introduced into the molecules of the silica aerogel, the hydrophobicity of the silica aerogel is particularly strong, the powdery aerogel is difficult to be mixed with water by a common method to prepare aerogel dispersible particles, and the invention provides a method for fully mixing the hydrophobic silica aerogel with water and other additives.
Most of the silica aerogel products on the market at present are aerogel powder, the hydrophobic silica aerogel powder is prepared into high-content aerogel dispersible particles for the first time, and the difference is that the hydrophobic silica aerogel powder is placed into an oven to be dried at the temperature of 140 ℃ as in example 1, the completely dried material is the aerogel dispersible particles, and the content of aerogel powder is 98.5%.
Application 1: heat insulation board
As shown in fig. 6, the aerogel particles produced by the present invention are applied to a commonly used insulation board (perlite) in the market, and the addition amount is 4% of the total weight, and the thermal conductivity is reduced by 10%.
The implementation method comprises the following steps: uniformly mixing 30g of aerogel particles with 0.5g of binder, 700g of perlite, 300g of water and the like, feeding the mixture into a pressing machine, demolding and drying to obtain the heat-insulating board containing the aerogel particles, wherein the heat conductivity coefficient is 0.052-0.047W/m.K.
Application 2: coating material
The aerogel particles produced by the method are put into water and stirred for 10 minutes to be completely dissolved, and a coating formula can be added to improve the functionality of the coating.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method of preparing aerogel dispersible particles, comprising:
firstly, aerogel powder is made into a master batch, and the method comprises the following steps:
step one, slowly adding a filler 1 into deionized water, wherein the filler 1 is one or a mixture of fatty alcohol polyether, polycarboxylate compound and EO/PO block polyether, and uniformly mixing in a stirrer;
step two, adding a filler 2 into the step one, wherein the filler 2 is one or a mixture of sodium chloride and sodium sulfate;
step three, slowly adding a filler 3 into the mixed step two, wherein the filler 3 is one or more of alkyl sulfate, a naphthalene sulfonic acid formaldehyde condensate, alkylaryl polyoxyethylene polyoxypropylene ether, an alkyl sulfonate anionic surfactant, polyvinyl alcohol, starch ether, xanthan gum, polyvinylpyrrolidone, a poly (alkenyl polyether) crosslinked acrylic acid polymer and cellulose polyether, uniformly mixing in a stirrer, and sealing for later use;
step four, taking aerogel powder, adding the aerogel powder into the solution obtained in the step two for a small number of times, stirring, stopping when the intermediate temperature rises, continuing to add the aerogel after cooling, stirring, and finally completely mixing all the aerogel powder with the components obtained in the step three to obtain a master batch;
the process for the aerogel dispersible granules is as follows:
and (3) feeding the prepared master batch into a mixer through a feeder to mix, and then putting the mixture into an oven to be dried at the temperature of 100-150 ℃ to obtain the aerogel dispersible particles.
2. The method of preparing aerogel dispersible particles of claim 1, wherein: the cellulose polyether in the third step is any one of hydroxyethyl cellulose, hydroxymethyl cellulose, carboxymethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose and lignocellulose.
3. The method of preparing aerogel dispersible particles of claim 1, wherein: in the first step, the temperature of the stirrer is controlled to be 20-30 ℃, the rotating speed is 1000rpm/min, in the third step, the temperature of the stirrer is controlled to be 20-30 ℃, the rotating speed is 2500rpm/min, and in the fourth step, the temperature of the stirrer is always controlled to be 20-30 ℃, and the rotating speed is 3000 rpm/min.
4. The method of preparing aerogel dispersible particles of claim 1, wherein: the mass ratio of the raw materials used for preparation is as follows:
silicon aerogel: 5 to 98 percent of the total weight of the steel,
packing 1: 0.2 to 10 percent of the total weight of the composition,
and (3) filler 2: 0.02 to 1 percent of the total weight of the alloy,
and (3) filler: 0.2 to 10 percent of the total weight of the composition,
water is added to make up to 100%.
5. The method of preparing aerogel dispersible particles of claim 1, wherein: cell type blendor includes the blendor main part, the control panel, the charge door, the eccentric swage, the pelletization sword, the pelletization net circle, the dispersion impeller, the discharge gate, the baffle, the copper pipe, the electrical control part is located the blendor main part, the control panel sets up in one side of blendor main part top, the charge door is located the opposite side of blendor main part top, the peripheral fixed connection of pelletization net circle of charge door and below being located, and charge door and the inside intercommunication of pelletization net circle, the pelletization sword sets up inside the pelletization net circle, the dispersion impeller encircles and sets up the outside at the pelletization net circle, one side of dispersion impeller is provided with the discharge gate, the baffle of slope is installed to the discharge gate, a copper pipe that has a lot of holes has been designed on the upper portion of baffle.
6. The method of preparing aerogel dispersible particles of claim 5, wherein: the mixing process in the groove type mixer is as follows:
the diameter size of the dispersible granule of size regulation aerogel through the different pelletization net ring particle diameters of adjustment is through the eccentric swage, presses the masterbatch to the pelletization edge of a knife, extrudees the granulation through the effort between pelletization sword and the pelletization net, and on the material fell into rotatory dispersion impeller after the granulation, through rotatory, conveyed the material to the discharge gate.
7. The method of preparing aerogel dispersible particles of claim 6, wherein: a rotatable rotating cage is arranged below the discharge port, and materials passing through the rotating cage enter the tray from the discharge port.
8. An aerogel dispersible particle made by the method of making the aerogel dispersible particle of any of claims 1-7.
9. Use of the aerogel dispersible particles made by the method of making the aerogel dispersible particles of any of claims 1-7 in an insulation board.
10. Use of the aerogel dispersible particles prepared by the method of making the aerogel dispersible particles of any of claims 1-7 in a coating.
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| CN203469944U (en) * | 2013-08-28 | 2014-03-12 | 云南锦润生物科技有限公司 | Rotary granulator |
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| CN203469944U (en) * | 2013-08-28 | 2014-03-12 | 云南锦润生物科技有限公司 | Rotary granulator |
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