CN109988480A - A kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid - Google Patents
A kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid Download PDFInfo
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- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/10—Homopolymers or copolymers of methacrylic acid esters
- C09D133/12—Homopolymers or copolymers of methyl methacrylate
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/69—Particle size larger than 1000 nm
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of preparation methods of nano-silicon anti-flaming thermal-insulation liquid, it include the preparation of compound resin liquid and the preparation of anti-flaming thermal-insulation liquid including nano-silicon anti-flaming thermal-insulation liquid and preparation method thereof, the preparation method of the nano-silicon anti-flaming thermal-insulation liquid including the following steps: step 1: the preparation flow of compound resin liquid, step 2: the preparation flow of anti-flaming thermal-insulation liquid, defoaming agent includes fatty acid amide, base oil, oily thickener and surfactant, and oily thickener is metallic soap, hydroxycarboxylic acid, amino acid gelating agent, one of polyglyceryl fatty acid ester and modified polyolefin waxes are a variety of, and fatty acid amide, base oil, the ratio of oily thickener and surfactant is 1~10:71~97:0.4~10:1~9.The preparation method of the nano-silicon anti-flaming thermal-insulation liquid, the resistance to flame retardant property of liquid is preferable, and lower production costs, is suitable for large batch of production, and the time-consuming produced is shorter, and production efficiency is higher, operates relatively simple.
Description
Technical field
The present invention relates to nano-silicon anti-flaming thermal-insulation liquid correlative technology field, specially a kind of system of nano-silicon anti-flaming thermal-insulation liquid
Preparation Method.
Background technique
Nano-silicon anti-flaming thermal-insulation liquid is a kind of material for building trade, be mainly used for current building exterior wall and
Roof, and this material is wide to the absorption region of light, amount of stored heat is big, and heat dissipation is slow, leads to quick heating inside building, and high temperature is lasting
Time is long, therefore needs insulating moulding coating in construction to solve the above problems, but current thermal insulating fluid existing in the market
And preparation method thereof there are still certain defects, such as:
1. it is in air due to external wall exposure, and very high to the requirement of the flame retardant property of thermal insulating fluid, and be in application publication number
The Chinese invention of CN102888135A: a kind of nano heat-insulating liquid coating, wherein the oxide of nanometer cobalt is that absorption mechanism is heat-insulated
Material, meanwhile, to make product that there is more excellent heat insulation, chooses the reflection type thermal insulations additives such as titanium dioxide and answered
It closes and uses, and moderately introduce high heating rate inorganic substances copper oxide etc., so that the heat-insulated formation of coating reflected, absorbed, radiate and combine
Heat insulation, but the resistance to flame retardant property of nano heat-insulating liquid coating is bad；
2. demand is larger since the nano-silicon anti-flaming thermal-insulation liquid is mainly used for the smearing of building wall, and it is general every
The higher cost of hydrothermal solution coating production, is not suitable for large batch of production, can not be widely used in the smearing of building wall；
3. the component content due to thermal insulating fluid is complex, and general thermal insulating fluid coating is in the preparation, generally requires to expend big
The time of amount, and production process and complicated operation, therefore cannot rapidly and efficiently carry out producing.
Therefore, it is proposed that a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid, is proposed with to solve above-mentioned background technique
Currently on the market the problem of the preparation method of thermal insulating fluid.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of nano-silicon anti-flaming thermal-insulation liquid, to solve above-mentioned background technique
The resistance to flame retardant property of most of thermal insulating fluids of middle proposition is bad, cannot play good resistance to flame retardant effect, and production cost is higher, no
Suitable for large batch of production, and the problem of what is produced takes a long time, and complicated operation.
To achieve the above object, the invention provides the following technical scheme: a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid,
It include the preparation of compound resin liquid and the preparation of anti-flaming thermal-insulation liquid including nano-silicon anti-flaming thermal-insulation liquid and preparation method thereof.
Preferably, the preparation method of the nano-silicon anti-flaming thermal-insulation liquid including the following steps:
Step 1: the preparation flow of compound resin liquid:
(1) silicic acid, methyl methacrylate and tetrabutyl titanate are added sequentially in reaction vessel, are stirred evenly；
(2) nano-titanium dioxide is added in container in (1) and stirs evenly, adds waterborne organic silicon resin, and successively
Isopropanol, polyethylene glycol and polystyrene is added, seals reaction vessel after uniform stirring, and to pressurizeing in reaction vessel, make
It is sufficiently reacted；
(3) reactant of (2) is cooled to room temperature, compound resin liquid can be obtained；
Step 2: the preparation flow of anti-flaming thermal-insulation liquid:
(1) inorganic composite nano material, magnesium hydroxide (or aluminium hydroxide) and organic clay reaction is sequentially added into hold
In device, and inorganic composite nano material, magnesium hydroxide (or aluminium hydroxide) and organic clay are fully ground, so that mixing
Uniformly；
(2) by inorganic composite nano material made from (1), magnesium hydroxide (or aluminium hydroxide) and organic clay mixture and addition
Into deionized water, and uniform stirring, so that aqueous slurry be made；
(3) by the acrylic resin film forming agent of certain weight proportion be added to (2) in aqueous slurry in, uniform stirring；
(4) compound resin liquid, pigment, defoaming agent, silica and stabilizer made from step 1 are added according to a certain percentage
Inside blender, and the mixing speed of blender is adjusted to 60 revs/min, it is fire-retardant that nano-silicon quickly can be obtained after mixing evenly
Thermal insulating fluid.
Preferably, nano-titanium dioxide, waterborne organic silicon resin, isopropanol, polyethylene glycol and polyphenyl in the step 1
Ethylene is 4-6 hours a length of when answering the reaction in container.
Preferably, the ingredient of the stabilizer be casein, carboxylate, sulfuric acid, sulfonate, gelatin, ethylene oxide with
The condensation product of fatty alcohol.
Preferably, the mass ratio of the compound resin liquid, pigment, defoaming agent and silica is 40:2:1:2, and dioxy
It is 5-15 μm that SiClx partial size, which takes range,.
Preferably, the defoaming agent includes fatty acid amide, base oil, oily thickener and surfactant, and oily thickener
For one of metallic soap, hydroxycarboxylic acid, amino acid gelating agent, polyglyceryl fatty acid ester and modified polyolefin waxes or a variety of,
And fatty acid amide, base oil, oily thickener and surfactant ratio be 1~10:71~97:0.4~10:1~9.
Preferably, the mass ratio of the magnesium hydroxide (or aluminium hydroxide) and organic clay is 80~99.5:0.5~20,
And magnesium hydroxide (or aluminium hydroxide) is the pulvis that diameter is less than 1mm.
Preferably, the organic clay is graininess, and the average grain diameter of organic clay is between 0.2-0.25 μm.
Preferably, the temperature of the sealing pressing reaction in the step 1 (2) is 70 °C, and pressure is in reaction vessel
5.5MPa。
Compared with prior art, the beneficial effects of the present invention are: the preparation method of the nano-silicon anti-flaming thermal-insulation liquid, the resistance to resistance of liquid
Better performances are fired, good resistance to flame retardant effect, and lower production costs can be played, be suitable for large batch of production, and produce
Time-consuming it is shorter, production efficiency is higher, operate it is relatively simple；
1, pass through inorganic composite nano material, magnesium hydroxide (or aluminium hydroxide) and organic clay and acrylic resin film forming agent etc.
Material composition and corresponding process operation can play so that the nano-silicon anti-flaming thermal-insulation liquid has good resistance to anti-flammability
Good resistance to flame retardant effect；
2, in entire preparation flow, other than the common devices such as blender and reaction vessel, expensive equipment investment is not needed, and
The cost of used material is all relatively low, so that the whole lower production costs of the nano-silicon anti-flaming thermal-insulation liquid therefore should
Nano-silicon anti-flaming thermal-insulation liquid can carry out large batch of production, and be suitble to the smearing of the large area such as external wall, building roof；
3, entire manufacture craft is very simple, does not need complicated reaction and operation, and the reaction duration of associated materials is also opposite
It is shorter, therefore the preparation efficiency of the nano-silicon anti-flaming thermal-insulation liquid is higher, quickly can be produced and be come into operation.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments, based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of technical solution: a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid, nano-silicon anti-flaming thermal-insulation
Liquid and preparation method thereof includes the preparation of compound resin liquid and the preparation of anti-flaming thermal-insulation liquid.
The preparation method of nano-silicon anti-flaming thermal-insulation liquid including the following steps:
Step 1: the preparation flow of compound resin liquid:
(1) silicic acid, methyl methacrylate and tetrabutyl titanate are added sequentially in reaction vessel, are stirred evenly；
(2) nano-titanium dioxide is added in container in (1) and stirs evenly, adds waterborne organic silicon resin, and successively
Isopropanol, polyethylene glycol and polystyrene is added, seals reaction vessel after uniform stirring, and to pressurizeing in reaction vessel, make
It is sufficiently reacted；
(3) reactant of (2) is cooled to room temperature, compound resin liquid can be obtained；
Step 2: the preparation flow of anti-flaming thermal-insulation liquid:
(1) inorganic composite nano material, magnesium hydroxide (or aluminium hydroxide) and organic clay reaction is sequentially added into hold
In device, and inorganic composite nano material, magnesium hydroxide (or aluminium hydroxide) and organic clay are fully ground, so that mixing
Uniformly；
(2) by inorganic composite nano material made from (1), magnesium hydroxide (or aluminium hydroxide) and organic clay mixture and addition
Into deionized water, and uniform stirring, so that aqueous slurry be made；
(3) by the acrylic resin film forming agent of certain weight proportion be added to (2) in aqueous slurry in, uniform stirring；
(4) compound resin liquid, pigment, defoaming agent, silica and stabilizer made from step 1 are added according to a certain percentage
Inside blender, and the mixing speed of blender is adjusted to 60 revs/min, it is fire-retardant that nano-silicon quickly can be obtained after mixing evenly
Thermal insulating fluid.
Nano-titanium dioxide, waterborne organic silicon resin, isopropanol, polyethylene glycol and polystyrene are answering container in step 1
In reaction when it is 4-6 hours a length of, the reaction duration is relatively short, improves the whole effect of nano-silicon anti-flaming thermal-insulation liquid preparation
Rate.
The ingredient of stabilizer is the condensation of casein, carboxylate, sulfuric acid, sulfonate, gelatin, ethylene oxide and fatty alcohol
Object.
Compound resin liquid, pigment, defoaming agent and silica mass ratio be 40:2:1:2, and silica partial size is taken
Range is 5-15 μm, by using the silica compared with small particle, so that the function and effect of silica in the production process are more
Height is more convenient production.
Defoaming agent includes fatty acid amide, base oil, oily thickener and surfactant, and oily thickener is metallic soap, hydroxyl
One of yl carboxylic acid, amino acid gelating agent, polyglyceryl fatty acid ester and modified polyolefin waxes are a variety of, and fatty acid acyl
Amine, base oil, oily thickener and surfactant ratio be 1~10:71~97:0.4~10:1~9, rationally control fatty acid
The ratio of amide, base oil, oily thickener and surfactant, so that the using effect of the defoaming agent is more preferable.
The mass ratio of magnesium hydroxide (or aluminium hydroxide) and organic clay is 80~99.5:0.5~20, and magnesium hydroxide
(or aluminium hydroxide) is the pulvis that diameter is less than 1mm, and the magnesium hydroxide (or aluminium hydroxide) of 1mm is less than by using diameter, is made
It is higher to obtain the reaction efficiency of magnesium hydroxide (or aluminium hydroxide) in the making step, to save more reaction time, mentions
The efficiency that height is integrally prepared.
Organic clay is graininess, and the average grain diameter of organic clay, between 0.2-0.25 μm, which has
Machine clay, it is easier to stirring and mixing with magnesium hydroxide (or aluminium hydroxide).
The temperature of sealing pressing reaction in step 1 (2) is 70 °C, and pressure is 5.5MPa, the temperature in reaction vessel
So that the reaction efficiency of (2) is higher in step 1, and effect is more preferable.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
Any actual relationship or order perhaps sequence moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art,
It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc.
With replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this
Within the protection scope of invention.
Claims (9)
1. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid, it is characterised in that: the nano-silicon anti-flaming thermal-insulation liquid and preparation method thereof
The preparation of preparation comprising compound resin liquid and anti-flaming thermal-insulation liquid.
2. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 1, it is characterised in that: the nano-silicon
The preparation method of anti-flaming thermal-insulation liquid including the following steps:
Step 1: the preparation flow of compound resin liquid:
(1) silicic acid, methyl methacrylate and tetrabutyl titanate are added sequentially in reaction vessel, are stirred evenly；
(2) nano-titanium dioxide is added in container in (1) and stirs evenly, adds waterborne organic silicon resin, and successively
Isopropanol, polyethylene glycol and polystyrene is added, seals reaction vessel after uniform stirring, and to pressurizeing in reaction vessel, make
It is sufficiently reacted；
(3) reactant of (2) is cooled to room temperature, compound resin liquid can be obtained；
Step 2: the preparation flow of anti-flaming thermal-insulation liquid:
(1) inorganic composite nano material, magnesium hydroxide (or aluminium hydroxide) and organic clay reaction is sequentially added into hold
In device, and inorganic composite nano material, magnesium hydroxide (or aluminium hydroxide) and organic clay are fully ground, so that mixing
Uniformly；
(2) by inorganic composite nano material made from (1), magnesium hydroxide (or aluminium hydroxide) and organic clay mixture and addition
Into deionized water, and uniform stirring, so that aqueous slurry be made；
(3) by the acrylic resin film forming agent of certain weight proportion be added to (2) in aqueous slurry in, uniform stirring；
(4) compound resin liquid, pigment, defoaming agent, silica and stabilizer made from step 1 are added according to a certain percentage
Inside blender, and the mixing speed of blender is adjusted to 60 revs/min, it is fire-retardant that nano-silicon quickly can be obtained after mixing evenly
Thermal insulating fluid.
3. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 2, it is characterised in that: the step 1
Middle nano-titanium dioxide, waterborne organic silicon resin, isopropanol, polyethylene glycol and polystyrene are a length of when answering the reaction in container
4-6 hours.
4. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 2, it is characterised in that: the stabilizer
Ingredient be casein, carboxylate, sulfuric acid, sulfonate, gelatin, ethylene oxide and fatty alcohol condensation product.
5. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 2, it is characterised in that: the compound tree
Rouge liquid, pigment, defoaming agent and silica mass ratio be 40:2:1:2, and it is 5-15 μm that silica partial size, which takes range,.
6. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 2, it is characterised in that: the defoaming agent
Including fatty acid amide, base oil, oily thickener and surfactant, and oily thickener is metallic soap, hydroxycarboxylic acid, amino acid cure
One of gelatinizing agent, polyglyceryl fatty acid ester and modified polyolefin waxes are a variety of, and fatty acid amide, base oil, oil thickening
The ratio of agent and surfactant is 1~10:71~97:0.4~10:1~9.
7. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 2, it is characterised in that: the hydroxide
The mass ratio of magnesium (or aluminium hydroxide) and organic clay is 80~99.5:0.5~20, and magnesium hydroxide (or aluminium hydroxide) is straight
Diameter is less than the pulvis of 1mm.
8. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 2, it is characterised in that: described organic glutinous
Soil is graininess, and the average grain diameter of organic clay is between 0.2-0.25 μm.
9. a kind of preparation method of nano-silicon anti-flaming thermal-insulation liquid according to claim 2, it is characterised in that: the step 1
(2) temperature of the sealing pressing reaction in is 70 °C, and pressure is 5.5MPa in reaction vessel.
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