CN111925747B - Reinforced flame-retardant powder for sealant and preparation method and application thereof - Google Patents

Reinforced flame-retardant powder for sealant and preparation method and application thereof Download PDF

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CN111925747B
CN111925747B CN202010841970.XA CN202010841970A CN111925747B CN 111925747 B CN111925747 B CN 111925747B CN 202010841970 A CN202010841970 A CN 202010841970A CN 111925747 B CN111925747 B CN 111925747B
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brucite
sealant
modifier
modification
retardant powder
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CN111925747A (en
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周峰
吴平飞
李海滨
彭鹤松
邓鹏�
吴维冰
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Jiangxi Guangyuan Chemical Co Ltd
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Jiangxi Guangyuan Chemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • 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
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • 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
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • 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

Abstract

The invention provides a reinforced flame-retardant powder for a sealant, and a preparation method and application thereof, and belongs to the technical field of sealant additives. The crystal form inducer is connected to the ground brucite by using the first modifier, so that the crystal form inducer is uniformly coated on the surface of the ground brucite; meanwhile, the crystal form inducer can induce calcium carbonate generated in the deposition coating process to be loaded on the modified brucite in a certain shape, namely, the shape of the brucite is modified, so that the brucite has the shapes of spheres, cubes and the like, and better fluidity or thixotropy is endowed. And when the deposition and coating are finished, the second modifier is added for modification, and the second modifier is uniformly and firmly coated on the brucite by utilizing a large amount of hydroxyl groups on the surface of the newly formed calcium carbonate, so that the final powder has excellent organic compatibility and can be better combined with resin.

Description

Reinforced flame-retardant powder for sealant and preparation method and application thereof
Technical Field
The invention relates to the technical field of sealant additives, in particular to a reinforced flame-retardant powder for a sealant, and a preparation method and application thereof.
Background
With the development of society, the living standard of people is continuously improved, and people also put higher demands on other functions besides the aesthetic property and the comfort of buildings and decorations. Various decorative materials bring convenience to life of people, and meanwhile, various fire-fighting hidden dangers also exist.
The traditional sealant is prepared from resin, an auxiliary agent, calcium carbonate, quartz powder, diatomite and other fillers; the filler is added in a large amount, so that the sealant not only plays a role in basic body filling, but also plays a role in reinforcing various performances of the sealant. If the sealant needs a certain fire-proof flame-retardant grade, some flame retardant is added. The flame retardant is mainly divided into two types of physical mixed addition type and reaction flame retardant type, and mainly comprises magnesium hydroxide, tributyl phosphate, trichlorobromomethane and the like, wherein the inorganic flame retardant such as magnesium hydroxide, aluminum hydroxide and the like has relatively low price, but the inorganic flame retardant has relatively high price compared with the conventional filler, has poor compatibility with organic resin and strong hygroscopicity, and is not beneficial to post processing.
Therefore, it is urgent to provide a reinforced flame retardant powder with good flame retardant effect, low cost and better compatibility with organic resin.
Disclosure of Invention
In view of the above, the present invention provides a reinforced flame retardant powder for a sealant, and a preparation method and an application thereof. The preparation method provided by the invention is simple and low in cost, and the obtained reinforced flame-retardant powder for the sealant has a good flame-retardant effect and good compatibility with organic resin.
The invention provides a preparation method of reinforced flame-retardant powder for a sealant, which comprises the following steps:
grinding brucite to obtain ground brucite;
mixing the ground brucite, a first modifier and a crystal form inducer, and then carrying out first modification to obtain modified brucite; the first modifier is one or more of 3-aminopropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane and ethylenediamine tetraacetic acid;
mixing the modified brucite and the lime cream, and carrying out deposition coating to obtain a coating material liquid;
adding a second modifier into the coating material liquid for second modification to obtain the reinforced flame-retardant powder for the sealant; the second modifier is one or more of aluminate, sodium stearate, hydrogenated rosin and sodium dodecyl benzene sulfonate.
Preferably, the addition amount of the first modifier is 8-12 per mill of the mass of the ground brucite.
Preferably, the crystal form inducer is MgSO4、AlCl3Glucose and ethylenediamine tetra (ethylene diamine tetra)One or more of acetic acid; the addition amount of the crystal form inducer is 0.015-0.02% of the mass of the ground brucite.
Preferably, the temperature of the first modification is 80-120 ℃, and the time is 15-30 min.
Preferably, the solid content of the lime milk is 81-85%; the addition amount of the lime milk is 180-220% of the mass of the modified brucite in terms of calcium hydroxide.
Preferably, the deposit coating is bubbling CO2The deposition and coating are carried out under the condition, and the temperature of the deposition and coating is 30-45 ℃.
Preferably, the addition amount of the second modifier is 6-12% of the mass of the modified brucite.
Preferably, the second modification is CO sparging2The temperature of the second modification is 60-85 ℃, and the time is 40-50 min.
The invention also provides the reinforced flame-retardant powder for the sealant, which is obtained by the preparation method in the technical scheme, wherein the granularity of the reinforced flame-retardant powder for the sealant is 2000-3000 meshes.
The invention also provides the application of the reinforced flame-retardant powder for the sealant in the technical scheme as a reinforced flame retardant in the field of sealants.
The invention provides a preparation method of reinforced flame-retardant powder for a sealant, which comprises the following steps: grinding brucite to obtain ground brucite; mixing the ground brucite, a first modifier and a crystal form inducer, and then carrying out first modification to obtain modified brucite; the first modifier is one or more of 3-aminopropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane and ethylenediamine tetraacetic acid; mixing the modified brucite and the lime cream, and carrying out deposition coating to obtain a coating material liquid; adding a second modifier into the coating material liquid for second modification to obtain the reinforced flame-retardant powder for the sealant; the second modifier is one or more of aluminate, sodium stearate, hydrogenated rosin and sodium dodecyl benzene sulfonate.
The brucite is used as a core carrier, the brucite generates water vapor through thermal decomposition, the water vapor can take away heat, and the generated magnesium oxide can adhere to the surface of a combustion layer to isolate oxygen to prevent combustion, so that the powder has flame retardance. Connecting a crystal form inducer to the ground brucite by using a first modifier so that the crystal form inducer is uniformly coated on the surface of the ground brucite; meanwhile, the crystal form inducer can induce calcium carbonate generated in the deposition coating process to be loaded on the modified brucite in a certain shape, namely, the shape of the brucite is modified, so that the final powder has the shapes of spheres, cubes and the like, and better fluidity or thixotropy is endowed to the powder. When the deposition coating is finished, a second modifier is added for modification, and the second modifier is uniformly and firmly coated on brucite by utilizing a large amount of hydroxyl groups existing on the surface of the newly formed calcium carbonate, so that the final powder has excellent organic compatibility and can be better combined with resin; in addition, the surface of the powder is hydrophobic due to the coating of the second modifier, so that the powder is prevented from absorbing moisture and being wetted.
Drawings
FIG. 1 is a flow chart of a method for preparing a reinforced flame-retardant powder for a sealant according to the present invention;
FIG. 2 is a scanning electron micrograph of the reinforced flame retardant powder for sealant obtained in example 1.
Detailed Description
The invention provides a preparation method of reinforced flame-retardant powder for a sealant, which comprises the following steps:
grinding brucite to obtain ground brucite;
mixing the ground brucite, a first modifier and a crystal form inducer, and then carrying out first modification to obtain modified brucite; the first modifier is one or more of 3-aminopropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane and ethylenediamine tetraacetic acid;
mixing the modified brucite and the lime cream, and carrying out deposition coating to obtain a coating material liquid;
immediately adding a second modifier into the coating material liquid for second modification to obtain the reinforced flame-retardant powder for the sealant; the second modifier is one or more of aluminate, sodium stearate, hydrogenated rosin and sodium dodecyl benzene sulfonate.
Grinding brucite to obtain ground brucite;
in the invention, the mass content of the magnesium hydroxide in the brucite is preferably more than or equal to 88%. In the present invention, the brucite is preferably brucite having a magnesium hydroxide content of 88% or more, available from Liaoning.
In the invention, the brucite is preferably cleaned and crushed before grinding, the cleaning reagent is preferably water, and the cleaning frequency is preferably 1-2 times. In the invention, the cleaning can clean and remove silt impurities on the surface of brucite.
In the present invention, the particle size of the crushed brucite is preferably 1 to 2cm, and the parameters of the crushing are not particularly limited as long as the particle size of the crushed brucite is 1 to 2 cm.
In the invention, the grinding method is preferably an air flow mill, and the granularity of the ground brucite is preferably 6000-8000 meshes; the parameters of the jet mill are not particularly limited, as long as the particle size of the finely ground brucite is 6000-8000 meshes.
In the invention, the granularity of the ground brucite is adjusted to 6000-8000 meshes, and the specific surface area is relatively large, thereby being beneficial to improving the glue peeling strength, the tensile strength and the thixotropy of the reinforced flame-retardant powder for the final sealant.
After obtaining the ground brucite, the invention mixes the ground brucite, the first modifier and the crystal form inducer, and then carries out the first modification, thus obtaining the modified brucite.
In the invention, the first modifier is one or more of 3-aminopropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane and Ethylene Diamine Tetraacetic Acid (EDTA), preferably 3-aminopropyltrimethoxysilane or 3-methacryloxypropyltrimethoxysilane; the addition amount of the first modifier is preferably 8-12 per mill of the mass of the ground brucite, and more preferably 10 per mill. In the invention, the first modification can fix the crystal form inducer on the surface of the powder particles, and plays a basic role in subsequent chemical deposition.
In the present invention, the crystal form inducer is preferably MgSO4、AlCl3Glucose and ethylenediaminetetraacetic acid (EDTA), further preferably MgSO4And ethylenediamine tetraacetic acid mixture, AlCl3And glucose mixtures or glucose; when the crystal form inducer is preferably MgSO4And ethylenediaminetetraacetic acid mixture, the MgSO4The mass ratio of ethylene diamine tetraacetic acid to ethylene diamine tetraacetic acid is preferably 1: 1; when the crystal form inducer is preferably AlCl3And glucose mixtures, the AlCl3The mass ratio of glucose to glucose is preferably 1: 1. In the invention, the addition amount of the crystal form inducer is preferably 0.015-0.02% of the mass of the ground brucite. In the present invention, when the crystal form inducer is EDTA and MgSO4When the brucite is in a cubic shape; when the crystal form inducer is glucose, the brucite is spherical in shape; when the crystal form inducer is glucose and AlCl3The brucite is spindle-shaped.
In the present invention, the mixing sequence is preferably that the first modifier and the crystal form inducer are first mixed and then are second mixed with the finely ground brucite, and when the first modifier and the crystal form inducer are first mixed, a small amount of water is preferably added to first mix the first modifier and the crystal form inducer. In the invention, the mixing time is preferably 2-3 min.
In the invention, the temperature of the first modification is preferably 80-120 ℃, and more preferably 90-100 ℃; the time is preferably 15-30 min.
In the invention, the mixing and the first modification of the ground brucite, the first modifier and the crystal form inducer are carried out under the condition of stirring, and the rotation speed of the stirring is preferably 1500-2500 r/min.
In the present invention, the mixing of the ground brucite, the first modifier and the crystal form inducer and the first modification are preferably carried out in a high-speed mixer.
After the first modification is completed, the invention preferably further comprises the step of sieving the obtained first modified material by a 300-mesh sieve to obtain the modified brucite. The invention can remove large particles formed by agglomeration by sieving the first modified material with a 300-mesh sieve, and prevent pocking marks and particles of the final product in downstream application.
In the invention, the first modification can connect the crystal form inducer to the finely ground brucite through the first modifier, and meanwhile, the use of the first modifier enables the crystal form inducer to be well coated on the modified brucite to prepare for the subsequent crystal form control of calcium carbonate.
After the modified brucite is obtained, the modified brucite and lime milk are mixed and deposited and coated to obtain a coating material liquid.
In the invention, the solid content of the lime milk is preferably 81-85%, and is further preferably 82%; the addition amount of the lime milk is preferably 180-220% of the mass of the modified brucite, and more preferably 200% of the mass of the calcium hydroxide in the lime milk. In the present invention, the lime milk is preferably prepared by the following steps:
cleaning and crushing calcite, and calcining to obtain quick lime;
mixing the quicklime with water, and digesting to obtain coarse lime milk;
and refining the coarse lime milk to obtain the lime milk.
According to the invention, calcite is cleaned, crushed and calcined to obtain quicklime;
in the invention, the mass content of calcium carbonate in the calcite is preferably more than or equal to 97%.
The parameters of the cleaning are not particularly limited, and the cleaning agent can be used for cleaning and removing impurities such as silt on the calcite.
In the invention, the particle size of the calcite obtained after crushing is preferably 1-2 cm; the parameters for the crushing are not particularly limited, as long as the particle size of the calcite obtained after the crushing is 1 to 2 cm.
In the invention, the calcining temperature is preferably 1000-1200 ℃, and more preferably 1100 ℃; the time is preferably 5-8 h.
In the present invention, the calcination is capable of decomposing calcium carbonate into calcium oxide and carbon dioxide.
In the present invention, the carbon dioxide generated by the calcination is preferably purified and then compressed for collection, and the parameters of the purification and compression collection of the carbon dioxide are not particularly limited in the present invention.
After the quicklime is obtained, the quicklime is mixed with water and digested to obtain coarse lime milk.
In the invention, the mass ratio of the quicklime to the water is preferably 1: 4.5-1: 5.5, and more preferably 1:5. In the present invention, the digestion is preferably carried out under stirring conditions, preferably at a speed of 60 r/min; the time for the digestion is not particularly limited in the present invention, as long as quicklime and water are reacted completely, and the reaction degree of quicklime and water is preferably roughly judged by measuring the temperature of the emulsion. In the present invention, the digestion is preferably carried out in a digester.
After the coarse lime milk is obtained, the coarse lime milk is refined to obtain the lime milk.
In the present invention, the refining is preferably carried out in a multistage hydrocyclone; the rotating speed of the multistage cyclone separator is not particularly limited, and the multistage cyclone separator can effectively separate impurities such as particles in a coarse lime-milk system from the emulsion.
After the refining is finished, the invention preferably comprises the step of naturally cooling the refined feed liquid after standing to obtain the lime milk.
In the present invention, the deposit coating is preferably carried out by bubbling CO2Under the conditions of (a); the CO is2The mol ratio of the calcium hydroxide to the calcium hydroxide in the lime milk is preferably (0.9-1.1): 1; the invention is directed to said CO2The blowing speed of (2) is not particularly limited as long as a predetermined amount of CO is supplied2And (5) finishing the blowing. In the present invention, the CO is2Preferably from carbon dioxide generated during calcination of calcite in the preparation of milk of lime. In the present invention, theThe temperature of deposition coating is preferably 15-80 ℃, the time of deposition coating is not particularly limited in the invention, as long as CO is used2All the materials are blown in. In the invention, the deposition coating is preferably carried out under the condition of stirring, and the rotation speed of the stirring is preferably 50-400 r/min, and more preferably 280-320 r/min. In the present invention, the process of depositing the coating is preferably: mixing the modified brucite and the lime cream, controlling the temperature to be 15-30 ℃, starting stirring, and then blowing CO2And maintaining the temperature at 30-80 ℃ for deposition coating. In the present invention, the deposition coating is preferably performed in a reaction vessel.
In the invention, the deposition coating can ensure that the calcium carbonate is coated on the modified brucite in a certain shape, so that the final powder has a specific shape and further has better fluidity or thixotropy; meanwhile, the deposition coating of the calcium carbonate can ensure that the specific surface area of the modified brucite is large and the surface activity is higher, thereby being beneficial to the second modification.
After the coating material liquid is obtained, a second modifier is added into the coating material liquid for second modification, so that the reinforced flame-retardant powder for the sealant is obtained.
In the present invention, CO is required to be bubbled in during deposition coating2After the addition is completed, the second modifier is preferably added immediately for the second modification.
In the present invention, the second modifier is one or more of aluminate, sodium stearate, hydrogenated rosin and sodium dodecylbenzene sulfonate, preferably a mixture of aluminate, sodium stearate and hydrogenated rosin, and a mixture of sodium stearate and sodium dodecylbenzene sulfonate; when the second modifier is preferably a mixture of sodium stearate and hydrogenated rosin, the mass ratio of sodium stearate to hydrogenated rosin is preferably 3: 1; when the second modifier is preferably a mixture of sodium stearate and sodium dodecylbenzene sulfonate, the mass ratio of sodium stearate to sodium dodecylbenzene sulfonate is preferably 5: 1. In the present invention, the amount of the second modifier added is preferably 6 to 12% by mass, and more preferably 9 to 10% by mass, of the modified brucite. In the invention, the temperature of the second modification is preferably 60-85 ℃, more preferably 65-80 ℃, and more preferably 70-75 ℃; the time is preferably 40-50 min. In the invention, the second modification is preferably carried out under the condition of stirring, and the rotation speed of the stirring is preferably 120-240 r/min. In the present invention, the second modification is preferably carried out in a reaction vessel.
After the second modification is finished, the invention preferably comprises the step of sieving the obtained second modified material through a 300-mesh sieve after spray drying to obtain the reinforced flame-retardant powder for the sealant.
In the present invention, the parameters of the spray drying are not particularly limited as long as the second modified product can be atomized and sprayed to be dried by hot air.
In the invention, after the carbon dioxide is introduced, the second modifier is added for second modification immediately, and the surface of the calcium carbonate which is just deposited contains a large amount of hydroxyl, so that the second modifier can be firmly combined with the calcium carbonate, and the coating effect of the second modifier layer is improved; meanwhile, the coating of the second modifier can improve the compatibility of the powder particles and the organic resin; but also can improve the hydrophobicity of the powder and prevent the powder from absorbing moisture.
FIG. 1 is a flow chart of a preparation method of the reinforced flame-retardant powder for the sealant, provided by the invention, calcite is cleaned, crushed and calcined to obtain quicklime, and the quicklime and water are mixed for digestion and refining to obtain lime milk for later use. The brucite is cleaned, crushed and ground by a jet mill to obtain ground brucite, and the ground brucite is mixed with a first modifier and a crystal form inducer for first modification to obtain the modified brucite. And mixing the obtained modified brucite and lime cream for deposition coating to obtain a coating material liquid, mixing the coating material liquid with a second modifier for second modification, and then performing spray drying, collection and packaging to obtain the reinforced flame-retardant powder for the sealant.
The invention also provides the reinforced flame-retardant powder for the sealant, which is obtained by the preparation method in the technical scheme, wherein the granularity of the reinforced flame-retardant powder for the sealant is 2000-3000 meshes. In the invention, the shape of the reinforced flame-retardant powder for the sealant is preferably cubic, spherical or spindle. In the invention, the spherical powder has better fluidity and cube thixotropy when being applied.
The invention also provides the application of the reinforced flame-retardant powder for the sealant in the technical scheme as a reinforced flame retardant in the sealant. In the invention, when the reinforcing flame-retardant powder for the sealant is used as a reinforcing flame retardant in the sealant, the dosage of the reinforcing flame-retardant powder for the sealant is not particularly limited, and the reinforcing flame-retardant powder is set according to the positioning of downstream application products.
In the invention, the reinforced flame-retardant powder for the sealant has reinforced flame-retardant performance, can have good compatibility with resin, and can play a better reinforcing effect; the functional colloid has functionality, and can improve the rheological property of the colloid to a certain extent; the hygroscopicity is low, and the downstream production and processing are facilitated; has better flame retardance.
The reinforced flame-retardant powder for sealant and the preparation method and application thereof provided by the present invention are described in detail below with reference to the examples, but they should not be construed as limiting the scope of the present invention
Example 1
Washing and crushing brucite (the mass content of magnesium hydroxide is 88%), and grinding to 6000 meshes by using an airflow mill to obtain ground brucite;
3-aminopropyl trimethoxy silane, EDTA and MgSO4Uniformly mixing a small amount of water, adding the mixture and the ground brucite powder into a high-speed mixer, carrying out first modification for 25min at 2000r/min and 80 ℃, and sieving the modified brucite powder by using a 300-mesh sieve to obtain modified brucite for later use; wherein the mass of the 3-aminopropyl trimethoxy silane accounts for 1 percent of the mass of the ground brucite, and EDTA and MgSO4Each is 0.01 percent of the mass of the ground brucite;
cleaning and crushing calcite (the mass content of calcium carbonate is 97 percent), calcining at 1100 ℃ to obtain quicklime, adding water which is 5 times of the mass of the quicklime to digest, stirring at the speed of 60r/min during digestion, separating and refining a digestion liquid by using a multistage hydrocyclone after digestion is finished, standing and cooling to room temperature to obtain lime milk with the solid content of 82 percent;
lime is prepared fromMixing milk and modified brucite in a reaction kettle (the mass ratio of the lime milk to the modified brucite is 1: 2 in terms of calcium hydroxide), and blowing CO from the bottom of the reaction kettle under the conditions that the initial temperature is 15 ℃ and the stirring speed is 320r/min2(the molar ratio of the carbon dioxide to the calcium hydroxide in the lime milk is 1:1), maintaining the temperature not to exceed 30 ℃, and depositing and coating until CO is blown in2Finishing; immediately adjusting the temperature to 75 ℃ and the rotating speed to 200r/min, adding aluminate with the mass of 9 percent of the modified brucite, stirring for 45min, after the second modification is finished, spraying and drying, and sieving with a 300-mesh sieve to obtain the reinforced flame-retardant powder for the sealant.
The performance of the reinforced flame-retardant powder for sealant was tested, and the results are shown in Table 1. As can be seen from table 1: the whiteness of the powder is higher, the whiteness reaches more than 98, D50About 3 μm, particle size of about 2500 meshes, large specific surface area (18 m)2About/g, better thixotropy can be provided, the activation degree is high and is close to 100%, meanwhile, the moisture content is lower, and compared with the moisture content of about 0.3-0.8% of a common product, the water content of the product is low.
TABLE 1 results of performance test of the reinforced flame retardant powder for sealant obtained in example 1
Figure BDA0002641762200000091
FIG. 2 is a scanning electron micrograph of the reinforced flame retardant powder for sealant obtained in this example, and it can be seen from FIG. 2 that: the particle shape of the reinforced flame-retardant powder for the sealant is modified into a similar cube.
Application test:
kneading 400g of 8 ten thousand molecular weight 107 resin, 80g of 3# white oil, 27.63g of 201 silicone oil, 500g of light nano calcium and 380g of the reinforced flame-retardant powder for the sealant obtained in the example 1 in vacuum at 110 ℃ for 3 hours to uniformly disperse the materials; after the materials are cooled to below 40 ℃, putting the materials into a double-planetary power mixer, adding 44.24g of methyl tributyl ketoxime, and stirring for 30 minutes in vacuum at the rotating speed of 600 r/min; adding the rest 3.6-3.6 gKH-550 parts of material, 1.8-1.8 gKH-560 parts of dibutyltin dilaurate, and stirring at the rotating speed of 600r for 15min to obtain the sealant 1.
380g of the reinforced flame-retardant powder for the sealant obtained in example 1 in the sealant 1 was replaced with 380gHX-1250 mesh calcium carbonate to obtain a sealant 2.
The sealant was tested for maximum force, bond strength, elongation at break, consistency and oxygen index using a universal mechanical tester, an oxygen index tester and a putty consistometer, respectively, and the results are shown in table 2.
Table 2 performance test results for sealant 1 and sealant 2
Figure BDA0002641762200000092
As can be seen from table 2: when the special reinforcing flame-retardant powder for sealing is used for a sealant, the bonding strength and the elongation at break of the sealant are both higher than those of the sealant prepared by the traditional heavy calcium carbonate product, and the oxygen index is also higher than that of the sealant prepared by the traditional heavy calcium carbonate product.
Example 2
Washing and crushing brucite (the mass content of magnesium hydroxide is 89%), and grinding to 6000 meshes by using an airflow mill to obtain ground brucite;
uniformly mixing 3-methacryloxypropyltrimethoxysilane and glucose with a small amount of water, adding the mixture and the ground brucite into a high-speed mixer, carrying out first modification for 20min at the temperature of 110 ℃ at 2500r/min, and sieving the modified brucite through a 300-mesh sieve to obtain modified brucite for later use, wherein the mass of the 3-methacryloxypropyltrimethoxysilane is 1% of the mass of the ground brucite, and the mass of the glucose is 0.015% of the mass of the ground brucite;
cleaning and crushing calcite (the mass content of calcium carbonate is 97 percent), calcining at 1100 ℃ to form quicklime, adding water which is 5 times of the mass of the quicklime for digestion, stirring at the speed of 60r/min, after digestion is finished, separating and refining a digestion material liquid by using a multistage hydrocyclone, standing and cooling to room temperature to obtain lime milk with the solid content of 82 percent;
mixing lime milk and modified brucite in a reaction kettle (the mass ratio of the lime milk to the modified brucite is 1: 2 in terms of calcium hydroxide), and blowing CO from the bottom of the reaction kettle under the conditions that the initial temperature is 30 ℃ and the stirring speed is 280r/min2(the molar ratio of the carbon dioxide to the calcium hydroxide in the lime milk is 1:1), maintaining the temperature below 45 ℃, and depositing and coating until CO is blown in2Finishing; immediately adjusting the temperature to 85 ℃, adjusting the rotating speed to 240r/min, adding a mixture of sodium stearate and hydrogenated rosin with the mass of 10% of that of the modified brucite (the mass ratio of the sodium stearate to the hydrogenated rosin in the mixture is 3: 1), stirring for 45min, after the second modification is finished, spray-drying, and sieving with a 300-mesh sieve to obtain the reinforced flame-retardant powder for the sealant.
The properties of the reinforced flame retardant powder for sealants are shown in Table 3. As can be seen from table 3: the whiteness of the powder is higher, the whiteness reaches more than 98, D50The particle size and the specific surface area are slightly reduced at about 3 mu m, but compared with the traditional product, the thixotropic agent still can provide better thixotropy, the activation degree is high and is close to 100%, and meanwhile, the water content is lower, and compared with the water content of about 0.3-0.8% of the common product, the water content of the product is low.
TABLE 3 results of performance test of the reinforced flame retardant powder for sealant obtained in example 2
Figure BDA0002641762200000101
Figure BDA0002641762200000111
Example 3
Washing and crushing brucite (the mass content of magnesium hydroxide is 90%), and grinding to 6000 meshes by using an airflow mill to obtain ground brucite;
3-aminopropyl trimethoxy silane and AlCl3Glucose is mixed with small amount of water and ground brucitePutting the mixture into a high-speed mixer, performing first modification for 25min at the temperature of 110 ℃ at 2300r/min, and sieving the modified brucite by a 300-mesh sieve to obtain modified brucite for later use; wherein the mass of the 3-methacryloxypropyltrimethoxysilane accounts for 1 percent of the mass of the ground brucite, and the mass of the glucose and the AlCl3Each is 0.01 percent of the mass of the ground brucite;
cleaning and crushing calcite (the mass content of calcium carbonate is 97 percent), calcining at 1100 ℃ to form quicklime, adding water which is 5 times of the mass of the quicklime for digestion, stirring at the speed of 60r/min, after digestion is finished, separating and refining a digestion material liquid by using a multistage hydrocyclone, standing and cooling to room temperature to obtain lime milk with the solid content of 81 percent;
mixing lime milk and modified brucite in a reaction kettle (the mass ratio of the lime milk to the modified brucite is 1: 2 in terms of calcium hydroxide), and blowing CO from the bottom of the reaction kettle under the conditions that the initial temperature is 25 ℃ and the stirring speed is 60r/min2(the molar ratio of the carbon dioxide to the calcium hydroxide in the lime milk is 1:1), maintaining the temperature not to exceed 65 ℃, and depositing and coating until CO is blown in2Finishing; immediately adjusting the temperature to 85 ℃, adjusting the rotation speed to 150r/min, adding a mixture of sodium stearate and sodium dodecyl benzene sulfonate (the mass ratio of the sodium stearate to the sodium dodecyl benzene sulfonate in the mixture is 5: 1) with the mass of the modified brucite powder being 12%, stirring for 45min, after the second modification is finished, spraying and drying, and sieving with a 300-mesh sieve to obtain the reinforced flame-retardant powder for the sealant.
The performance of the reinforced flame retardant powder for sealant was tested, and the results are shown in Table 4. As can be seen from table 4: the whiteness of the powder is higher, the whiteness reaches more than 98, D50About 3 μm, the particle size is about 2000 meshes, the specific surface area is relatively large, 16m2About/g, better thixotropy can be provided, the activation degree is high and is close to 100%, meanwhile, the moisture content is lower, and compared with the moisture content of about 0.3-0.8% of a common product, the water content of the product is low.
TABLE 4 test results of the properties of the reinforced flame retardant powder for sealant obtained in example 3
Figure BDA0002641762200000121
The examples show that the reinforced flame-retardant powder for the sealant prepared by the invention has the advantages of high whiteness, large specific surface area, good thixotropy, high activation degree, low moisture content and flame-retardant effect. When the special reinforcing flame-retardant powder for sealing is used for a sealant, the bonding strength, the elongation at break and the oxygen index of the sealant are all higher than those of the sealant prepared by the traditional heavy calcium product.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. The preparation method of the reinforced flame-retardant powder for the sealant is characterized by comprising the following steps of:
grinding brucite to obtain ground brucite;
mixing the ground brucite, a first modifier and a crystal form inducer, and then carrying out first modification to obtain modified brucite; the first modifier is one or more of 3-aminopropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane and ethylenediamine tetraacetic acid;
mixing the modified brucite and the lime cream, and carrying out deposition coating to obtain a coating material liquid;
adding a second modifier into the coating material liquid for second modification to obtain the reinforced flame-retardant powder for the sealant; the second modifier is one or more of aluminate, sodium stearate, hydrogenated rosin and sodium dodecyl benzene sulfonate;
the crystal form inducer is MgSO4、AlCl3One or more of glucose and ethylene diamine tetraacetic acid; the addition amount of the crystal form inducer is 0.015-0.02% of the mass of the ground brucite.
2. The preparation method of claim 1, wherein the first modifier is added in an amount of 8-12% by weight of the ground brucite.
3. The method according to claim 1 or 2, wherein the first modification is carried out at a temperature of 80 to 120 ℃ for 15 to 30 min.
4. The preparation method of claim 1, wherein the solid content of the lime milk is 81-85%; the addition amount of the lime milk is 180-220% of the mass of the modified brucite in terms of calcium hydroxide.
5. A method as claimed in claim 1 or 4, wherein the deposit coating is bubbling CO2The deposition and coating are carried out under the condition, and the temperature of the deposition and coating is 30-45 ℃.
6. The preparation method according to claim 1, wherein the second modifier is added in an amount of 6 to 12% by mass of the modified brucite.
7. The method of claim 1 or 6, wherein the second modification is CO bubbling2The temperature of the second modification is 60-85 ℃, and the time is 40-50 min.
8. The reinforced flame-retardant powder for the sealant prepared by the preparation method of any one of claims 1 to 7, wherein the particle size of the reinforced flame-retardant powder for the sealant is 2000-3000 meshes.
9. The use of the reinforced flame retardant powder for sealant according to claim 8 as a reinforcing flame retardant in the field of sealants.
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CN106220890A (en) * 2016-07-26 2016-12-14 江苏西贝力新材料有限公司 A kind of preparation method of superfine active basic magnesite fire-retardant filler

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