CN113402902A - Production process of silicon-based sunscreen heat-insulation powder - Google Patents

Production process of silicon-based sunscreen heat-insulation powder Download PDF

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CN113402902A
CN113402902A CN202110682949.4A CN202110682949A CN113402902A CN 113402902 A CN113402902 A CN 113402902A CN 202110682949 A CN202110682949 A CN 202110682949A CN 113402902 A CN113402902 A CN 113402902A
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intermediate product
stirring
heat
dropwise adding
silicon
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刘溧
周喆
黄玉叶
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Jiangsu Mibaful Nano Material Co ltd
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Jiangsu Mibaful Nano Material 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
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/16—Preparation of silica xerogels
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043—Drying, calcination
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/32—Thermal properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/62—L* (lightness axis)

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Abstract

The invention discloses a production process of silicon-based sunscreen heat-insulating powder, which relates to the field of coatings2Adding alkali catalyst into hydrosol, and gelatinizing to obtain SiO2Gelling, aging, surface modification, drying, heat treatment and other processes to obtain dry gel coarse powder, and then performing air flow crushing to obtain aerogel microparticles; in the process, boric acid, calcium chloride, aluminum chloride and zirconium oxychloride are used as raw materials and are doped with SiO2In (1),the problems that the thermal conductivity coefficient of the nano silicon oxide thermal insulation material is sharply increased along with the temperature rise, and the thermal insulation capability at high temperature is greatly reduced are solved; by doping SiO with a modifier2Modifying to eliminate doped SiO2The surface has a large amount of hydroxyl groups, so that the coating can be easily dispersed in the coating, and the sun-proof and heat-insulating effects of the coating are further improved.

Description

Production process of silicon-based sunscreen heat-insulation powder
Technical Field
The invention relates to the field of coatings, in particular to a production process of silicon-based sunscreen heat-insulating powder.
Background
The existing sun-proof heat insulation in the building field is generally applied to reflective heat insulation coating, although the coating has good effect, the heat insulation performance of the coating still can not meet the requirement of the current high-grade green building on building energy conservation, so that the development of a new generation of green building sun-proof heat insulation product has important social benefit and potential huge economic benefit;
the unique microscopic nano structure of the silicon dioxide aerogel enables the silicon dioxide aerogel to have the characteristics of low density, high specific surface area and high porosity, and the characteristics enable the silicon dioxide aerogel to have unique excellent properties in the aspects of thermal, optical, electrical, acoustic and the like, so that the silicon dioxide aerogel can be used as a high-efficiency heat-insulation material, and the sun-proof heat-insulation coating taking silicon dioxide as a main material has good heat-insulation and sun-proof effects;
but the effective extinction coefficient of the nano silicon dioxide material to the wave band of 2.5-7.5 mu m is 0.1-19.5m2The temperature of the sample is measured by using a temperature measuring device, and the temperature of the sample is measured by using a temperature measuring device;
therefore, a doped silicon-based sunscreen and heat-insulating powder is needed to solve the above problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps: boric acid, calcium chloride, aluminum chloride and zirconium oxychloride are taken as raw materials and are doped with SiO2In the preparation of the doped microparticles, the problem that the thermal conductivity coefficient of the existing nano silicon oxide thermal insulation material is sharply increased along with the temperature rise, so that the thermal insulation capability of the existing nano silicon oxide thermal insulation material at high temperature is greatly reduced is solved.
The purpose of the invention can be realized by the following technical scheme:
a production process of silicon-based sunscreen heat-insulation powder comprises the following steps:
the method comprises the following steps: adding water glass and ethanol water solution into a three-neck flask provided with a stirrer and a constant pressure dropping funnel, and stirring at the stirring speed of 300-After 20-30min, the stirred product is subjected to ion exchange by using cation exchange resin to obtain an intermediate product A, namely SiO with the pH value of 2.1-2.42Hydrosol;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 20-30min, adding an alkali catalyst to adjust the pH of the reaction system to 5.0-5.5, then continuously stirring for 3-5min, standing for aging, and gelling to obtain an intermediate product B, namely the doped SiO2Gelling;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 10-30min under the condition that the ultrasonic frequency is 55-75kHz to obtain dispersion liquid of the intermediate product B;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.0-5.5, then stirring and dropwise adding a modifier under the condition that the stirring speed is 300-500r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10-15min after the dropwise adding is finished, then stirring and dropwise adding a dispersion liquid of an intermediate product B, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 20-30h after the dropwise adding is finished, centrifuging a reaction product after the reaction is finished, collecting a precipitate to obtain an intermediate product C, namely the modified doped SiO2；
Step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 2-3 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 60-70 ℃ for 3-5h, then calcining the dried product at 500 ℃ for 1h, then preserving heat for 4h, and cooling to room temperature to obtain an intermediate product D, namely dry gel coarse powder;
step six: and (3) performing air flow crushing on the intermediate product D to obtain aerogel microparticles, namely the silicon-based sunscreen heat-insulation powder.
As a further scheme of the invention: the dosage ratio of the water glass to the ethanol water solution in the first step is 0.40 mol: 1.0L, wherein the ethanol aqueous solution is prepared by mixing absolute ethanol and deionized water according to a volume ratio of 1: 8, and the ion exchange resin is strong-acid styrene cation exchange resin.
As a further scheme of the invention: and in the second step, the dopant is a solution formed by dissolving one or more than two of boric acid, calcium chloride, aluminum chloride and zirconium oxychloride in deionized water, the alkali catalyst is ammonia water, and the molar concentration of the ammonia water is 0.5-5 mol/L.
As a further scheme of the invention: the dosage ratio of the intermediate product B to the absolute ethyl alcohol in the third step is 1-10 g: 150 and 200 mL.
As a further scheme of the invention: the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B in the step four is 15-16 mL: 1-2 mL: 0.5-1 g: 15-20mL, wherein the modifier is a silane coupling agent KH-540 or a silane coupling agent KH-550.
The invention has the beneficial effects that:
the invention relates to a production process of silicon-based sun-proof heat-insulation powder, which is characterized in that industrial water glass is used as a silicon source, a sol-gel method is adopted to prepare silicon oxide-based sun-proof heat-insulation powder, and the water glass is treated by ion exchange resin to obtain SiO2Adding alkali catalyst into hydrosol, and gelatinizing to obtain SiO2And (3) gelling, aging, surface modification, drying, heat treatment and other processes to obtain dry gel coarse powder, and then performing air flow crushing to obtain the aerogel microparticles.
In the process, boric acid, calcium chloride, aluminum chloride and zirconium oxychloride are used as raw materials and are doped with SiO2The doped microparticles are prepared, and have the characteristics of higher reflectivity or refractive index, can change the propagation path of infrared radiation, play a role in blocking infrared radiation heat transfer, can generate a large scattering effect on infrared light, and solve the problems that the thermal conductivity of the nano silicon oxide heat-insulating material is sharply increased along with the temperature rise, so that the heat-insulating capability of the nano silicon oxide heat-insulating material at high temperature is greatly reduced; by doping SiO with a modifier2Modifying to eliminate doped SiO2The surface has a large amount of hydroxyl groups, so that the hydrophilicity of the coating is reduced, the coating can be more easily dispersed in the coating, and the sun-proof and heat-insulating effects of the coating are further improved.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the 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 embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 20min under the condition that the stirring speed is 300r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 20min, adding an alkali catalyst to adjust the pH of the reaction system to 5.0, then continuously stirring for 3min, standing for aging, and gelling to obtain an intermediate product B; controlling the dopant to be boric acid, the alkali catalyst to be ammonia water, and the molar concentration of the ammonia water to be 0.5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 10min under the condition that the ultrasonic frequency is 55kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 1 g: 150 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.0, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 300r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 20h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 15 mL: 1mL of: 0.5 g: 15mL, the modifier is a silane coupling agent KH-540;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 2 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 60 ℃ for 3 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Example 2:
the embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 30min under the condition that the stirring speed is 500r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 30min, adding an alkali catalyst to adjust the pH of the reaction system to 5.5, then continuously stirring for 5min, standing for aging, and gelling to obtain an intermediate product B; controlling a doping agent to be boric acid, wherein the doping amount is 2 times that of example 1, an alkali catalyst is ammonia water, and the molar concentration of the ammonia water is 5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 30min under the condition that the ultrasonic frequency is 75kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 10 g: 200 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.5, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 500r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 15min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 30h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 16 mL: 2mL of: 1 g: 20mL, the modifier is a silane coupling agent KH-550;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 3 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 70 ℃ for 5 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Example 3:
the embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 20min under the condition that the stirring speed is 300r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 20min, adding an alkali catalyst to adjust the pH of the reaction system to 5.0, then continuously stirring for 3min, standing for aging, and gelling to obtain an intermediate product B; controlling the dopant to be calcium chloride, the alkali catalyst to be ammonia water, and the molar concentration of the ammonia water to be 0.5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 10min under the condition that the ultrasonic frequency is 55kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 1 g: 150 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.0, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 300r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 20h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 15 mL: 1mL of: 0.5 g: 15mL, the modifier is a silane coupling agent KH-540;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 2 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 60 ℃ for 3 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Example 4:
the embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 30min under the condition that the stirring speed is 500r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 30min, adding an alkali catalyst to adjust the pH of the reaction system to 5.5, then continuously stirring for 5min, standing for aging, and gelling to obtain an intermediate product B; controlling a doping agent to be calcium chloride, wherein the doping amount is 2 times that of example 3, an alkali catalyst is ammonia water, and the molar concentration of the ammonia water is 5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 30min under the condition that the ultrasonic frequency is 75kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 10 g: 200 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.5, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 500r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 15min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 30h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 16 mL: 2mL of: 1 g: 20mL, the modifier is a silane coupling agent KH-550;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 3 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 70 ℃ for 5 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Example 5:
the embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 20min under the condition that the stirring speed is 300r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 20min, adding an alkali catalyst to adjust the pH of the reaction system to 5.0, then continuously stirring for 3min, standing for aging, and gelling to obtain an intermediate product B; controlling the dopant to be aluminum chloride, the alkali catalyst to be ammonia water, and the molar concentration of the ammonia water to be 0.5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 10min under the condition that the ultrasonic frequency is 55kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 1 g: 150 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.0, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 300r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 20h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 15 mL: 1mL of: 0.5 g: 15mL, the modifier is a silane coupling agent KH-540;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 2 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 60 ℃ for 3 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Example 6:
the embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 30min under the condition that the stirring speed is 500r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 30min, adding an alkali catalyst to adjust the pH of the reaction system to 5.5, then continuously stirring for 5min, standing for aging, and gelling to obtain an intermediate product B; controlling a doping agent to be aluminum chloride, wherein the doping amount is 2 times that of example 5, an alkali catalyst is ammonia water, and the molar concentration of the ammonia water is 5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 30min under the condition that the ultrasonic frequency is 75kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 10 g: 200 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.5, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 500r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 15min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 30h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 16 mL: 2mL of: 1 g: 20mL, the modifier is a silane coupling agent KH-550;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 3 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 70 ℃ for 5 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Example 7:
the embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 20min under the condition that the stirring speed is 300r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 20min, adding an alkali catalyst to adjust the pH of the reaction system to 5.0, then continuously stirring for 3min, standing for aging, and gelling to obtain an intermediate product B; controlling the dopant to be zirconium oxychloride, the alkali catalyst to be ammonia water, and the molar concentration of the ammonia water to be 0.5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 10min under the condition that the ultrasonic frequency is 55kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 1 g: 150 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.0, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 300r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 20h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 15 mL: 1mL of: 0.5 g: 15mL, the modifier is a silane coupling agent KH-540;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 2 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 60 ℃ for 3 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Example 8:
the embodiment is a production process of silicon-based sunscreen heat-insulating powder, which comprises the following steps:
the method comprises the following steps: adding water glass and an ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 30min under the condition that the stirring speed is 500r/min, and then performing ion exchange on a stirring product by using cation exchange resin to obtain an intermediate product A; controlling the dosage ratio of the water glass to the ethanol water solution to be 0.40 mol: 1.0L, wherein the ethanol aqueous solution is absolute ethanol and deionized water according to the volume ratio of 1: 8, ion exchange resin is strong acid styrene cation exchange resin;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 30min, adding an alkali catalyst to adjust the pH of the reaction system to 5.5, then continuously stirring for 5min, standing for aging, and gelling to obtain an intermediate product B; controlling a doping agent to be zirconium oxychloride, wherein the doping amount is 2 times that of example 7, an alkali catalyst is ammonia water, and the molar concentration of the ammonia water is 5 mol/L;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 30min under the condition that the ultrasonic frequency is 75kHz to obtain dispersion liquid of the intermediate product B; controlling the dosage ratio of the intermediate product B to the absolute ethyl alcohol to be 10 g: 200 mL;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.5, then dropwise adding the mixture into a modifier while stirring under the condition that the stirring speed is 500r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 15min after the dropwise adding is finished, then dropwise adding the dispersion liquid of an intermediate product B while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 30h after the dropwise adding is finished, centrifuging the reaction product after the reaction is finished, and collecting precipitates to obtain an intermediate product C; controlling the dosage ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B to be 16 mL: 2mL of: 1 g: 20mL, the modifier is a silane coupling agent KH-550;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 3 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 70 ℃ for 5 hours, then placing the dried product at 500 ℃ for calcining for 1 hour, then preserving heat for 4 hours, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
Comparative example 1:
comparative example 1 differs from example 8 in that no dopant is added and the remaining steps are the same.
The silicon-based sunscreen heat-insulating powder of the examples 1 to 8 and the comparative example 1 is detected, the heat-insulating property at the temperature of 20 to 800 ℃ is detected, and the detection result is as follows:
Figure BDA0003123395950000131
referring to the data in the above table, it can be seen that the silicon-based sunscreen thermal insulation powder has a good thermal insulation effect at a low temperature without adding any dopant, but the thermal insulation performance is greatly reduced after the temperature is raised, and the silicon-based sunscreen thermal insulation powder has good thermal insulation performance at 20-800 ℃ after adding the dopant.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.

Claims (5)

1. A production process of silicon-based sunscreen heat-insulation powder is characterized by comprising the following steps:
the method comprises the following steps: adding water glass and ethanol water solution into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, stirring for 20-30min under the condition that the stirring speed is 300-500r/min, and then performing ion exchange on the stirred product by using cation exchange resin to obtain an intermediate product A;
step two: dropwise adding a doping agent into the intermediate product A, continuously stirring for 20-30min, adding an alkali catalyst to adjust the pH of the reaction system to 5.0-5.5, then continuously stirring for 3-5min, standing for aging, and gelling to obtain an intermediate product B;
step three: adding the intermediate product B into absolute ethyl alcohol, and performing ultrasonic dispersion for 10-30min under the condition that the ultrasonic frequency is 55-75kHz to obtain dispersion liquid of the intermediate product B;
step four: adding absolute ethyl alcohol a and deionized water into a three-neck flask provided with a stirrer and a constant-pressure dropping funnel, adding glacial acetic acid to adjust the pH value to 5.0-5.5, then stirring and dropwise adding the modifier under the condition that the stirring speed is 300-500r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10-15min after dropwise adding is finished, then stirring and dropwise adding the dispersion liquid of the intermediate product B, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 20-30h after dropwise adding is finished, centrifuging the reaction product after the reaction is finished, collecting precipitate, and obtaining an intermediate product C;
step five: washing the intermediate product C with absolute ethyl alcohol b, tetrahydrofuran and acetone for 2-3 times in sequence, centrifuging, placing the precipitate in a vacuum drying oven, drying at 60-70 ℃ for 3-5h, then calcining the dried product at 500 ℃ for 1h, then preserving heat for 4h, and cooling to room temperature to obtain an intermediate product D;
step six: and (4) carrying out jet milling on the intermediate product D to obtain the silicon-based sunscreen heat-insulating powder.
2. The production process of the silicon-based sunscreen and heat insulation powder as claimed in claim 1, wherein the dosage ratio of the water glass to the ethanol aqueous solution in the first step is 0.40 mol: 1.0L, wherein the ethanol aqueous solution is prepared by mixing absolute ethanol and deionized water according to a volume ratio of 1: 8, and the ion exchange resin is strong-acid styrene cation exchange resin.
3. The process for producing a silicon-based sunscreen thermal insulation powder according to claim 1, wherein the dopant in the second step is a solution formed by dissolving one or more of boric acid, calcium chloride, aluminum chloride and zirconium oxychloride in deionized water, the alkali catalyst is ammonia water, and the molar concentration of the ammonia water is 0.5-5 mol/L.
4. The production process of the silicon-based sunscreen and heat-insulating powder as claimed in claim 1, wherein the dosage ratio of the intermediate product B to the absolute ethyl alcohol in the third step is 1-10 g: 150 and 200 mL.
5. The production process of the silicon-based sunscreen and heat-insulating powder as claimed in claim 1, wherein the amount ratio of the absolute ethyl alcohol a, the deionized water, the modifier and the dispersion liquid of the intermediate product B in the fourth step is 15-16 mL: 1-2 mL: 0.5-1 g: 15-20mL, wherein the modifier is a silane coupling agent KH-540 or a silane coupling agent KH-550.
CN202110682949.4A 2021-06-21 2021-06-21 Production process of silicon-based sunscreen heat-insulation powder Pending CN113402902A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1241953A (en) * 1996-11-26 2000-01-19 卡伯特公司 Method for producing organically modified, permanently hydrophobic aerogels
CN101200293A (en) * 2007-11-16 2008-06-18 北京科技大学 Method for rapid preparation of SiO2 aerogel micro-balloons
CN106745000A (en) * 2016-12-23 2017-05-31 伊科纳诺（北京）科技发展有限公司 A kind of preparation method of waterglass base aerosil
CN107662923A (en) * 2017-10-19 2018-02-06 加新科技(深圳)有限公司 A kind of continuous boron for preparing adulterates SiO2The method of aeroge

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1241953A (en) * 1996-11-26 2000-01-19 卡伯特公司 Method for producing organically modified, permanently hydrophobic aerogels
CN101200293A (en) * 2007-11-16 2008-06-18 北京科技大学 Method for rapid preparation of SiO2 aerogel micro-balloons
CN106745000A (en) * 2016-12-23 2017-05-31 伊科纳诺（北京）科技发展有限公司 A kind of preparation method of waterglass base aerosil
CN107662923A (en) * 2017-10-19 2018-02-06 加新科技(深圳)有限公司 A kind of continuous boron for preparing adulterates SiO2The method of aeroge

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
江包家褀: "铝掺杂二氧化硅溶胶、气凝胶及其复合材料的制备", 《工程科技I辑》 *

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