CN111995882A - Porous calcium silicate rare earth ion-loaded filler powder and preparation method thereof - Google Patents

Porous calcium silicate rare earth ion-loaded filler powder and preparation method thereof Download PDF

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CN111995882A
CN111995882A CN202010770672.6A CN202010770672A CN111995882A CN 111995882 A CN111995882 A CN 111995882A CN 202010770672 A CN202010770672 A CN 202010770672A CN 111995882 A CN111995882 A CN 111995882A
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calcium silicate
rare earth
porous calcium
earth ion
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张印民
张永锋
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Inner Mongolia University of Technology
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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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
    • C09C3/041—Grinding
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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
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • 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
    • C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
    • 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
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    • C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2201/005—Additives being defined by their particle size in general
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    • C08K2201/00—Specific properties of additives
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Abstract

The invention discloses a functional filler prepared by porous calcium silicate loaded rare earth ions and a preparation method thereof, wherein the porous calcium silicate raw material is added with water and a dispersant according to the weight proportion to prepare a suspension; preparing a soluble precursor of a rare earth component and water into impregnation liquid according to a weight ratio, mixing the porous calcium silicate suspension and the rare earth component impregnation liquid, adjusting the pH value of the system to 8-11, and uniformly stirring; after the reaction is finished, directly spray-drying or drying and roasting after filtering and washing(ii) a Finally, after crushing and scattering, obtaining porous calcium silicate loaded rare earth ion powder with the average particle size of 1-10 mu m and the specific surface area of 150-200 m2(ii) in terms of/g. The invention improves and enhances the processing property, the mechanical property, the flame retardant property and the like of the polymer composite material product; meanwhile, the large specific surface area of the porous calcium silicate can also provide a good carrier environment for various active components.

Description

Porous calcium silicate rare earth ion-loaded filler powder and preparation method thereof
Technical Field
The invention belongs to the field of inorganic functional fillers, and particularly relates to porous calcium silicate rare earth ion-loaded filler powder and a preparation method thereof.
Background
The enhancement modification of the polymer material is an important component for improving the application performance of the polymer product, which is the key point of research in the fields of polymer material science and engineering, and the design of the reinforcing filler is an effective, universal and cheap means for the enhancement modification of the polymer material. With the enhancement of social environmental awareness, the research on non-petroleum-based green functional reinforcing filler is one of the future development trends in the field of polymer reinforcement.
When the rare earth element filled polymer is acted by external force, transient huge complex compounds can be formed between the rare earth element and polymer molecules, so that the aging resistance, fatigue resistance, heat resistance, oil resistance and other properties of the filled polymer material are obviously improved. The research trend in the field of rare earth reinforced modified polymers is nanocrystallization, multifunction and low cost. However, rare earth particles are easy to agglomerate after being nanocrystallized, so that the reinforcing and modifying effect is greatly reduced, and how to ensure that nanoscale rare earth particles are uniformly dispersed in a polymer system becomes a precondition for realizing the rare earth functionality, a functional filler capable of being prepared by loading rare earth ions and a preparation method thereof are needed.
Disclosure of Invention
The invention aims to provide a filler powder product of porous calcium silicate loaded with rare earth ions, which realizes the uniform dispersion of rare earth components and the surface modification of porous calcium silicate and can be widely applied to the fields of polymers, plastics, catalysis and the like.
The invention also aims to provide a preparation method of the porous calcium silicate rare earth ion-loaded filler powder product, which is low in cost and easy for industrial production.
In order to achieve the purpose of the invention, the invention provides a preparation method of porous calcium silicate rare earth ion-loaded filler powder, which comprises the following steps: adding water and a dispersing agent into a porous calcium silicate raw material according to a weight ratio to prepare a suspension;
1) preparing a soluble precursor of a rare earth component into impregnation liquid in water according to a weight ratio, wherein the rare earth ion component is in a lanthanum or cerium compound form, and the compound form is an oxide or carboxylate form; the proportion of the rare earth component and the active calcium silicate is 1.5 to 30 percent; when the double rare earth ion component is adopted, the ratio of two metal elements, namely lanthanum and cerium, is 2: 1 to 1: 2;
2) mixing the porous calcium silicate suspension with the rare earth component impregnation liquid, adjusting the pH value of the system to 8-11, and uniformly stirring; after the reaction is finished, directly carrying out spray drying or drying and roasting after filtering and washing;
3) finally, after crushing and scattering, obtaining porous calcium silicate loaded rare earth ion powder with the average particle size of 1-10 mu m and the specific surface area of 150-200 m2/g。
Further, the porous calcium silicate is prepared by hydrothermal synthesis, the average particle size of the porous calcium silicate is 1-5 mu m, and the specific surface area of the porous calcium silicate is 170-300 m2/g。
Further, the porous calcium silicate raw material in the step 1) is refined through a grinding and stripping machine; the stirring speed is 400-1500 rpm, the grinding and peeling time is 1-2 hours, and the content of the suspension during grinding and peeling is 15-35%.
Further, the addition amount of the dispersing agent in the step 1) is 0.5-1.5% of the weight of the porous calcium silicate, and the preferable addition proportion is 0.5-1.0% of the porous calcium silicate; the dispersing agent is one of sodium polyacrylate, sodium stearate and sodium hexametaphosphate; the stirring speed is 400-500 rpm, the stirring time is 0.5-1 hour, and the solid content of the suspension is 15-25%.
Further, the rare earth soluble precursor in the step 2) is one or more of hydrated lanthanum nitrate, lanthanum chloride, cerium nitrate hexahydrate or ammonium ceric nitrate; the mass fraction of the impregnation liquid is 1-10%.
Further, the alkaline substance for adjusting the pH value in step 3) is one of ammonia water, tetraethylammonium hydroxide or tetramethylammonium hydroxide, and it is preferably ammonia water.
Further, the mixing and stirring time of the porous calcium silicate suspension and the impregnation liquid in the step 3) is 5-40 minutes, and the mixing and stirring temperature is 30-75 ℃.
Further, the temperature of the spray drying in the step 3) is 350-450 ℃; the drying temperature is 105-120 ℃, the roasting temperature is 350-450 ℃, and the roasting time is 2-4 hours.
Further, the crushing and breaking in the step 4) are carried out in a high-speed crusher, a breaker or a high-speed mechanical impact mill at 1000 rpm-4500 rpm for 1 min-10 min.
The filler powder is subjected to dispersed loading through porous calcium silicate, the average particle size of the filler powder is 1-10 mu m, and the specific surface area of the filler powder is 150-200 m2The mass ratio of the rare earth ion component to the active calcium silicate is 1 to 30 percent.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of porous calcium silicate-loaded rare earth ion filler powder.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings.
As shown in fig. 1, a method for preparing a functional filler by using porous calcium silicate loaded rare earth ions, which comprises the following steps:
examples 1
1) Preparing a soluble precursor of a rare earth component into impregnation liquid in water according to a weight ratio, wherein the rare earth ion component is in the form of lanthanum or cerium oxide or carboxylate; lanthanum oxide with a rare earth component to active calcium silicate ratio of 30% when a double rare earth ionic component is used, the ratio of the two metal elements lanthanum and cerium is 2: 1;
2) the porous calcium silicate is prepared by hydrothermal synthesis, the average particle size of the porous calcium silicate is 1 μm, and the specific surface area is 170m2(ii) in terms of/g. Refining the porous calcium silicate raw material by a grinding and stripping machine; the stirring speed is 500 r/min, the grinding and peeling time is 1 hour, and the content of the suspension during grinding and peeling is 15 percent.
3) Mixing the porous calcium silicate suspension with the rare earth component impregnation liquid, adjusting the pH value of the system to 9, uniformly stirring, and adjusting the pH value to obtain an alkaline substance which is ammonia water; after the reaction is finished, directly carrying out spray drying or drying and roasting after filtering and washing, wherein the addition amount of the dispersing agent is 0.5 percent of the weight of the porous calcium silicate, the dispersing agent is sodium stearate, the mixing and stirring time of the porous calcium silicate suspension and the impregnation liquid is 5 minutes, the mixing and stirring temperature is 30 ℃, the stirring speed is 400 r/m, the stirring time is 0.5 hour, and the solid content of the suspension is 15 percent. The rare earth soluble precursor is hydrated lanthanum nitrate, and the temperature of spray drying is 360 ℃; the drying temperature is 110 ℃, the roasting temperature is 350 ℃, and the roasting time is 2 hours.
4) Finally, after crushing and scattering, obtaining porous calcium silicate loaded rare earth ion powder with average particle size of 1-10 mu m and specific surface area of 150m2(ii) in terms of/g. The comminution is carried out in a high-speed comminution mechanical impact mill at 1000 rpm for 3 minutes.
The obtained porous calcium silicate-loaded rare earth ion filler powder is subjected to dispersion loading through porous calcium silicate, the average particle size of the filler powder is 5 mu m, and the specific surface area is 160m2The mass ratio of the rare earth ion component to the active calcium silicate is 15 percent.
Example 2 of embodiment
1) Preparing a soluble precursor of a rare earth component into impregnation liquid in water according to a weight ratio, wherein the rare earth ion component is in the form of lanthanum or cerium oxide or carboxylate; cerium oxide with a ratio of rare earth component to active calcium silicate of 30% when a double rare earth ionic component is used, the ratio of the two metal elements lanthanum and cerium is 1: 2;
2) the porous calcium silicate is prepared by hydrothermal synthesis, the average particle size of the porous calcium silicate is 5 mu m, and the specific surface area of the porous calcium silicate is 170m2(ii) in terms of/g. Refining the porous calcium silicate raw material by a grinding and stripping machine; the stirring speed is 500 r/min, the grinding and peeling time is 1 hour, and the content of the suspension during grinding and peeling is 20 percent.
3) Mixing the porous calcium silicate suspension with the rare earth component impregnation liquid, adjusting the pH value of the system to 10, uniformly stirring, and adjusting the pH value to obtain an alkaline substance which is ammonia water; after the reaction is finished, directly carrying out spray drying or drying and roasting after filtering and washing, wherein the addition amount of the dispersing agent is 1.0 percent of the weight of the porous calcium silicate, the dispersing agent is sodium stearate, the mixing and stirring time of the porous calcium silicate suspension and the impregnation liquid is 5 minutes, the mixing and stirring temperature is 30 ℃, the stirring speed is 400 r/m, the stirring time is 0.5 hour, and the solid content of the suspension is 15 percent. The rare earth soluble precursor is lanthanum nitrate, and the temperature of spray drying is 360 ℃; the drying temperature is 110 ℃, the roasting temperature is 400 ℃, and the roasting time is 2 hours.
4) Finally, after crushing and scattering, porous calcium silicate loaded rare earth ion powder is obtained, the average particle size is 6 mu m, and the specific surface area is 190m2(ii) in terms of/g. The comminution is carried out in a high-speed comminution mechanical impact mill at 1000 rpm for 6 minutes.
The obtained porous calcium silicate-loaded rare earth ion filler powder is subjected to dispersion loading through porous calcium silicate, the average particle size of the filler powder is 6 mu m, and the specific surface area is 190m2The mass ratio of the rare earth ion component to the active calcium silicate is 25 percent.
EXAMPLE 3
1) Preparing a soluble precursor of a rare earth component into impregnation liquid in water according to a weight ratio, wherein the rare earth ion component is in the form of lanthanum or cerium oxide or carboxylate; lanthanum oxide with a rare earth component to active calcium silicate ratio of 30% when a double rare earth ionic component is used, the ratio of the two metal elements lanthanum and cerium is 2: 1;
2) the porous calcium silicate is prepared by hydrothermal synthesis, the average particle size of the porous calcium silicate is 5 mu m, and the specific surface area is 270m2(ii) in terms of/g. Refining the porous calcium silicate raw material by a grinding and stripping machine; the stirring speed is 1500 rpm, the grinding and peeling time is 2 hours, and the content of the suspension during grinding and peeling is 35 percent.
3) Mixing the porous calcium silicate suspension with the rare earth component impregnation liquid, adjusting the pH value of the system to 11, uniformly stirring, and adjusting the pH value to obtain an alkaline substance tetraethylammonium hydroxide; after the reaction is finished, directly carrying out spray drying or drying and roasting after filtering and washing, wherein the addition amount of the dispersing agent is 1.0 percent of the weight of the porous calcium silicate; the dispersing agent is sodium hexametaphosphate, the mixing and stirring time of the porous calcium silicate suspension and the impregnation liquid is 5 minutes, the mixing and stirring temperature is 30 ℃, the stirring speed is 500 r/min, the stirring time is 1 hour, and the solid content of the suspension is 25 percent. The rare earth soluble precursor is ammonium ceric nitrate, and the temperature of spray drying is 450 ℃; the drying temperature is 120 ℃, the roasting temperature is 450 ℃, and the roasting time is 4 hours.
4) Finally, after crushing and scattering, porous calcium silicate loaded rare earth ion powder is obtained, the average particle size is 10 mu m, and the specific surface area is 200m2(ii) in terms of/g. The pulverization and breaking are carried out in a mechanical impact mill with high-speed pulverization at 4000 rpm for 10 minutes.
The obtained porous calcium silicate-loaded rare earth ion filler powder is subjected to dispersion loading through porous calcium silicate, the average particle size of the filler powder is 10 mu m, and the specific surface area is 200m2The mass ratio of the rare earth ion component to the active calcium silicate is 30 percent.
The porous calcium silicate is artificially synthesized by a hydrothermal method, has the characteristics of low density, large specific surface area and the like, is a fluffy porous structural inorganic material with aggregates, has the characteristics of void development in the particle and honeycomb aggregate appearance, has high adsorption property to powder due to the pore effect, light base effect, nano effect and strong light base holding capacity of the particles, and can improve and enhance the processing property, mechanical property, flame retardant property and the like of a polymer composite material product by using the inorganic reinforced filler as a non-petroleum base green functional inorganic reinforced filler; meanwhile, the large specific surface area of the porous calcium silicate can also provide a good carrier environment for various active components.
Although the embodiments of the present invention have been described above, the above descriptions are only for the convenience of understanding the present invention, and are not intended to limit the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The preparation method of the porous calcium silicate rare earth ion-loaded filler powder is characterized by comprising the following steps:
1) adding water and a dispersing agent into a porous calcium silicate raw material according to a weight ratio to prepare a suspension;
2) preparing a soluble precursor of a rare earth component into impregnation liquid in water according to a weight ratio, wherein the rare earth ion component is in a lanthanum or cerium compound form, and the compound form is an oxide or carboxylate form; the proportion of the rare earth component and the active calcium silicate is 1.5 to 30 percent; when the double rare earth ion component is adopted, the ratio of two metal elements, namely lanthanum and cerium, is 2: 1 to 1: 2;
3) mixing the porous calcium silicate suspension with the rare earth component impregnation liquid, adjusting the pH value of the system to 8-11, and uniformly stirring; after the reaction is finished, directly carrying out spray drying or drying and roasting after filtering and washing;
4) finally, after crushing and scattering, obtaining porous calcium silicate loaded rare earth ion powder with the average particle size of 1-10 mu m and the specific surface area of 150-200 m2/g。
2. The method for preparing the porous calcium silicate rare earth ion-loaded filler powder according to claim 1, wherein the porous calcium silicate is prepared by hydrothermal synthesis, the average particle size of the porous calcium silicate is 1-5 μm, and the specific surface area of the porous calcium silicate is 170-300 m2/g。
3. The preparation method of the porous calcium silicate rare earth ion-loaded filler powder according to claim 1, characterized in that the porous calcium silicate raw material in the step 1) is refined by a mill-stripper; the stirring speed is 400-1500 rpm, the grinding and peeling time is 1-2 hours, and the content of the suspension during grinding and peeling is 15-35%.
4. The porous calcium silicate rare earth ion-loaded filler powder and the preparation method thereof according to claim 1, wherein the addition amount of the dispersant in the step 1) is 0.5-1.5% of the weight of the porous calcium silicate, and the preferable addition ratio is 0.5-1.0% of the porous calcium silicate; the dispersing agent is one of sodium polyacrylate, sodium stearate and sodium hexametaphosphate; the stirring speed is 400-500 rpm, the stirring time is 0.5-1 hour, and the solid content of the suspension is 15-25%.
5. The method for preparing the porous calcium silicate rare earth ion-loaded filler powder according to claim 1, wherein the rare earth soluble precursor in the step 2) is one or more of lanthanum nitrate hydrate, lanthanum chloride, cerium nitrate hexahydrate and ammonium cerium nitrate; the mass fraction of the impregnation liquid is 1-10%.
6. The method for preparing the porous calcium silicate rare earth ion-loaded filler powder according to claim 1, wherein the alkaline substance for regulating the pH value in the step 3) is one of ammonia water, tetraethylammonium hydroxide or tetramethylammonium hydroxide, and preferably the alkaline substance is ammonia water.
7. The method for preparing the porous calcium silicate rare earth ion-loaded filler powder according to claim 1, wherein the mixing and stirring time of the porous calcium silicate suspension and the impregnation liquid in the step 3) is 5-40 minutes, and the mixing and stirring temperature is 30-75 ℃.
8. The method for preparing the porous calcium silicate rare earth ion-loaded filler powder according to claim 1, wherein the temperature of the spray drying in the step 3) is 350-450 ℃; the drying temperature is 105-120 ℃, the roasting temperature is 350-450 ℃, and the roasting time is 2-4 hours.
9. The method for preparing the porous calcium silicate rare earth ion-loaded filler powder according to claim 1, wherein the pulverization and scattering in the step 4) are performed in a high-speed pulverizer, a scattering machine or a high-speed mechanical impact mill at 1000 rpm to 4500 rpm for 1 minute to 10 minutes.
10. The filler powder of porous calcium silicate loaded rare earth ions is characterized in that the filler powder is dispersed and loaded through porous calcium silicate, the average particle size of the filler powder is 1-10 mu m, and the specific surface area of the filler powder is 150-200 m2The mass ratio of the rare earth ion component to the active calcium silicate is 1 to 30 percent.
CN202010770672.6A 2020-08-04 2020-08-04 Porous calcium silicate rare earth ion-loaded filler powder and preparation method thereof Pending CN111995882A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1698932A (en) * 2005-04-21 2005-11-23 内蒙古大学 Supported nano gold catalyst for clearing formaldehyde from indoor air and method for preparing the same
CN101658790A (en) * 2008-08-28 2010-03-03 北京三聚环保新材料股份有限公司 Method for preparing dehydrogenation catalyst
CN103785413A (en) * 2012-10-31 2014-05-14 中国石油化工股份有限公司 Hydrogenation catalyst, and preparation method and application thereof
CN103816908A (en) * 2014-03-20 2014-05-28 神华集团有限责任公司 Catalyst for preparing alcohol by hydrogenising acetate and preparation method of catalyst
CN104194404A (en) * 2014-08-20 2014-12-10 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 Active calcium silicate, and preparation method and application thereof
CN106391021A (en) * 2016-08-19 2017-02-15 内蒙古大学 Preparation method and use of high dispersion supported catalyst for methane reforming with carbon dioxide
CN107754849A (en) * 2017-11-17 2018-03-06 西安元创化工科技股份有限公司 A kind of preparation method of support type high temperature denitrating catalyst
CN108031433A (en) * 2017-12-14 2018-05-15 湖南科技大学 A kind of preparation method of mesoporous calcium silicates load nano zero-valence iron composite material
CN110841589A (en) * 2019-12-16 2020-02-28 北京工商大学 Adsorbent with photocatalytic activity and preparation method and application thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1698932A (en) * 2005-04-21 2005-11-23 内蒙古大学 Supported nano gold catalyst for clearing formaldehyde from indoor air and method for preparing the same
CN101658790A (en) * 2008-08-28 2010-03-03 北京三聚环保新材料股份有限公司 Method for preparing dehydrogenation catalyst
CN103785413A (en) * 2012-10-31 2014-05-14 中国石油化工股份有限公司 Hydrogenation catalyst, and preparation method and application thereof
CN103816908A (en) * 2014-03-20 2014-05-28 神华集团有限责任公司 Catalyst for preparing alcohol by hydrogenising acetate and preparation method of catalyst
CN104194404A (en) * 2014-08-20 2014-12-10 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 Active calcium silicate, and preparation method and application thereof
CN106391021A (en) * 2016-08-19 2017-02-15 内蒙古大学 Preparation method and use of high dispersion supported catalyst for methane reforming with carbon dioxide
CN107754849A (en) * 2017-11-17 2018-03-06 西安元创化工科技股份有限公司 A kind of preparation method of support type high temperature denitrating catalyst
CN108031433A (en) * 2017-12-14 2018-05-15 湖南科技大学 A kind of preparation method of mesoporous calcium silicates load nano zero-valence iron composite material
CN110841589A (en) * 2019-12-16 2020-02-28 北京工商大学 Adsorbent with photocatalytic activity and preparation method and application thereof

Non-Patent Citations (8)

* Cited by examiner, † Cited by third party
Title
FENG WANG ET AL.: "High adsorption activated calcium silicate enabling high-capacity adsorption for sulfur dioxide", 《NEW JOURNAL OF CHEMISTRY》 *
LE KANG ET AL.: "Preparation, characterization and photocatalytic activity of novel CeO2 loaded porous alkali-activated steel slag-based binding material", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》 *
XIAOYAN WANG ET AL.: "Study on the correlation between pore morphology of porous calcium silicate and high capacity formaldehyde adsorption", 《ENVIRONMENTAL TECHNOLOGY》 *
康乐等: "CeO2负载多孔碱激发钢渣基催化剂的制备及其光催化性能", 《光谱学与光谱分析》 *
徐祥瀚等: "高比表面多孔材料的制备研究进展 ", 《粉末冶金工业》 *
梁海欧: "多孔硅酸钙载银系掺杂二氧化钛光催化剂的制备及性能研究", 《中国优秀硕士学位论文全文数据库》 *
郭文霞等: "TiO2/CaSiO3复合型光催化剂的制备及其性能研究", 《广州化工》 *
金凌云等: "CeO2-Y2O3涂层和负载型Pd催化剂催化燃烧VOCs(英文)", 《物理化学学报》 *

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