CN115159532A - Method for preparing porous white carbon black by taking industrial silicon dioxide solid waste as raw material - Google Patents
Method for preparing porous white carbon black by taking industrial silicon dioxide solid waste as raw material Download PDFInfo
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- CN115159532A CN115159532A CN202210973555.9A CN202210973555A CN115159532A CN 115159532 A CN115159532 A CN 115159532A CN 202210973555 A CN202210973555 A CN 202210973555A CN 115159532 A CN115159532 A CN 115159532A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 175
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 65
- 239000006229 carbon black Substances 0.000 title claims abstract description 44
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000002994 raw material Substances 0.000 title claims abstract description 20
- 239000002910 solid waste Substances 0.000 title claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000006227 byproduct Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- 230000032683 aging Effects 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims description 8
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000018109 developmental process Effects 0.000 abstract description 3
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010415 colloidal nanoparticle Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000010423 industrial mineral Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Classifications
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- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- 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
- C01P2006/12—Surface area
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for preparing porous white carbon black by taking industrial silicon dioxide solid waste as a raw material, which belongs to the technical field of novel porous white carbon black development and comprises the following steps: taking industrial byproducts containing SiO2, adding the industrial byproducts into 3-4 times of water, adding 20-50% of sodium hydroxide and 10-20% of hexadecyl trimethyl ammonium bromide (CTAB) at one time, uniformly stirring at 20-40 ℃, and carrying out pre-reaction for 30 minutes. Then the temperature is raised to 60-80 ℃, and the reaction time is 48-72 hours. And after the reaction is finished, aging for 4-6 h. Finally, washing with water to remove redundant sodium hydroxide, drying at 80-110 ℃, and finally calcining at 550-600 ℃ to remove CTAB to obtain the porous white carbon black. The preparation method is simple in preparation process and low in preparation cost.
Description
Technical Field
The invention belongs to the technical field of development of novel porous white carbon black, and particularly relates to a method for preparing porous white carbon black by taking industrial silicon dioxide solid waste as a raw material.
Background
With the rapid development of the fluorosilicone industry, the discharge amount of the silicon dioxide-containing byproducts accounts for 10% -15% of the yield of the fluorosilicone material in the year along with more and more silicon dioxide-containing byproducts, so that a large amount of silicon dioxide byproducts are generated, the economic benefit of the silicon dioxide byproducts is reduced, and the silicon dioxide byproducts are often used as solid wastes and are stored in plants. More serious, the silicon dioxide by-products are often abandoned at will, which not only brings huge environmental pollution problem, but also severely restricts the capacity improvement and industry upgrade of enterprises. Although small amounts of silica by-product are often treated as building filler or industrial mineral fines, these requirements are far from digesting the increasing amount of silica by-product. Therefore, it would be of great practical significance to find a preparation method that can convert industrial silica by-products into high value products.
The white carbon black is used as an environment-friendly auxiliary agent with excellent performance and is widely applied to the fields of rubber, textile, papermaking, pesticides, food additives and the like. The preparation method mainly comprises a precipitation method and a gas phase method. The former mainly comprises sulfuric acid, hydrochloric acid and CO 2 Producing white carbon black with water glass as basic raw material or producing white carbon black by using special methods such as a supergravity technology, a sol-gel method, a chemical crystal method, a secondary crystallization method or a reversed phase micelle microemulsion method; the latter is mainly white amorphous flocculent semi-transparent solid colloidal nano-particles (the particle diameter is less than 100 nm), is nontoxic, has huge specific surface area, but has complex preparation process and high price. Compared with the traditional method for producing the white carbon black by using water glass as a basic raw material, the method has the advantages that the industrial silicon dioxide byproduct is a hard solid with low surface area and insolubility in water, and the silicon dioxide byproduct hardly reacts with various acids (except hydrofluoric acid) at normal temperature and normal pressure, so that the application of the silicon dioxide is limited.
In recent years, strong alkali is used to dissolve industrial silica byproducts to prepare white carbon black, for example, CN104512896B discloses a method for preparing white carbon black from silica-containing high-alumina fly ash, in which fly ash is ground and magnetically separated, then mixed with an alkali solution and reacted to prepare a desiliconized solution, and then the desiliconized solution is heated, carbonized, aged and spray-dried to prepare a white carbon black product. And CN103395792B also discloses a method for preparing silica from bayan obo ore or its tailings, which comprises the steps of adding alkali into bayan obo ore or its tailings, roasting, washing with water, leaching with hydrochloric acid to obtain silica raw material, and finally preparing silica by a precipitation method. However, these reported methods require complex treatment of raw materials, which greatly increases the economic cost of producing white carbon.
Disclosure of Invention
Aim at the presentThe invention provides a method for preparing porous white carbon black by taking industrial silicon dioxide solid waste as a raw material, and aims to find a method for preparing porous white carbon black by taking industrial silicon dioxide solid waste as a raw material, wherein the prepared white carbon black has a high oil absorption value (more than 2.0) and a large specific surface area (more than 160 m) 2 /g)。
The purpose of the invention can be realized by the following technical scheme:
(1) Preparing a porous white carbon black precursor: directly adding a silicon dioxide byproduct, sodium hydroxide, CTAB and water into a 10-liter reaction kettle, stirring for a certain time, and then heating to a certain temperature for reaction; then ageing, naturally cooling to room temperature, and preparing a porous white carbon black precursor after suction filtration, washing and drying;
(2) Preparing porous white carbon black: and (2) filtering, washing and drying the product obtained in the step (1), heating to a certain temperature at a certain heating rate, and calcining in an air atmosphere to prepare the porous white carbon black.
Preferably, the adding amount ratio of the silica by-product, the sodium hydroxide, the CTAB and the water in the step (1) is determined according to the capacity (5-10L) of the hydrothermal reaction kettle: 1-2 kg: 0.5-1 kg: 0.1-0.2 kg: 3-6 kg.
Preferably, the certain heating rate in the step (1) is 1-3 ℃/min; the certain temperature is 60-80 ℃, and the reaction time is 48-72 h.
Preferably, the aging time in the step (1) is 6 to 10 hours.
Preferably, the certain heating rate in the step (2) is 1-5 ℃/min; the calcining temperature is 550-600 ℃, and the calcining time is 3-6 h.
The invention has the beneficial effects that:
1. according to the invention, cetyl Trimethyl Ammonium Bromide (CTAB) is added as a pore-forming agent, and the electrostatic attraction of CTAB and silicon dioxide is beneficial to the uniform distribution of CTAB in each part of the silicon dioxide, so that the specific surface area and the oil absorption value of the white carbon black are improved.
2. According to the invention, the dissolution degree of the silica by-product and the pore diameter of the white carbon black can be regulated and controlled by the adding amount of sodium hydroxide and CTAB, so that the porous white carbon black product with wide pore diameter distribution and high oil absorption value can be prepared.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a BET diagram I of porous silica according to one embodiment of the present invention;
FIG. 2 is a BET diagram II of porous silica in the first embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
The method for preparing porous white carbon black by using industrial silicon dioxide solid waste as a raw material uses the silicon dioxide solid waste as the raw material, wherein the oil absorption value of dibutyl phthalate (DBP) of the silicon dioxide solid waste is about 1.7, the specific area is 10m & lt 2 & gt/g, and the particle size is about 1-3 micrometers. In the preparation process of the white carbon black, a silicon dioxide solid waste is directly used as a raw material, and the pretreatment is not needed.
The purity of the used Cetyl Trimethyl Ammonium Bromide (CTAB) is 99 percent, the purity of the used sodium hydroxide is 96 percent, the white carbon black preparation reaction system is a water system, the white carbon black preparation process is carried out under the conditions of normal temperature and normal pressure, the added sodium hydroxide can well dissolve silicon dioxide, the electrostatic attraction of the CTAB and the silicon dioxide is favorable for the CTAB to be uniformly distributed at each part inside and outside the silicon dioxide, the preparation of the porous white carbon black is realized, and the used sodium hydroxide and the CTAB are sequentially added into the system; the mass of the sodium hydroxide adopted by the reaction is 10-60% of that of the silicon dioxide raw material, and the adding amount can be used for regulating and controlling the dissolving degree of the silicon dioxide by-product.
The mass amount of CTAB is 20-40% of the silica raw material, the concentration range can be used for regulating and controlling the specific surface area of the white carbon black, and the larger the amount of CTAB is, the larger the specific surface area is, and the larger the oil absorption value of DBP is.
In order to ensure that the silicon dioxide has sufficient dissolving time in the sodium hydroxide solution, the silicon dioxide is firstly stirred uniformly and pre-reacted for 30 minutes, and then the reaction is carried out for 48 to 72 hours at the temperature of 70 ℃ so that the dissolved silicon dioxide and CTAB are fully mixed to achieve the purpose of preparing the porous white carbon black, the system after the reaction needs to be aged for 6 to 10 hours, the calcining method of the prepared white carbon black is one-step temperature programming, and the calcining procedure is as follows: raising the temperature to 550-600 ℃ at room temperature (3 ℃ per minute), and keeping the temperature for 3-6 hours.
The water used in the invention is 4-20 times of the raw material, the pre-reaction temperature of the reaction system is controlled at 20-40 ℃, the pre-reaction time of the reaction system is 30 minutes, the reaction temperature of the reaction system is controlled at 60-80 ℃, the reaction time of the reaction system is 48-72 hours, and the aging temperature of the reaction system is 40-50 ℃. The aging time of the reaction system is 4-6 h, and the washing method of the reaction product is to wash the reaction product for several times by water until the reaction product is neutral. The drying temperature of the reaction is 80-110 ℃, and the drying time is 10-24 h. The mass ratio of the added silicon dioxide product, sodium hydroxide, CTAB and water is based on the capacity (5-10L) of the hydrothermal reaction kettle: 1-2 kg: 0.5-1 kg: 0.1-0.2 kg: 3-6 kg; the addition amount of sodium hydroxide, CTAB and water and the dosage ratio of the silicon dioxide byproduct raw materials are respectively 20-50%, 10-20% and 300-400%, so that good effect can be achieved.
Example one
Adding 100g of silica byproduct into a reaction kettle (1L), adding 400mL of water, 50g of sodium hydroxide and 5g of CTAB, mechanically stirring and uniformly mixing, dissolving at a constant temperature of 80 ℃ for 24 hours, naturally cooling to 50 ℃, slowly aging for 4 hours, and then centrifugally washing with water for several times until the solution is neutral. The prepared sample is dried at 100 ℃, and then slowly heated to 550 ℃ to remove CTAB by calcination to obtain the porous white carbon black.
Example two
Adding 100g of silicon dioxide byproduct into a reaction kettle (1L), adding 400mL of water, 50g of sodium hydroxide and 20g of CTAB, mechanically stirring and uniformly mixing, dissolving at a constant temperature of 80 ℃ for 24h, naturally cooling to 50 ℃, slowly aging for 4 hours, and then centrifugally washing for several times by using water until the solution is neutral. The prepared sample is dried at 100 ℃, and then slowly heated to 550 ℃ to remove CTAB by calcination to obtain the porous white carbon black.
EXAMPLE III
Adding 100g of silicon dioxide byproduct into a reaction kettle (1L), adding 400mL of water, 80g of sodium hydroxide and 10g of CTAB, mechanically stirring and uniformly mixing, dissolving at a constant temperature of 80 ℃ for 24h, naturally cooling to 50 ℃, slowly aging for 4 hours, and then centrifugally washing for several times by using water until the solution is neutral. The prepared sample is dried at 100 ℃, and then slowly heated to 550 ℃ to remove CTAB by calcination to obtain the porous white carbon black.
Example four
Adding 200g of silicon dioxide byproduct into a reaction kettle (1L), adding 600mL of water, 100g of sodium hydroxide and 10g of CTAB, mechanically stirring and uniformly mixing, dissolving at a constant temperature of 80 ℃ for 24h, naturally cooling to 50 ℃, slowly aging for 4 hours, and then centrifugally washing for several times by using water until the solution is neutral. The prepared sample is dried at 100 ℃, and then slowly heated to 550 ℃ to remove CTAB by calcination to obtain the porous white carbon black.
EXAMPLE five
Adding 1000g of silicon dioxide byproduct into a reaction kettle (5L), adding 3000mL of water, 500g of sodium hydroxide and 100g of CTAB, mechanically stirring and uniformly mixing, dissolving at a constant temperature of 80 ℃ for 24 hours, naturally cooling to 50 ℃, slowly aging for 4 hours, and then centrifugally washing for several times by using water until the solution is neutral. The prepared sample is dried at 100 ℃, and then slowly heated to 550 ℃ to remove CTAB by calcination to obtain the porous white carbon black.
EXAMPLE six
Adding 2000g of silicon dioxide byproduct into a reaction kettle (10L), adding 5000mL of water, 1000g of sodium hydroxide and 200g of CTAB, mechanically stirring and uniformly mixing, dissolving at a constant temperature of 80 ℃ for 24 hours, naturally cooling to 50 ℃, slowly aging for 4 hours, and then centrifugally washing for several times by using water until the solution is neutral. The prepared sample is dried at 100 ℃, and then slowly heated to 550 ℃ to be calcined to remove CTAB, so that the porous white carbon black is obtained.
As shown in FIG. 1-2, the oil absorption value of the developed porous silica is 2.0-3.0, the specific surface area is about 160-300 m2/g, and the yield of the developed porous silica is about 50-70% calculated according to the added silica raw material.
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 shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (8)
1. A method for preparing porous white carbon black by taking industrial silicon dioxide solid waste as a raw material is characterized in that a silicon dioxide byproduct, sodium hydroxide, cetyl trimethyl ammonium bromide and water are added into a reaction kettle, and the temperature is raised after stirring for reaction; aging, cooling to room temperature, performing suction filtration, washing and drying to prepare a porous white carbon black precursor;
and filtering, washing and drying the prepared porous white carbon black precursor, heating, and calcining in the air atmosphere to prepare the porous white carbon black.
2. The method for preparing porous silica according to claim 1, wherein the silica byproduct contains 90% silica, has an oil absorption value for dibutyl phthalate of 1.7, and has a specific area of 10m 2 The grain diameter is 1-3 microns.
3. The method for preparing porous silica white according to claim 2, wherein the mass ratio of the sodium hydroxide, the cetyl trimethyl ammonium bromide and the water to the raw material of the silica byproduct is 20-50%, 10-20% and 300-400%, respectively.
4. The preparation method of porous white carbon black according to claim 3, wherein the reaction is carried out at 20-40 ℃, the mixture is uniformly stirred, the pre-reaction is carried out for 30 minutes, the temperature is 60-80 ℃, and the reaction time is 48-72 hours.
5. The method for preparing porous white carbon black according to claim 4, wherein the system is aged at 40-50 ℃ for 4-6 hours after the reaction is finished.
6. The method for preparing porous silica white according to claim 5, wherein after the reaction, the solid is centrifugally separated, washed with clean water, repeatedly washed with clean water for 4-8 times, and then dried at 80-110 ℃ for 10-24 hours.
7. The method for preparing porous silica white according to claim 6, wherein air is continuously introduced into the furnace during the calcination process, and the temperature is raised to 550-600 ℃ for 3-6 hours at a time.
8. Porous silica obtained by the method according to any one of claims 1 to 7.
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CN113912071A (en) * | 2021-09-17 | 2022-01-11 | 龙岩市荣雁新材料科技有限公司 | Preparation method of modified nano white carbon black |
CN113943006A (en) * | 2021-12-07 | 2022-01-18 | 安徽进化硅纳米材料科技有限公司 | High-reinforcement white carbon black and preparation method and application thereof |
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- 2022-08-15 CN CN202210973555.9A patent/CN115159532A/en active Pending
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KR20090048082A (en) * | 2007-11-09 | 2009-05-13 | 학교법인 함주학원 | A production method of porous silica |
CN103130228A (en) * | 2011-11-28 | 2013-06-05 | 陈昆先 | Preparation method of high dispersion white carbon black from bentonite by making use of non-metallic mine dissociation method |
CN103360798A (en) * | 2013-07-19 | 2013-10-23 | 合肥工业大学 | Method for preparing hydrophobic white carbon black |
WO2015101361A1 (en) * | 2014-01-06 | 2015-07-09 | 中盈长江国际新能源投资有限公司 | Method of producing nanoscale white carbon black by using furnace flue gas directly to carbonize water glass |
CN104402006A (en) * | 2014-11-05 | 2015-03-11 | 昆明理工大学 | Method for preparing meso-porous silica material by using silicon micro-powder |
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