[go: up one dir, main page]

CN119263341A - A method for preparing potassium titanate powder - Google Patents

A method for preparing potassium titanate powder Download PDF

Info

Publication number
CN119263341A
CN119263341A CN202411810511.XA CN202411810511A CN119263341A CN 119263341 A CN119263341 A CN 119263341A CN 202411810511 A CN202411810511 A CN 202411810511A CN 119263341 A CN119263341 A CN 119263341A
Authority
CN
China
Prior art keywords
potassium titanate
potassium
titanium
titanate powder
precursor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202411810511.XA
Other languages
Chinese (zh)
Other versions
CN119263341B (en
Inventor
韩晖
赵一昕
李若尘
曹宇
王晓东
王积涛
葛信信
胡玮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Kaisheng Applied Materials Co ltd
Original Assignee
Anhui Kaisheng Applied Materials Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Kaisheng Applied Materials Co ltd filed Critical Anhui Kaisheng Applied Materials Co ltd
Priority to CN202411810511.XA priority Critical patent/CN119263341B/en
Publication of CN119263341A publication Critical patent/CN119263341A/en
Application granted granted Critical
Publication of CN119263341B publication Critical patent/CN119263341B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/003Titanates
    • C01G23/005Alkali titanates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

本发明公开一种钛酸钾粉体的制备方法,属于无机材料技术领域,以钛的氧化物或氢氧化物、钾的化合物为反应原料,将可溶性钾源完全溶解后,加入到钛前驱体中,再采用无损喷雾造粒的方式将钾源重结晶在钛前驱体表面,得到钛、钾组分均匀的钛酸钾前驱体微粒,并能按要求调整钛酸钾前驱体微粒的大小;再通过控制不同的煅烧温度、保温时间以及研磨粉碎的冲击力和剪切力,制备得到不同微观形貌、结晶度高的钛酸钾粉体;制备过程中加入分散剂用于提高钛源的分散程度,加入插层剂和表面活性剂用以调整钛酸钾粉体的微观形貌。

The invention discloses a preparation method of potassium titanate powder, belonging to the technical field of inorganic materials. Titanium oxide or hydroxide and potassium compound are used as reaction raw materials, a soluble potassium source is completely dissolved and then added into a titanium precursor, and then the potassium source is recrystallized on the surface of the titanium precursor by a non-destructive spray granulation method to obtain potassium titanate precursor particles with uniform titanium and potassium components, and the size of the potassium titanate precursor particles can be adjusted as required; and potassium titanate powders with different microscopic morphologies and high crystallinity are prepared by controlling different calcination temperatures, heat preservation times, and impact forces and shear forces of grinding and crushing; and a dispersant is added in the preparation process to improve the dispersion degree of the titanium source, and an intercalation agent and a surfactant are added to adjust the microscopic morphology of the potassium titanate powder.

Description

Preparation method of potassium titanate powder
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly discloses a preparation method of potassium titanate powder.
Background
The potassium titanate is widely used for high molecular polymers, metals, ceramics and the like, and can greatly improve the high temperature resistance, the wear resistance, the weather resistance, the mechanical properties and the like of the related composite materials. Potassium titanate is generally represented by K 2O•nTiO2 (n=1, 2,4,6, 8), where the practical value of n=4 or 6 (i.e., potassium tetratitanate and potassium hexatitanate) is greatest.
The chemical formula of the potassium hexatitanate is K 2Ti6O13, the potassium hexatitanate is an inorganic compound, the appearance is gray yellow powder, the potassium hexatitanate has the characteristics of stable chemical property, excellent mechanical property, corrosion resistance, heat insulation, wear resistance, low high-temperature hardness and the like, and the potassium hexatitanate has been widely applied to the fields of petrochemical industry, automobiles, electronic appliances, buildings, machinery, environmental protection catalysis, sewage treatment, energy conversion, aerospace and the like.
According to different morphologies, the potassium hexatitanate is divided into whisker-shaped potassium hexatitanate, tunnel-shaped potassium hexatitanate, platelet-shaped potassium hexatitanate and the like, and the potassium hexatitanate with different morphologies has certain differences in performance, characteristics, application and the like, such as the columnar potassium hexatitanate has the characteristics of large specific surface area, regular shape and the like, the flaky potassium hexatitanate is more excellent in strength and modulus, and the whisker-shaped potassium hexatitanate has the characteristics of good lubricity, extremely high infrared reflection, diffuse reflectance and the like. The whisker-shaped potassium hexatitanate, namely potassium hexatitanate whisker, is a novel needle-shaped short fiber compound, and the atomic structure arrangement is highly ordered when the whisker is crystallized, so that the whisker strength is extremely high and far exceeds various reinforcing agents.
The existing potassium titanate preparation method is beneficial to a cosolvent method, a hydrothermal method, a melting method, a microwave synthesis method, a sol-gel method, a sintering method and the like, but has the common limitations that, for example, the melting method is used for melting and cooling raw materials to cultivate crystals, the yield is low, the reaction temperature is high, the hydrothermal method is used for reacting the raw materials in hot water under high pressure to generate crystals, longer fibers can be prepared, however, the method needs to use high temperature and high pressure, the production cost is high and the danger is high, the cosolvent method is a method for reacting the raw materials in a solvent (the currently adopted solvent is KCl, KF, KMnO 4、K2WO4 and the like), the yield is high, the prepared potassium titanate monocrystal fibers are good in crystallinity, but the use of the cosolvent can erode a sagger when the materials are sintered at high temperature, the sagger cannot be reused, the production cost is increased, the existence of fluorine ions can cause environmental pollution, the existence of manganese and tungsten can influence the product quality, and the sintering method is used for sintering the raw material mixture at a certain time and a certain temperature, so that the method has the disadvantages of high synthetic product purity and various potassium titanate can appear if the appearance and the product purity are not high.
The patent with publication number CN113403686B discloses a preparation method of potassium titanate whisker for friction materials, which takes titanium dioxide and a potassium source as raw materials, takes a K 2O-MoO3 composite cosolvent as a cosolvent, and prepares the potassium titanate whisker for friction materials by a flux method. The method has complex production process, the potassium hexatitanate can be prepared by firstly preparing the titanium source and the potassium source into the potassium tetratitanate and then washing and secondary sintering, the cosolvent can seriously corrode the sagger at high temperature, the product quality is affected, and a large amount of alkaline wastewater is generated in the production.
The patent with publication number CN102304762A discloses a preparation method of potassium hexatitanate whisker, which comprises the steps of mixing potassium carbonate and metatitanic acid at room temperature, drying, calcining a precursor, and carrying out water leaching treatment to prepare the potassium hexatitanate whisker. The method is easy to generate a large amount of byproducts in the preparation process, and needs to be removed by water washing, so that raw materials are wasted, and a large amount of high-salt wastewater which is difficult to treat is increased.
The patent with publication number CN115747967B discloses a preparation method of potassium hexatitanate whisker, which comprises the steps of mixing titanium-containing raw materials and potassium-containing raw materials, sintering the mixed materials at the temperature of 600-800 ℃, dispersing the mixed materials in water after cooling along with a furnace, introducing acid gas, adjusting the pH value, carrying out suction filtration, drying, and sintering and cooling the dried product at the temperature of 1000-1250 ℃ to obtain the coarse potassium hexatitanate whisker with the diameter of more than 3 mu m. The production method is insufficient in reaction, excessive titanium sources are required to be put into, and finally, the titanium sources are lost and wasted, and the production process is required to be calcined for many times and acid gas is introduced, so that the industrial production is not facilitated.
Disclosure of Invention
The invention aims to solve the problem that the existing potassium titanate preparation method is generally limited, and provides a preparation method of potassium titanate powder, which is used for preparing a potassium titanate product with whisker-like, tunnel-like and platelet-like microstructures and high crystallinity by regulating and controlling the processes of raw material proportioning, pretreatment, mixing, surface treatment, calcination and the like, and can be used as a friction material, a reinforcing material and a heat insulation material in the new material high-tech field.
In order to solve the technical problems, the invention provides a preparation method of potassium titanate powder, which comprises the following steps:
(1) Adding a dispersing agent into the titanium source slurry with the concentration of 20-40%, mixing, grinding and sieving to obtain a titanium precursor;
(2) Preparing a potassium source saturated solution, adding 1 into a titanium precursor according to the molar ratio of titanium to potassium of (2.5-3.5), and uniformly mixing to obtain potassium titanate precursor slurry;
(3) Adding a surfactant into the potassium titanate precursor slurry, and performing spray granulation to obtain potassium titanate precursor particles with the particle size of 10-50 mu m;
(4) Adding an intercalation agent into the potassium titanate precursor particles, uniformly mixing, calcining for synthesis, and grinding and crushing to obtain the potassium titanate powder.
As a further description of the invention, the titanium source in the step (1) is one or more of rutile titanium dioxide, anatase titanium dioxide, orthotitanic acid and metatitanic acid, the dispersing agent is one or more of sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, sodium dodecyl sulfate, polyvinylpyrrolidone and cellulose derivatives, the adding amount of the dispersing agent is 0.1-0.5% of the dry weight of the titanium source, the grinding is wet ball milling, and the sieving is 325-mesh sieving.
As a further description of the present invention, the potassium source in step (2) is one or more of potassium carbonate, potassium bicarbonate, and potassium hydroxide.
As a further description of the invention, the surfactant in the step (3) is one or more of titanate, aluminate, stearic acid, oleic acid and polysorbate, the addition of the surfactant is 1-5% of the dry weight of the titanium source, the spray granulation equipment is preferably a centrifugal spray granulator, and the spray temperature is less than or equal to 300 ℃.
As a further description of the invention, the intercalation agent in the step (4) is one or more of potassium acetate, dimethyl sulfoxide, urea, graphite and isopropylamine, the addition amount of the intercalation agent is 3-8% of the dry weight of a titanium source, the calcining equipment is preferably a muffle furnace, a roller kiln, a tunnel kiln or a push plate furnace, the calcining carrier is preferably alumina, zirconia or a ceramic sagger with the surface sprayed with alumina and zirconia, the calcining temperature rising rate is 3-8 ℃ per minute, the calcining temperature is 900-1200 ℃ and is controlled within a set temperature +/-5 ℃, the heat preservation time is 2-6 hours, and the grinding and crushing equipment is preferably a Raymond mill, an air flow mill or a powder mill so as to ensure that the microscopic morphology of the potassium titanate powder is not damaged.
The preparation method of the potassium titanate powder takes oxides or hydroxides of titanium and potassium compounds as reaction raw materials, after the soluble potassium source is completely dissolved, the soluble potassium source is added into a titanium precursor, then the potassium source is recrystallized on the surface of the titanium precursor in a nondestructive spray granulation mode to obtain potassium titanate precursor particles with uniform titanium and potassium components, the size of the potassium titanate precursor particles can be regulated as required, and then the potassium titanate powder with different microcosmic morphologies and high crystallinity is prepared by controlling different calcination temperatures, heat preservation time and impact force and shearing force of grinding and crushing, wherein a dispersing agent is added in the preparation process to improve the dispersion degree of the titanium source, and an intercalating agent and a surfactant are added to regulate the microcosmic morphology of the potassium titanate powder.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the preparation method, a potassium source recrystallization process is utilized, a titanium source is uniformly dispersed in a dispersing agent, then the potassium source is recrystallized on the surface of the titanium source, so that a uniformly mixed potassium titanate precursor with a high uniform titanium-potassium molar ratio is obtained, and the crystallinity of potassium titanate powder after calcination and dispersion is improved;
2. By adding the intercalation agent, potassium titanate powder with different microcosmic morphologies is prepared, so that the application of the potassium titanate in the field of new materials is greatly widened, and the potassium titanate powder serving as a friction material is particularly suitable for manufacturing automobile brake pads and serving as a heat insulation material is particularly suitable for various heat insulation and preservation;
3. The size of the potassium titanate precursor particles can be controlled by adjusting the parameters of the spray granulator, so that the microcosmic appearance of the potassium titanate powder after calcination and crushing is regulated and controlled, and the applicability of the product is improved;
4. The preparation method does not need adding KCl, KF, KMnO 4、K2WO4 or other cosolvent, does not need washing to remove cosolvent after the preparation is finished, and is clean and friendly in preparation process.
Drawings
FIG. 1 is an SEM image of whisker-like potassium titanate powder obtained in example 1;
FIG. 2 is an XRD characterization diagram of whisker-like potassium titanate powder obtained in example 1;
FIG. 3 is an SEM image of tunnel-like potassium titanate powder obtained in example 2;
FIG. 4 is an XRD characterization of the tunnel-like potassium titanate powder obtained in example 2;
FIG. 5 is an SEM image of a platelet-shaped potassium titanate powder obtained in example 3;
FIG. 6 is an XRD characterization pattern of the platelet-shaped potassium titanate powder obtained in example 3;
FIG. 7 is an SEM image of the potassium titanate powder obtained in the comparative example;
fig. 8 is an XRD characterization of the potassium titanate powder obtained in the comparative example.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. Any person skilled in the art can make possible variations and modifications of the technical solution of the present invention or modifications to equivalent embodiments of the equivalent variations, using the methods and technical contents of the present invention, without departing from the scope of the technical solution of the present invention. Therefore, any simple modification, equivalent replacement, equivalent variation and modification made according to the technical content of the present invention without departing from the technical content of the present invention shall fall within the scope of the technical protection of the present invention.
Example 1:
the embodiment provides a preparation method of potassium titanate powder, which comprises the following steps:
(1) Adding sodium dodecyl sulfate with the weight of 0.1% of the dry weight of titanium dioxide into anatase titanium dioxide slurry with the concentration of 20%, mixing, ball milling, and sieving with a 325-mesh sieve to obtain a titanium precursor;
(2) Preparing a potassium carbonate saturated solution, adding the solution into a titanium precursor according to the molar ratio of titanium to potassium of 3:1, and uniformly mixing to obtain potassium titanate precursor slurry;
(3) Adding 1% of titanate into the potassium titanate precursor slurry, feeding the slurry into a centrifugal spray granulator, setting the spraying temperature to 250 ℃ and adjusting the parameters of the spray granulator to carry out spray granulation to obtain dry potassium titanate precursor particles with the particle size of 10 mu m;
(4) Adding graphite accounting for 3% of the dry weight of titanium dioxide into potassium titanate precursor particles, sending the mixture into a ball mill for uniform mixing, then sending the mixture into a ceramic sagger made of aluminum oxide, sending the ceramic sagger into a tunnel kiln, adjusting the heating rate of the tunnel kiln to 3 ℃ per minute, heating to 1000+/-5 ℃ and preserving heat to 2h for calcination synthesis, grinding and crushing the mixture by using a Raymond mill after sintering, and obtaining potassium titanate powder after grinding and crushing.
As can be seen from FIG. 1, the potassium titanate prepared in the embodiment is whisker-shaped potassium titanate, has obvious whisker structure and moderate length-diameter ratio, is uniformly dispersed, has no obvious clusters, and can be widely used for reinforcing materials and friction materials. As can be seen from fig. 2, the potassium titanate prepared in this example is potassium hexatitanate.
Example 2:
the embodiment provides a preparation method of potassium titanate powder, which comprises the following steps:
(1) Adding sodium hexametaphosphate accounting for 0.3 percent of the weight of the dry basis of the meta-titanic acid into the meta-titanic acid slurry with the concentration of 30 percent, mixing, ball milling and sieving with a 325-mesh sieve to obtain a titanium precursor;
(2) Preparing a potassium bicarbonate saturated solution, adding the solution into a titanium precursor according to the molar ratio of titanium to potassium of 3:1, and uniformly mixing to obtain potassium titanate precursor slurry;
(3) Adding 2.5% oleic acid into potassium titanate precursor slurry, feeding into a centrifugal spray granulator, setting the spray temperature to 220 ℃ and adjusting the parameters of the spray granulator to carry out spray granulation to obtain dry potassium titanate precursor particles with the particle size of 20 mu m;
(4) Adding urea accounting for 5% of the dry weight of the metatitanic acid into potassium titanate precursor particles, sending the mixture into a ball mill, uniformly mixing the mixture, then sending the mixture into a ceramic sagger made of zirconia material, sending the mixture into a roller kiln, adjusting the temperature rise rate of the roller kiln to be 5 ℃ per min, heating the mixture to 1100+/-5 ℃ and preserving heat to 4 h ℃ for calcination synthesis, grinding and crushing the mixture by using an air flow mill after sintering, and obtaining tunnel-shaped potassium titanate powder after grinding and crushing.
As can be seen from fig. 3, the potassium titanate prepared in this example is tunnel-like potassium titanate, has an obvious columnar structure, and as can be seen from fig. 4, the potassium titanate prepared in this example is potassium hexatitanate.
Example 3:
the embodiment provides a preparation method of potassium titanate powder, which comprises the following steps:
(1) Adding sodium tripolyphosphate with the weight of 0.5% of the dry weight of the orthotitanic acid into the orthotitanic acid slurry with the concentration of 40%, mixing, ball milling, and sieving with a 325-mesh sieve to obtain a titanium precursor;
(2) Preparing a potassium carbonate saturated solution, adding the solution into a titanium precursor according to the molar ratio of titanium to potassium of 3.5:1, and uniformly mixing to obtain potassium titanate precursor slurry;
(3) Adding 5% polysorbate into potassium titanate precursor slurry, feeding into a centrifugal spray granulator, setting the spray temperature to 230 ℃ and adjusting the parameters of the spray granulator to carry out spray granulation to obtain dry potassium titanate precursor particles with the particle size of 50 mu m;
(4) Adding isopropyl amine accounting for 8% of the dry weight of normal titanic acid into potassium titanate precursor particles, sending the mixture into a ball mill, uniformly mixing the mixture, then sending the mixture into a ceramic sagger with zirconia sprayed on the surface, sending the ceramic sagger into a pushed slab kiln, adjusting the temperature rising rate of the pushed slab kiln to be 8 ℃ per min, rising the temperature to 1200+/-5 ℃ and preserving the temperature to 4h for calcination synthesis, grinding and crushing the mixture by an air flow mill after sintering, and obtaining the sheet crystalline potassium titanate powder after grinding and crushing.
As can be seen from fig. 1, the potassium titanate prepared in this embodiment is in a flake structure, is platelet-shaped potassium titanate, has uniform particle size and good dispersibility, and the potassium titanate in the flake structure can better prevent or slow down the transmission of energy into the brake pad in the braking process, absorb noise generated in the braking process, and is particularly suitable for manufacturing novel environment-friendly automobile brake pads. As can be seen from FIG. 6, the potassium titanate prepared by the method is potassium hexatitanate, and has good crystallinity.
The invention has the innovation point that the potassium source and the titanium source which participate in the synthesis reaction can be fully mixed, the dispersing agent is added in the preparation process to improve the dispersing degree of the titanium source, the intercalating agent and the surfactant are added to adjust the micro morphology of the potassium titanate powder, and simultaneously the potassium titanate powder with different particle size distribution is prepared by adjusting the size of the precursor particles of the potassium titanate reaction.
Comparative example:
(1) Preparing orthotitanic acid slurry with the concentration of 40%, uniformly dispersing, and sieving with a 325-mesh sieve to obtain a titanium precursor;
(2) Preparing a potassium hydroxide saturated solution, adding the solution into a titanium precursor according to the molar ratio of titanium to potassium of 3:1, and uniformly mixing to obtain potassium titanate precursor slurry;
(3) Drying the potassium titanate precursor slurry in an oven, grinding the blocky material after drying, and sieving the blocky material with a 200-mesh sieve;
(4) And loading the potassium titanate precursor powder into a ceramic sagger with zirconia sprayed on the surface, feeding the ceramic sagger into a roller kiln for calcination, adjusting the temperature rising rate of the roller kiln to be 5 ℃ per min, rising to 1000+/-5 ℃ and preserving heat for 4 hours for calcination synthesis, and grinding and crushing by using an air flow mill after sintering to obtain the potassium titanate powder.
As can be seen from FIG. 7, the potassium titanate powder prepared in the comparative example has irregular particle shape, quite uneven size, quite obvious aggregation phenomenon of particles with different shapes, and quite high difficulty in further dispersion. As can be seen from FIG. 8, the potassium titanate prepared by this comparison is inferior in crystallinity and has many unreacted impurity residues.
The foregoing is only the best mode of carrying out the invention. It should be noted that, for those skilled in the art, several modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the principles of the present invention, and the technical effects of the present invention can be achieved, and the present invention shall also be considered as falling within the protection scope of the present invention.

Claims (9)

1.一种钛酸钾粉体的制备方法,其特征在于,包括以下步骤:1. A method for preparing potassium titanate powder, characterized in that it comprises the following steps: (1)向浓度为20~40%的钛源浆料中加入分散剂,混合研磨后过筛,得到钛前驱体;(1) adding a dispersant to a titanium source slurry having a concentration of 20-40%, mixing, grinding, and sieving to obtain a titanium precursor; (2)配制钾源饱和溶液,并按钛:钾的摩尔比为(2.5~3.5):1加入到钛前驱体中,混合均匀,得到钛酸钾前驱体浆料;(2) preparing a saturated potassium source solution, and adding it to the titanium precursor at a molar ratio of titanium to potassium of (2.5-3.5):1, and mixing them evenly to obtain a potassium titanate precursor slurry; (3)在钛酸钾前驱体浆料中加入表面活性剂,喷雾造粒,获得粒径为10~50μm的钛酸钾前驱体微粒;(3) adding a surfactant to the potassium titanate precursor slurry and spray granulating the slurry to obtain potassium titanate precursor particles with a particle size of 10 to 50 μm; (4)在钛酸钾前驱体微粒中加入插层剂,混合均匀后煅烧合成,研磨粉碎后获得具有晶须状、隧道状或片晶状微观形貌的钛酸钾粉体。(4) adding an intercalating agent to potassium titanate precursor particles, mixing them evenly and then calcining them for synthesis, and grinding and crushing them to obtain potassium titanate powder having a whisker-like, tunnel-like or lamellar-like microstructure. 2.如权利要求1所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(1)所述的钛源为金红石型二氧化钛、锐钛型二氧化钛、正钛酸、偏钛酸中的一种或多种;所述的分散剂为六偏磷酸钠、三聚磷酸钠、焦磷酸钠、十二烷基硫酸钠、聚乙烯吡咯烷酮、纤维素衍生物中的一种或多种;分散剂的添加量为钛源干基重量0.1~0.5%。2. The method for preparing potassium titanate powder according to claim 1, characterized in that: the titanium source in step (1) is one or more of rutile titanium dioxide, anatase titanium dioxide, orthotitanic acid, and metatitanic acid; the dispersant is one or more of sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, sodium dodecyl sulfate, polyvinyl pyrrolidone, and cellulose derivatives; and the amount of the dispersant added is 0.1-0.5% of the dry weight of the titanium source. 3.如权利要求1所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(2)所述的钾源为碳酸钾、碳酸氢钾、氢氧化钾中的一种或多种。3. The method for preparing potassium titanate powder according to claim 1, characterized in that: the potassium source in step (2) is one or more of potassium carbonate, potassium bicarbonate, and potassium hydroxide. 4.如权利要求1所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(3)所述的表面活性剂为钛酸酯、铝酸酯、硬脂酸、油酸、聚山梨酯中的一种或多种,表面活性剂的加入量为钛源干基重量的1~5%。4. The method for preparing potassium titanate powder according to claim 1, characterized in that: the surfactant described in step (3) is one or more of titanate, aluminate, stearic acid, oleic acid, polysorbate, and the amount of the surfactant added is 1-5% of the dry weight of the titanium source. 5.如权利要求1所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(4)所述的插层剂为醋酸钾、二甲基亚砜、尿素、石墨、异丙胺中的一种或多种,插层剂的加入量为钛源干基重量的3~8%。5. The method for preparing potassium titanate powder according to claim 1, characterized in that: the intercalating agent in step (4) is one or more of potassium acetate, dimethyl sulfoxide, urea, graphite, and isopropylamine, and the amount of the intercalating agent added is 3-8% of the dry weight of the titanium source. 6.如权利要求1或2所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(1)所述的研磨为湿法球磨,所述的过筛为过325目筛。6. The method for preparing potassium titanate powder according to claim 1 or 2, characterized in that: the grinding in step (1) is wet ball milling, and the screening is through a 325 mesh sieve. 7.如权利要求1或4所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(3)中喷雾造粒的喷雾温度≤300 ℃。7. The method for preparing potassium titanate powder according to claim 1 or 4, characterized in that the spray temperature of the spray granulation in step (3) is ≤300°C. 8.如权利要求1或5所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(4)中煅烧的升温速率为3~8 ℃/min,煅烧温度为900~1200 ℃,保温时间为2~6 h。8. The method for preparing potassium titanate powder according to claim 1 or 5, characterized in that: the heating rate of calcination in step (4) is 3-8 °C/min, the calcination temperature is 900-1200 °C, and the holding time is 2-6 h. 9.如权利要求8所述的一种钛酸钾粉体的制备方法,其特征在于:步骤(4)中煅烧的载具为氧化铝、氧化锆材质或表面喷涂氧化铝、氧化锆的陶瓷匣钵。9. The method for preparing potassium titanate powder according to claim 8, characterized in that the carrier for calcination in step (4) is made of alumina, zirconia or a ceramic sagger with alumina or zirconia sprayed on the surface.
CN202411810511.XA 2024-12-10 2024-12-10 A method for preparing potassium titanate powder Active CN119263341B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202411810511.XA CN119263341B (en) 2024-12-10 2024-12-10 A method for preparing potassium titanate powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202411810511.XA CN119263341B (en) 2024-12-10 2024-12-10 A method for preparing potassium titanate powder

Publications (2)

Publication Number Publication Date
CN119263341A true CN119263341A (en) 2025-01-07
CN119263341B CN119263341B (en) 2025-03-07

Family

ID=94109598

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202411810511.XA Active CN119263341B (en) 2024-12-10 2024-12-10 A method for preparing potassium titanate powder

Country Status (1)

Country Link
CN (1) CN119263341B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6677041B1 (en) * 1999-03-16 2004-01-13 Otsuka Chemical Co., Ltd. Platy potassium titanate, process for producing the same, and friction material
JP2012030989A (en) * 2010-07-28 2012-02-16 Hitachi Chem Co Ltd Titanium dioxide, method of manufacturing the same, electrode for lithium ion battery using the same, and lithium ion battery
KR101727503B1 (en) * 2016-01-07 2017-04-19 주식회사 비앤비 Method of manufacturing 6 potassium titanate using hydrated porous potassium sources
CN108166051A (en) * 2018-03-08 2018-06-15 合肥工业大学 A kind of morphology controllable potassium hexatitanate powder crystal material and its low energy consumption preparation method
US20190248671A1 (en) * 2017-05-30 2019-08-15 Lg Chem, Ltd. Method for producing potassium titanate
CN117285068A (en) * 2022-12-30 2023-12-26 常州泰特耐特新材料科技有限公司 Preparation method of carbon intercalation modified potassium magnesium titanate and friction material
CN117466330A (en) * 2023-09-19 2024-01-30 安徽凯盛应用材料有限公司 A kind of tetragonal phase nanometer barium titanate and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6677041B1 (en) * 1999-03-16 2004-01-13 Otsuka Chemical Co., Ltd. Platy potassium titanate, process for producing the same, and friction material
JP2012030989A (en) * 2010-07-28 2012-02-16 Hitachi Chem Co Ltd Titanium dioxide, method of manufacturing the same, electrode for lithium ion battery using the same, and lithium ion battery
KR101727503B1 (en) * 2016-01-07 2017-04-19 주식회사 비앤비 Method of manufacturing 6 potassium titanate using hydrated porous potassium sources
US20190248671A1 (en) * 2017-05-30 2019-08-15 Lg Chem, Ltd. Method for producing potassium titanate
CN108166051A (en) * 2018-03-08 2018-06-15 合肥工业大学 A kind of morphology controllable potassium hexatitanate powder crystal material and its low energy consumption preparation method
CN117285068A (en) * 2022-12-30 2023-12-26 常州泰特耐特新材料科技有限公司 Preparation method of carbon intercalation modified potassium magnesium titanate and friction material
CN117466330A (en) * 2023-09-19 2024-01-30 安徽凯盛应用材料有限公司 A kind of tetragonal phase nanometer barium titanate and preparation method thereof

Also Published As

Publication number Publication date
CN119263341B (en) 2025-03-07

Similar Documents

Publication Publication Date Title
Xia et al. Novel route to nanoparticle synthesis by salt‐assisted aerosol decomposition
CN109440051A (en) A kind of alumina ceramic coating and preparation method thereof
CN101148779B (en) Preparation method for potassium titanate crystal whisker
WO2009087997A1 (en) Process for production of aluminum titanate-based ceramics
CN109081684A (en) A kind of preparation method of carbon nanotube enhancing alumina matrix composite
CN115974111B (en) A controllable preparation method of flaky aluminum oxide
CN108640677A (en) A kind of nano composite oxides zirconium powder preparation that crystallite dimension is controllable
CN102328941A (en) Method for preparing nano alumina
CN109336143B (en) Method for preparing nano magnesium oxide by one-step pyrolysis method
CN101311372A (en) Low-temperature molten salt thermal inversion preparation method of aporate-crystal antifungin whiskers
CN106801256A (en) A kind of method that solid phase method prepares potassium hexatitanate platelet
Singh et al. Ceramic matrix composites: processing techniques and recent advancements
CN119263341B (en) A method for preparing potassium titanate powder
Chu et al. Synthesis and characterization of novel coral spherical bismuth oxide
CN114436314A (en) Preparation method of nano yttrium oxide, nano yttrium oxide and yttrium oxide micron hollow sphere
CN104788094B (en) A kind of preparation method of bismuth titanate ceramics material
CN114477969A (en) Preparation method of high-purity superfine alumina for ceramic tube
CN117534460B (en) Perovskite type ceramic material with high infrared emissivity and preparation method and application thereof
CN118723993A (en) Method for preparing plate-like crystal tungsten carbide powder and plate-like crystal tungsten carbide powder
CN112588282A (en) Method for preparing binary composite catalytic cracking molecular sieve precursor from coal gangue
CN114656246B (en) Regular octahedral alpha alumina and preparation method and application thereof
Kong et al. Mullite whiskers derived from an oxide mixture activated by a mechanochemical process
CN100577571C (en) A kind of preparation method of aluminum oxide nanopowder
CN109485387A (en) A kind of preparation method of Environmental Barrier Coatings on Si-based Ceramics hollow ball shape BSAS powder
CN112479251A (en) Preparation method of large-particle-size non-fibrous potassium hexatitanate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant