CN110078119A - A kind of air cleaning nano-titanium dioxide preparation method - Google Patents
A kind of air cleaning nano-titanium dioxide preparation method Download PDFInfo
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- CN110078119A CN110078119A CN201910228728.2A CN201910228728A CN110078119A CN 110078119 A CN110078119 A CN 110078119A CN 201910228728 A CN201910228728 A CN 201910228728A CN 110078119 A CN110078119 A CN 110078119A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- 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
- C01P2006/80—Compositional purity
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Abstract
A kind of air cleaning nano-titanium dioxide preparation method, comprising the following steps: choose titanium iron ore, and titanium iron ore is processed into powdered;Concentrated hydrochloric acid is added into powdered titanium iron ore and carries out acidolysis;It is stood after the molten mine of acidolysis, refilters removal slag, obtain once filtering titanium liquid A;Titanium liquid A is cooled to room temperature, and Iron dichloride tetrahydrate is precipitated in crystallization in titanium liquid A, and secondary filter titanium liquid B is obtained by filtration;Oxidant is added into secondary filter titanium liquid B, obtains solution D;Cerous nitrate is added into solution D, and sodium hydroxide is added and adjusts PH as alkalinity, is sufficiently mixed;Activated carbon fibre is being added, and is being impregnated under ultrasound condition, is obtaining mixed liquor D;Mixed liquor D is dried, then is milled into powder after being calcined, obtains the nano titanium dioxide powder for mixing cerium.In the present invention, the partial size of nano-titanium dioxide is small, good dispersion, improves the quantum effect of nano-titanium dioxide, to improve air purification effect;Reaction process is environment friendly and pollution-free.
Description
Technical field
The present invention relates to field more particularly to a kind of air cleaning nano-titanium dioxide preparation methods.
Background technique
Titanium dioxide has stable physical property, chemical property and excellent optics, electrical properties and excellent face
Expect that performance, purposes are very extensive.Coating, plastics, rubber, chemical fibre, papermaking, ink, cosmetics, toy, capacitor, kinescope,
National defence sophisticated technology, food, medicine, chemical reagent, welding rod, enamel, ceramics, glass, refractory material, metallurgy, synthetic cut stone,
Art painting, leather, printing and dyeing mill base, soap, catalyst etc. will use titanium dioxide.
The manufacture of titanium dioxide mainly has chloridising and sulfuric acid process at present.Chloridising is technologically advanced, and process is short, it is easy to accomplish
Automation, good product quality.But ingredient requirement high-grade is high, using rutile ore, belongs to scarce resource;Technical difficulty is big, it is desirable that
The material and facility of resistance to titanium tetrachloride, chlorine, oxygen under high temperature, investment cost are high, maintenance difficult, advantage oneself do not exist.Sulfuric acid process
Raw material is cheap, and technical maturity, equipment is simple, but process flow is long, and energy consumption is high, and three waste discharge is more, poor product quality.
Summary of the invention
(1) goal of the invention
To solve technical problem present in background technique, the present invention proposes a kind of air cleaning nano-titanium dioxide preparation side
The partial size of method, obtained nano-titanium dioxide is small, and particle size distribution range is small, good dispersion, improves the quantum of nano-titanium dioxide
Effect, to improve air purification effect;Reaction process is environment friendly and pollution-free.
(2) technical solution
To solve the above problems, the present invention provides a kind of air cleaning nano-titanium dioxide preparation methods, comprising the following steps:
S1, titanium iron ore is chosen, and titanium iron ore is processed into powdered;
S2, concentrated hydrochloric acid progress acidolysis is added into powdered titanium iron ore, the mine acid of molten mine compares for 4-6, acidolysis temperature 50-
100 degrees Celsius;1-2 hours are stood after the molten mine of acidolysis, refilters removal slag, obtains once filtering titanium liquid A;
S3, titanium liquid A are cooled to room temperature, and Iron dichloride tetrahydrate is precipitated in crystallization in titanium liquid A, and four chloride hydrates in titanium liquid A are sub-
Iron is filtered removal, obtains secondary filter titanium liquid B;
S4, oxidant is added into secondary filter titanium liquid B, converts iron chloride for remaining frerrous chloride, obtains solution D;
S5, cerous nitrate is added into solution D, and be added sodium hydroxide adjust PH for alkalinity after, be sufficiently mixed to obtain suspension C;
S5, activated carbon fibre is added into suspension C, and is impregnated 0.5-1 hours under ultrasound condition, obtain mixed liquor D;
S6, mixed liquor D is evaporated and is dried, obtain mixture E;
S7, mixture is heated 2-4 hours under 200-250 degrees Celsius of temperature environment, then is calcined, obtain block F;
S8, block F is milled into powder, obtains the nano titanium dioxide powder for mixing cerium.
Preferably, in S2, the concentration of concentrated hydrochloric acid is 30-38%.
Preferably, in S4, oxidant is hydrogen peroxide.
Preferably, in the filter process of S2 and S4, distilled water flushing is used to filter cake, flushing liquor is back in filtrate.
Preferably, in S7, calcination temperature is 700-800 degrees Celsius.
Above-mentioned technical proposal of the invention has following beneficial technical effect:
In the present invention, raw material is easy to get, and raw material cost is low, and low energy consumption for process, and reaction condition is mild, and working condition is easy control
System reacts noon pollutant emission, energy conservation and environmental protection.In production, obtained nano-titanium dioxide powder purity is up to 99.5%, nanometer
The partial size of titanium dioxide is small, and particle size distribution range is small, good dispersion;In production, the rare earth cerium doping into titanium dioxide, to extend
In the service life of photo-generate electron-hole pair, the quantum effect of nano-titanium dioxide is improved, and then reaches the light for improving nano-titanium dioxide
The purpose of catalytic activity, the drop to improve air purification effect, especially to volatile organic contaminant (such as: formaldehyde gas)
Solve it is high-efficient, up to 90% or more, good air purification effect.
In the present invention, guarantee that titanium elements are fully dissolved in hydrochloric acid, improves yield.It is double that oxidant is used in reaction process
Oxygen water, hydrogen peroxide is at low cost, and oxidation effectiveness is good, and does not generate additional pollution, and environment protecting is good;Titanium dioxide is in high temperature 700-
It is calcined under conditions of 800 degrees Celsius, the unstable sundries in titanium dioxide gasifies under the high temperature conditions, to improve dioxy
Change the purity of titanium;Meanwhile the titanium dioxide agglomeration after high-temperature calcination is easy to break into pieces, and the nano-titanium dioxide tool formed after breaking into pieces
There is good dispersibility, is conducive to nano-titanium dioxide and is dissolved in other solvents and subsequent use.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment, right
The present invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the invention.
It is of the invention general to avoid unnecessarily obscuring in addition, in the following description, descriptions of well-known structures and technologies are omitted
It reads.
A kind of air cleaning nano-titanium dioxide preparation method proposed by the present invention, comprising the following steps:
S1, titanium iron ore is chosen, and titanium iron ore is processed into powdered;
S2, concentrated hydrochloric acid progress acidolysis is added into powdered titanium iron ore, the mine acid of molten mine compares for 4-6, acidolysis temperature 50-
100 degrees Celsius;1-2 hours are stood after the molten mine of acidolysis, refilters removal slag, obtains once filtering titanium liquid A;
S3, titanium liquid A are cooled to room temperature, and Iron dichloride tetrahydrate is precipitated in crystallization in titanium liquid A, and four chloride hydrates in titanium liquid A are sub-
Iron is filtered removal, obtains secondary filter titanium liquid B;
S4, oxidant is added into secondary filter titanium liquid B, converts iron chloride for remaining frerrous chloride, obtains solution D;
S5, cerous nitrate is added into solution D, and be added sodium hydroxide adjust PH for alkalinity after, be sufficiently mixed to obtain suspension C;
S5, activated carbon fibre is added into suspension C, and is impregnated 0.5-1 hours under ultrasound condition, obtain mixed liquor D;
S6, mixed liquor D is evaporated and is dried, obtain mixture E;
S7, mixture is heated 2-4 hours under 200-250 degrees Celsius of temperature environment, then is calcined, obtain block F;
S8, block F is milled into powder, obtains the nano titanium dioxide powder for mixing cerium.
In the present invention, raw material is easy to get, and raw material cost is low, and low energy consumption for process, and reaction condition is mild, and working condition holds
It is easy to control, react noon pollutant emission, energy conservation and environmental protection.
In the present invention, the nano-titanium dioxide powder purity that produces is up to 99.5%, the partial size of nano-titanium dioxide
Small, particle size distribution range is small, good dispersion;In production, the rare earth cerium doping into titanium dioxide, to extend photo-generate electron-hole
Pair service life, improve the quantum effect of nano-titanium dioxide, so reach improve nano-titanium dioxide photocatalytic activity mesh
, it is especially high to the degradation efficiency of volatile organic contaminant (such as: formaldehyde gas) to improve air purification effect, it can
Up to 90% or more, good air purification effect.
In an alternative embodiment, in S2, the concentration of concentrated hydrochloric acid is 30-38%, improves hydrochloric acid to titanium iron ore
Acidolysis effect guarantees that titanium elements are fully dissolved in hydrochloric acid, improves yield.
In an alternative embodiment, in S4, oxidant is hydrogen peroxide, and hydrogen peroxide is at low cost, and oxidation effectiveness is good, and not
Additional pollution is generated, environment protecting is good.
In an alternative embodiment, in the filter process of S2 and S4, distilled water flushing, flushing liquor are used to filter cake
It is back in filtrate, to avoid the filtrate adsorbed in recycling filter cake, filter cake is rinsed using distilled water, to guarantee to filter
The content of titanium in liquid improves output, guarantees the quality of production.
In an alternative embodiment, in S7, calcination temperature is 700-800 degrees Celsius;
It should be noted that the substance in filtrate is fully calcined under conditions of 700-800 degrees Celsius of high temperature, part is unstable
Determine sundries to gasify under the high temperature conditions, to guarantee the purity of product;Meanwhile the titanium dioxide agglomeration after high-temperature calcination is easy to strike
It is broken, and the nano-titanium dioxide formed after breaking into pieces has dispersibility well, being conducive to nano-titanium dioxide, to be dissolved in other molten
Agent and subsequent use.
It should be understood that above-mentioned specific embodiment of the invention is used only for exemplary illustration or explains of the invention
Principle, but not to limit the present invention.Therefore, that is done without departing from the spirit and scope of the present invention is any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.In addition, appended claims purport of the present invention
Covering the whole variations fallen into attached claim scope and boundary or this range and the equivalent form on boundary and is repairing
Change example.
Claims (5)
1. a kind of air cleaning nano-titanium dioxide preparation method, which comprises the following steps:
S1, titanium iron ore is chosen, and titanium iron ore is processed into powdered;
S2, concentrated hydrochloric acid progress acidolysis is added into powdered titanium iron ore, the mine acid of molten mine compares for 4-6, acidolysis temperature 50-
100 degrees Celsius;1-2 hours are stood after the molten mine of acidolysis, refilters removal slag, obtains once filtering titanium liquid A;
S3, titanium liquid A are cooled to room temperature, and Iron dichloride tetrahydrate is precipitated in crystallization in titanium liquid A, and four chloride hydrates in titanium liquid A are sub-
Iron is filtered removal, obtains secondary filter titanium liquid B;
S4, oxidant is added into secondary filter titanium liquid B, converts iron chloride for remaining frerrous chloride, obtains solution D;
S5, cerous nitrate is added into solution D, and be added sodium hydroxide adjust PH for alkalinity after, be sufficiently mixed to obtain suspension C;
S5, activated carbon fibre is added into suspension C, and is impregnated 0.5-1 hours under ultrasound condition, obtain mixed liquor D;
S6, mixed liquor D is evaporated and is dried, obtain mixture E;
S7, mixture is heated 2-4 hours under 200-250 degrees Celsius of temperature environment, then is calcined, obtain block F;
S8, block F is milled into powder, obtains the nano titanium dioxide powder for mixing cerium.
2. air cleaning nano-titanium dioxide water solution preparation method according to claim 1, which is characterized in that in S2
In, the concentration of concentrated hydrochloric acid is 30-38%.
3. air cleaning nano-titanium dioxide water solution preparation method according to claim 1, which is characterized in that in S4,
Oxidant is hydrogen peroxide.
4. air cleaning nano-titanium dioxide water solution preparation method according to claim 1, which is characterized in that in S2 and
In the filter process of S4, distilled water flushing is used to filter cake, flushing liquor is back in filtrate.
5. air cleaning nano-titanium dioxide water solution preparation method according to claim 1, which is characterized in that in S7,
Calcination temperature is 700-800 degrees Celsius.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114105475A (en) * | 2021-11-30 | 2022-03-01 | 汕头职业技术学院 | Nano titanium dioxide glaze and preparation method thereof |
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US20070082959A1 (en) * | 2005-09-27 | 2007-04-12 | Guangdong Institute Of Eco-Environment And Soil Science | Method for producing high-active titanium dioxide hydrosol by using metatitanate as precursor |
CN102658115A (en) * | 2012-05-09 | 2012-09-12 | 桂林电子科技大学 | Cerium-doped nano titanium dioxide/activated carbon fiber composite photocatalyst for air purification and preparation method thereof |
CN104071830A (en) * | 2014-04-30 | 2014-10-01 | 山东天大傅山工程技术研究院 | Method for preparing high-purity rutile type or anatase type nanometer titanium dioxide |
CN108554417A (en) * | 2018-05-28 | 2018-09-21 | 昆明理工大学 | A kind of preparation method of iron cerium-doped nanometer titanium dioxide multiple elements design semiconductor light-catalyst and application |
US20180318820A1 (en) * | 2016-12-01 | 2018-11-08 | GM Global Technology Operations LLC | Nucleation layers for enhancing photocatalytic activity of titanium dioxide (tio2) coatings |
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2019
- 2019-03-25 CN CN201910228728.2A patent/CN110078119A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US20070082959A1 (en) * | 2005-09-27 | 2007-04-12 | Guangdong Institute Of Eco-Environment And Soil Science | Method for producing high-active titanium dioxide hydrosol by using metatitanate as precursor |
CN102658115A (en) * | 2012-05-09 | 2012-09-12 | 桂林电子科技大学 | Cerium-doped nano titanium dioxide/activated carbon fiber composite photocatalyst for air purification and preparation method thereof |
CN104071830A (en) * | 2014-04-30 | 2014-10-01 | 山东天大傅山工程技术研究院 | Method for preparing high-purity rutile type or anatase type nanometer titanium dioxide |
US20180318820A1 (en) * | 2016-12-01 | 2018-11-08 | GM Global Technology Operations LLC | Nucleation layers for enhancing photocatalytic activity of titanium dioxide (tio2) coatings |
CN108554417A (en) * | 2018-05-28 | 2018-09-21 | 昆明理工大学 | A kind of preparation method of iron cerium-doped nanometer titanium dioxide multiple elements design semiconductor light-catalyst and application |
Cited By (1)
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CN114105475A (en) * | 2021-11-30 | 2022-03-01 | 汕头职业技术学院 | Nano titanium dioxide glaze and preparation method thereof |
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