CN106115775B - Adulterate the preparation method of positive metatitanic acid - Google Patents
Adulterate the preparation method of positive metatitanic acid Download PDFInfo
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- CN106115775B CN106115775B CN201610498988.8A CN201610498988A CN106115775B CN 106115775 B CN106115775 B CN 106115775B CN 201610498988 A CN201610498988 A CN 201610498988A CN 106115775 B CN106115775 B CN 106115775B
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- titanium
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- metatitanic acid
- sulphate solution
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
Abstract
The present invention relates to a kind of preparation method for the positive metatitanic acid that adulterates, belong to chemical field.The preparation method of positive metatitanic acid of adulterating comprises the following steps：(1) using industrial titanium sulphate solution as raw material, industrial titanium sulphate solution is added into solid ammonium class carbonate powder, preneutralization is carried out to industrial titanium sulphate solution, pH value is adjusted, the ferrous ion in industrial titanium sulphate solution is crystallized；(2) after crystallization is separated, filter cake and filtrate are obtained；(3) filtrate is diluted；(4) filtrate is slowly added to ammoniacal liquor and carries out second of neutralization, controls endpoint pH, titanium hydrolysis is obtained milky titanium hydrolysate；(5) hydrolysate is washed after separation of solid and liquid, that is, obtains the positive metatitanic acid that adulterates.The preparation method for the positive metatitanic acid of doping that the present invention is provided, using industrial titanium sulphate solution as titanium source, cheap and easy to get, the preparation method simplicity of titanium source, the titanic acid activity height prepared etc..
Description
Technical field
The present invention relates to a kind of preparation method for the positive metatitanic acid that adulterates, belong to chemical field.
Technical background
Positive metatitanic acid, white non-crystalline solids, also known as amorphous compound, α metatitanic acids.Positive metatitanic acid is amphiprotic substance, solvable
In hot concentrated alkali liquid, it is dissolved at normal temperatures in the inorganic acids such as watery hydrochloric acid, dilute sulfuric acid and acid stronger organic acid.In water and alcohol
It is insoluble, but easily it is converted into colloid in water.Positive metatitanic acid, with very high reactivity, is increasingly becoming as amphiprotic substance
Research emphasis of art circle in terms of novel energy.
There are some methods for synthesizing positive metatitanic acid at present, but be with expensive tetraethyl titanate, metatitanic acid isopropanol, titanium mostly
The inorganic ti sources such as organic titanium source or analytically pure titanium tetrachloride, titanium sulfate, titanyl sulfate such as sour four butyl esters are used as the initial of synthesis
Raw material prepares positive metatitanic acid, and cost is higher.
The content of the invention
For above-mentioned technical problem, cheap industrial titanium sulphate solution is used for titanium source the invention provides one kind, prepares doping titanic
The preparation method of acid.It is characterized in using industrial titanium sulphate solution as initial feed, terminal is neutralized using weak base regulation, carries out secondary neutralize and make
Standby positive metatitanic acid.
The technical solution adopted for the present invention to solve the technical problems is implemented as follows：
Adulterate the preparation method of positive metatitanic acid, comprise the following steps：
(1) using industrial titanium sulphate solution as initial titanium source, industrial titanium sulphate solution is added into solid ammonium class carbonate ammonium carbonate powder, to industry
Titanium liquid carries out preneutralization to pH 1-1.5, enough time is kept, by the ferrous ion mass crystallization in industrial titanium sulphate solution；
(2) iron, titanium separation are realized after Crystallization Separation substantially, filter cake is Mohr's salt, to filter cake pH=1 saturation Mohr's salt
Solution washing is handled, and filtrate is then the titanium salt solution containing Low Concentration Iron；
(3) filtrate is diluted, control titanium concentration is within the scope of 0.1-0.5mol/L；
(4) it is slowly added to certain density ammoniacal liquor and carries out second to neutralize, control endpoint pH is in 5-7 but no more than 7
Scope, makes titanium hydrolysis obtain milky titanium hydrolysate；
(5) after separation of solid and liquid to hydrolysate with pH=2~3 (dilute sulfuric acid) and containing reducing agent (hydroxylamine hydrochloride or ascorbic acid)
Mixed solution for 1%~5% (mass percent) is washed, you can obtain the positive metatitanic acid of doping with high reaction activity.
Because industrial titanium sulphate solution has the titanium of high content, iron, sulfuric acid and containing other more impurity, pass through and regulate and control hydrolysis work
Skill condition, prepares the impurity composition of doping catalytic activity, reaches that a step prepares advanced function material by industrial primary raw materials, can
Realization is with being prepared into local reduction and synthesis step simplified.
The preparation method for the positive metatitanic acid of doping that the present invention is provided, is synchronously prepared for iron ammonium sulfate, iron ammonium sulfate is one
Important industrial chemicals is planted, purposes is quite varied.It can make water purification agent；In inorganic chemistry industry, it is to produce other iron
The raw material of compound, is such as used to manufacture iron oxide pigment, magnetic material, potassium ferrocyanide and other molysite；It also has many sides
The direct application in face, such as can be used as being used to be used as anti-corrosion in tanning, timber industry in the mordant of printing and dyeing industry, leather industry
It is used to treat in agent, medicine to be applied in iron-deficient soil, animal husbandry in hypoferric anemia, agricultural and is used as feed addictive etc.,
Blue-black ink is configured after can also being mixed with tannic acid, gallic acid etc..
The preparation method for the positive metatitanic acid of doping that the present invention is provided, using industrial titanium sulphate solution as titanium source, cheap and easy to get, the preparation of titanium source
Method is easy, titanic acid activity height prepared etc..
Embodiment
Present invention is expanded on further with reference to embodiment, but these embodiments are not intended to limit the protection model of the present invention
Enclose.
The present invention is described in detail below by reference to embodiment.The industrial titanium sulphate solution specific targets that this example is used are such as
Shown in table 1：
The industrial sulphuric acid titanium liquid index of table 1
| TiO2g/l | Fe/TiO2 | F values | Ti3+g/l |
| 198.08g/L | 0.32 | 1.88 | 1.63 |
Embodiment 1
Take 80ml industrial titanium sulphate solutions to be put into jar agitation, add common 15.88g solid carbonic acids ammonium powdered reaction for a period of time until
Without substantially acutely bubble generation, viscosity occurs significant change, measures now pH value 1.0.Slurries suction filtration is obtained into greenish transparent
Filtrate, it is 0.2mol/L that filtrate is diluted into titanium concentration with deionized water, the ammoniacal liquor that concentration is 3mol/L is slowly added dropwise, in control
With terminal 6, hydrolysis obtains milky suspension, and suction filtration is that can obtain titanic acid product.The made positive metatitanic acids of 10g are taken to add 30ml
Deionized water stirs, and adding citric acid can dissolve at once, and activity is higher.
Embodiment 2
Take 80ml industrial titanium sulphate solutions to be put into jar agitation, add common 16.09g solid carbonic acids ammonium powdered reaction for a period of time until
Without substantially acutely bubble generation, viscosity occurs significant change, measures now pH value 1.1.Slurries suction filtration is obtained into greenish transparent
Filtrate, it is 0.3mol/L that filtrate is diluted into titanium concentration with deionized water, the ammoniacal liquor that concentration is 3mol/L is slowly added dropwise, in control
With terminal 5.5, hydrolysis obtains milky suspension, and suction filtration is that can obtain titanic acid product.The made positive metatitanic acids of 20g are taken to add
50ml deionized waters stir, and adding acetylacetone,2,4-pentanedione can dissolve at once, and activity is higher.
Embodiment 3
Take 80ml industrial titanium sulphate solutions to be put into jar agitation, add common 17.018g solid carbonic acids ammonium powdered reaction straight for a period of time
To without substantially acutely bubble generation, viscosity occurs significant change, measures now pH value 1.2.Slurries suction filtration is obtained into light green color saturating
Bright filtrate, it is 0.4mol/L that filtrate is diluted into titanium concentration with deionized water, and the ammoniacal liquor that concentration is 3mol/L, control is slowly added dropwise
Terminal is neutralized 6.2, hydrolysis obtains milky suspension, and suction filtration is that can obtain titanic acid product.The made positive metatitanic acids of 15g are taken to add
40ml deionized waters stir, and adding ammonium fluoride can dissolve at once, and activity is higher.
Embodiment 4
Take 80ml industrial titanium sulphate solutions to be put into jar agitation, add common 17.03g solid carbonic acids ammonium powdered reaction for a period of time until
Without substantially acutely bubble generation, viscosity occurs significant change, measures now pH value 1.3.Slurries suction filtration is obtained into greenish transparent
Filtrate, it is 0.15mol/L that filtrate is diluted into titanium concentration with deionized water, and the ammoniacal liquor that concentration is 3mol/L, control is slowly added dropwise
Terminal is neutralized 6.8, hydrolysis obtains milky suspension, and suction filtration is that can obtain titanic acid product.The made positive metatitanic acids of 18g are taken to add
20ml deionized waters stir, and adding tartaric acid can dissolve at once, and activity is higher.
Embodiment 5
Take 80ml industrial titanium sulphate solutions to be put into jar agitation, add common 16.53g solid carbonic acids ammonium powdered reaction for a period of time until
Without substantially acutely bubble generation, viscosity occurs significant change, measures now pH value 0.89.Slurries suction filtration is obtained into greenish transparent
Filtrate, it is 0.2mol/L that filtrate is diluted into titanium concentration with deionized water, the ammoniacal liquor that concentration is 3mol/L is slowly added dropwise, in control
With terminal 5.8, hydrolysis obtains milky suspension, and suction filtration is that can obtain titanic acid product.The made positive metatitanic acids of 13g are taken to add
25ml deionized waters stir, and adding acetic acid can dissolve at once, and activity is higher.
Disclosed herein is the embodiment of the present invention, although has used specific term, but only with general sum
The descriptive meaning uses and explained that these belong to, rather than limitation purpose.Therefore, those of ordinary skill in the art should
Understand, can be in form and details in the case where not departing from the spirit and scope of the present invention as set forth in the claims
Make change.
Claims (4)
1. the preparation method of the positive metatitanic acid of doping, it is characterised in that comprise the following steps：
（1）Using industrial titanium sulphate solution as raw material, described industrial titanium sulphate solution is industrial sulphuric acid titanium liquid, and industrial titanium sulphate solution is added into solid ammonium class carbon
Hydrochlorate powder, preneutralization is carried out to industrial titanium sulphate solution, adjusts pH value, pH value regulates and controls to 1-1.5, by the ferrous ion in industrial titanium sulphate solution
Crystallization；
（2）After crystallization is separated, filter cake and filtrate are obtained；Filter cake is Mohr's salt, molten with the saturation Mohr's salt of pH=1 to filter cake
Liquid is washed；
（3）Filtrate is diluted；
（4）Filtrate is slowly added to ammoniacal liquor and carries out second of neutralization, and control endpoint pH makes titanium hydrolysis obtain milky titanium in 5-7
Hydrolysate；
（5）Hydrolysate is washed after separation of solid and liquid, that is, obtains the positive metatitanic acid that adulterates.
2. the preparation method of the positive metatitanic acid of doping according to claim 1, it is characterised in that described step（1）In, solid
Ammonium class carbonate powder is solid carbonic acid ammonium powder.
3. the preparation method of the positive metatitanic acid of doping according to claim 1, it is characterised in that described step（3）Middle filtrate
The concentration of dilution is in 0.1-0.5mol/L.
4. the preparation method of the positive metatitanic acid of doping according to claim 1, it is characterised in that described step（5）In to water
Solution thing is washed, and is washed with pickling and reducing agent, and detergent used is the dilution heat of sulfuric acid of pH=2 ~ 3, and reducing agent is to contain matter
Measure the hydroxylamine hydrochloride or ascorbic acid solution of percentage 1% ~ 5%.
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| CN1078181C (en) * | 1997-11-14 | 2002-01-23 | 中国科学院化工冶金研究所 | Process for producing nanometre-grade titanic-schorl type titanium dioxide |
| CN1324767A (en) * | 2001-07-12 | 2001-12-05 | 张汝冰 | Low temperature prepn. of rutile type nanometer titania by using titanic acid as raw material |
| CN1206164C (en) * | 2003-02-12 | 2005-06-15 | 成都理工大学 | Method for preparing liquid state predecessor of nano titanium dioxide |
| CN1552785A (en) * | 2003-06-05 | 2004-12-08 | 上海祥雅涂料有限公司 | Orthobutyl titanate modified organic specific condensate coating material and its preparation |
| CN1264754C (en) * | 2004-07-19 | 2006-07-19 | 南京大学 | Preparation method of nanometer rutile type titanium dioxide |
| CN100484880C (en) * | 2005-09-22 | 2009-05-06 | 中国科学院理化技术研究所 | Low temperature crystallized nano titanium dioxide powder and sol synthesizing method |
| CN101456583B (en) * | 2007-12-12 | 2011-05-25 | 中国科学院理化技术研究所 | Synthetic method for preparing rutile type nano titanic oxide sol or powder at low temperature |
| CN101300982A (en) * | 2008-06-27 | 2008-11-12 | 中南大学 | Method for preparing silver-carrying nano titanic oxide |
| CN101643358A (en) * | 2009-08-24 | 2010-02-10 | 山东国瓷功能材料有限公司 | Microwave liquid phase compounding process of high-purity barium titanate powder |
| CN101967010B (en) * | 2010-11-04 | 2012-07-25 | 中南大学 | Method for preparing nano-TiO2 serving as cathode material of lithium ion battery |
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| CN102963925B (en) * | 2012-11-26 | 2014-08-20 | 山东大学 | Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor |
| CN103193478B (en) * | 2013-04-15 | 2014-04-09 | 陕西师范大学 | Magnesium titanate based composite ceramic sintered at low temperature and preparation method thereof |
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