CN106115775A - Adulterate the preparation method of positive metatitanic acid - Google Patents
Adulterate the preparation method of positive metatitanic acid Download PDFInfo
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- CN106115775A CN106115775A CN201610498988.8A CN201610498988A CN106115775A CN 106115775 A CN106115775 A CN 106115775A CN 201610498988 A CN201610498988 A CN 201610498988A CN 106115775 A CN106115775 A CN 106115775A
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- C01—INORGANIC CHEMISTRY
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- 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
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Abstract
The present invention relates to the preparation method of a kind of positive metatitanic acid that adulterates, belong to chemical field.The preparation method of positive metatitanic acid of adulterating comprises the following steps: industrial titanium sulphate solution, with industrial titanium sulphate solution as raw material, is added solid ammonium class carbonate powder by (1), and industrial titanium sulphate solution carries out preneutralization, regulates pH value, is crystallized by the ferrous ion in industrial titanium sulphate solution；(2), after crystallization separates, filter cake and filtrate are obtained；(3) filtrate is diluted；(4) filtrate be slowly added to ammonia carry out second time neutralize, control endpoint pH, make titanium hydrolysis obtain milky titanium hydrolysate；(5) after solid-liquid separation, hydrolysate is washed, i.e. obtain the positive metatitanic acid that adulterates.The preparation method of what the present invention provided adulterate positive metatitanic acid, with industrial titanium sulphate solution for titanium source, titanium source cheap and easy to get, preparation method is easy, and the titanic acid activity prepared is high.
Description
Technical field
The present invention relates to the preparation method of a kind of positive metatitanic acid that adulterates, belong to chemical field.
Technical background
Positive metatitanic acid, white non-crystalline solids, amorphous compound, it is also called α metatitanic acid.Positive metatitanic acid is amphiprotic substance, solvable
In hot concentrated alkali liquid, it is dissolved at normal temperatures in the mineral acid such as dilute hydrochloric acid, dilute sulfuric acid and the stronger organic acid of acidity.In water and alcohol
Insoluble, but in water, easily it is converted into colloid.Positive metatitanic acid, as amphiprotic substance, has the highest reactivity, is increasingly becoming
Art circle research emphasis in terms of novel energy.
There are some methods synthesizing positive metatitanic acid at present, but are 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 acid four butyl esters are initial as synthesize
Positive metatitanic acid prepared by raw material, relatively costly.
Summary of the invention
For above-mentioned technical problem, the invention provides the cheap industrial titanium sulphate solution of a kind of employing is titanium source, preparation doping titanic
The preparation method of acid.It is characterized in industrial titanium sulphate solution as initial feed, utilizes weak base regulation to neutralize terminal, carry out in secondary and system
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) with industrial titanium sulphate solution for initial titanium source, industrial titanium sulphate solution is added solid ammonium class carbonate ammonium carbonate powder, to industry
Titanium liquid carries out preneutralization to pH 1-1.5, keeps enough time, by the ferrous ion mass crystallization in industrial titanium sulphate solution；
(2) substantially realize ferrum after Crystallization Separation, titanium separates, and filter cake is Mohr's salt, the saturated Mohr's salt to filter cake pH=1
Solution washing processes, and filtrate is then the titanium salt solution containing Low Concentration Iron；
(3) filtrate is diluted, control titanium concentration within the scope of 0.1-0.5mol/L；
(4) it is slowly added to certain density ammonia carry out neutralizing for the second time, controls endpoint pH and at 5-7 but be less than 7
Scope, makes titanium hydrolysis obtain milky titanium hydrolysate；
(5) to hydrolysate pH=2～3 (dilute sulfuric acid) and (oxammonium hydrochloride. or ascorbic acid) Han reducing agent after solid-liquid separation
It is that the mixed solution of 1%～5% (mass percent) washs, i.e. can obtain the positive metatitanic acid of doping with high reaction activity.
Owing to industrial titanium sulphate solution has the titanium of high-load, ferrum, sulphuric acid and contains other more impurity, by regulation and control hydrolysis work
Skill condition, prepares the impurity composition of doping catalysis activity, reaches a step and is prepared advanced function material by industry primary raw materials, can
Realization simplifies with being prepared as local reduction and synthesis step.
The preparation method of the positive metatitanic acid of doping that the present invention provides, synchronizes to be prepared for Ferrous ammonium sulfate, and Ferrous ammonium sulfate is one
Planting important industrial chemicals, purposes is quite varied.It can make water purification agent；In inorganic chemistry industry, it is to produce other ferrum
The raw material of compound, as being used for manufacturing iron oxide pigment, magnetic material, potassium ferrocyanide and other iron salt etc.；It also has many sides
The directly application in face, as can be used as the mordant of printing and dyeing industry, for tanning in leather industry, is used as anticorrosion in timber industry
Agent, is used for treating iron deficiency anemia in medicine, be applied to iron-deficient soil in agricultural, is used as feed additive etc. in animal husbandry,
Blue-black ink can also be configured with tannic acid, gallic acid etc. after mixing.
The preparation method of what the present invention provided adulterate positive metatitanic acid, with industrial titanium sulphate solution for titanium source, titanium source cheap and easy to get, preparation
Method is easy, and the titanic acid activity prepared is high.
Detailed description of the invention
Present invention is expanded on further below in conjunction with embodiment, but these embodiments are not limiting as the protection model of the present invention
Enclose.
Below by reference to embodiment, the present invention is described in detail.The industrial titanium sulphate solution specific targets that this example uses are such as
Shown in table 1:
Table 1 industrial sulphuric acid titanium liquid index
| TiO2g/l | Fe/TiO2 | F value | Ti3+g/l |
| 198.08g/L | 0.32 | 1.88 | 1.63 |
Embodiment 1
Take 80ml industrial titanium sulphate solution and put into jar agitation, add altogether 15.88g solid carbonic acid ammonium powdered reaction a period of time until
Produce without the most acutely bubble, viscosity generation significant change, record now pH value 1.0.Serosity sucking filtration is obtained greenish transparent
Filtrate, filtrate deionized water is diluted to titanium concentration is 0.2mol/L, is slowly added dropwise the ammonia that concentration is 3mol/L, in control
With terminal 6, hydrolysis obtains milky suspension, and sucking filtration i.e. can get titanic acid product.Take the made positive metatitanic acid of 10g and add 30ml
Deionized water stirs, and adding citric acid can dissolve at once, and activity is higher.
Embodiment 2
Take 80ml industrial titanium sulphate solution and put into jar agitation, add altogether 16.09g solid carbonic acid ammonium powdered reaction a period of time until
Produce without the most acutely bubble, viscosity generation significant change, record now pH value 1.1.Serosity sucking filtration is obtained greenish transparent
Filtrate, filtrate deionized water is diluted to titanium concentration is 0.3mol/L, is slowly added dropwise the ammonia that concentration is 3mol/L, in control
With terminal 5.5, hydrolysis obtains milky suspension, and sucking filtration i.e. can get titanic acid product.Take the made positive metatitanic acid of 20g to add
50ml deionized water stirs, and adding acetylacetone,2,4-pentanedione can dissolve at once, and activity is higher.
Embodiment 3
Take 80ml industrial titanium sulphate solution and put into jar agitation, add 17.018g solid carbonic acid ammonium powdered reaction a period of time altogether straight
Produce to without the most acutely bubble, viscosity generation significant change, record now pH value 1.2.Serosity sucking filtration is obtained light green color saturating
Bright filtrate, filtrate deionized water is diluted to titanium concentration is 0.4mol/L, is slowly added dropwise the ammonia that concentration is 3mol/L, controls
Neutralization terminal is 6.2, and hydrolysis obtains milky suspension, and sucking filtration i.e. can get titanic acid product.Take the made positive metatitanic acid of 15g to add
40ml deionized water stirs, and adding ammonium fluoride can dissolve at once, and activity is higher.
Embodiment 4
Take 80ml industrial titanium sulphate solution and put into jar agitation, add altogether 17.03g solid carbonic acid ammonium powdered reaction a period of time until
Produce without the most acutely bubble, viscosity generation significant change, record now pH value 1.3.Serosity sucking filtration is obtained greenish transparent
Filtrate, filtrate deionized water is diluted to titanium concentration is 0.15mol/L, is slowly added dropwise the ammonia that concentration is 3mol/L, controls
Neutralization terminal is 6.8, and hydrolysis obtains milky suspension, and sucking filtration i.e. can get titanic acid product.Take the made positive metatitanic acid of 18g to add
20ml deionized water stirs, and adding tartaric acid can dissolve at once, and activity is higher.
Embodiment 5
Take 80ml industrial titanium sulphate solution and put into jar agitation, add altogether 16.53g solid carbonic acid ammonium powdered reaction a period of time until
Produce without the most acutely bubble, viscosity generation significant change, record now pH value 0.89.Serosity sucking filtration is obtained greenish transparent
Filtrate, filtrate deionized water is diluted to titanium concentration is 0.2mol/L, is slowly added dropwise the ammonia that concentration is 3mol/L, in control
With terminal 5.8, hydrolysis obtains milky suspension, and sucking filtration i.e. can get titanic acid product.Take the made positive metatitanic acid of 13g to add
25ml deionized water stirs, and adding acetic acid can dissolve at once, and activity is higher.
Disclosed herein is the embodiment of the present invention, although employ specific term, but only with general sum
The illustrative meaning uses and explains these purposes belonging to rather than limiting.Therefore, those of ordinary skill in the art should
Understand, in the case of without departing from the spirit and scope of the present invention as set forth in the claims, can be in form and details
Make change.
Claims (7)
1. the preparation method of the positive metatitanic acid of doping, it is characterised in that comprise the following steps:
(1) with industrial titanium sulphate solution as raw material, industrial titanium sulphate solution is added solid ammonium class carbonate powder, industrial titanium sulphate solution is carried out pre-in
With, regulate pH value, the ferrous ion in industrial titanium sulphate solution is crystallized；
(2), after crystallization separates, filter cake and filtrate are obtained；
(3) filtrate is diluted；
(4) filtrate be slowly added to ammonia carry out second time neutralize, control endpoint pH, make titanium hydrolysis obtain milky titanium hydrolysis
Thing；
(5) after solid-liquid separation, hydrolysate is washed, i.e. obtain the positive metatitanic acid that adulterates.
The preparation method of the positive metatitanic acid of doping the most according to claim 1, it is characterised in that pre-in described step (1)
Neutralizing pH value to regulate and control to 1-1.5, solid ammonium class carbonate powder is solid carbonic acid ammonium powder.
The preparation method of the positive metatitanic acid of doping the most according to claim 1, it is characterised in that in described step (1), solid
Ammonium class carbonate powder is solid carbonic acid ammonium powder.
The preparation method of the positive metatitanic acid of doping the most according to claim 1, it is characterised in that gained in described step (2)
Filter cake is Mohr's salt, washs the saturated mohr salt solution of filter cake pH=1.
The preparation method of the positive metatitanic acid of doping the most according to claim 1, it is characterised in that filtrate in described step (3)
The concentration of dilution is at 0.1-0.5mol/L.
The preparation method of the positive metatitanic acid of doping the most according to claim 1, it is characterised in that described in step (4) two
Secondary neutralization pH value is at 5-7.
The preparation method of the positive metatitanic acid of doping the most according to claim 1, it is characterised in that to water in described step (5)
Solving thing to wash, wash with pickling and reducing agent, detergent used is the dilution heat of sulfuric acid of pH=2～3, and reducing agent is for containing
The oxammonium hydrochloride. of mass percent 1%～5% or ascorbic acid solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111847520A (en) * | 2020-08-07 | 2020-10-30 | 攀枝花学院 | Preparation method of ammonium ferrous sulfate |
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| CN111847520A (en) * | 2020-08-07 | 2020-10-30 | 攀枝花学院 | Preparation method of ammonium ferrous sulfate |
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