CN1071145A - Introduce iron protochloride and prepare rutile titanium dioxide - Google Patents

Introduce iron protochloride and prepare rutile titanium dioxide Download PDF

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Publication number
CN1071145A
CN1071145A CN 91108973 CN91108973A CN1071145A CN 1071145 A CN1071145 A CN 1071145A CN 91108973 CN91108973 CN 91108973 CN 91108973 A CN91108973 A CN 91108973A CN 1071145 A CN1071145 A CN 1071145A
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China
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titanium dioxide
rutile
rutile titanium
introduce
metatitanic acid
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CN 91108973
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CN1029466C (en
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张允什
张大昕
封显抱
臧石
刘占泉
王虹
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Nankai University
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Nankai University
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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
    • C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

A kind of calcining obtains the method that metatitanic acid prepares rutile titanium dioxide from hydrolysising titanium salt---introduce the protochloride iron processes, it is to introduce a certain amount of iron protochloride in the titanyl sulfate solution of the removal of impurities that obtains with sulfuric acid decomposition ilmenite, add crystal seeds of rutile again, heating hydrolysis generates metatitanic acid, after washing down, dry, grinding, add (perhaps not adding) crystal type promoting reagent ZnO, MgO, calcining is 6-10 hours in 750-850 ℃ of temperature ranges.Gained titanium dioxide rutile content is 100%.

Description

Introduce iron protochloride and prepare rutile titanium dioxide
The invention belongs to the preparation of inorganic, metal oxide.
At present the production method of the titanium dioxide of existing bibliographical information mainly contains sulfuric acid process [the clear 54-04899 of Ri Tekai], chlorination process volumes such as [, " sulfate process titanium dioxide production ", Chemical Industry Press, 1982] Pei Run, salt acid system [coatings industry, 1974, No1,18; No 2 22; No 3,66; 1976 No 1,26; CN 86106205] and complex salt method [CN 1034703A] etc.
Sulfuric acid process is loaded down with trivial details, and useless byproduct is many, pollutes more serious, the invert point height of production rutile titanium dioxide; The salt acid system is strict to the corrosion resistant requirement of equipment; The chlorination rule is all strict to equipment material and ingredient requirement; The operating process of complex salt method is numerous and diverse, does not see the report of scale operation as yet.
The objective of the invention is to create a kind of new method for preparing rutile titanium dioxide: promptly introduce the protochloride iron processes.The equipment that this method has not only kept sulfuric acid process is simple, and the salt acid system easily forms the advantage of rutile-type crystal formation, has overcome the shortcoming in above-mentioned each method again.
The present invention is that to decompose ilmenite gained titanyl sulfate solution with sulfuric acid be starting raw material, and after deironing purified, (consumption was TiO to introduce solution of ferrous chloride 2: FeCl 2.4H 2O=1: remove the ferrous sulfate of separating out after 0.97～3.88) freezing, the crystal seeds of rutile that adds 1-6% then, heating hydrolysis, with the washing of gained metatitanic acid, removal of impurities, rinsing, drying, grinding, add again crystal type promoting reagent ZnO.MgO each 1.0%, sent into temperature range and be in 750-850 ℃ the retort furnace calcining 6-10 hour, making rutile titanium dioxide content is 100%.
The present invention is less demanding to equipment material, obtains the high rutile titanium dioxide of rate of formation easily.
Example 1
To decompose the titanyl sulfate solution that ilmenite obtains with sulfuric acid and (contain TiO 2206g/l) 100ml adds FeCl 2.4H 2O 80g is through dissolving, remove the FeSO that separates out after freezing 4.7H 2O adds rutilization nuclei (6%) again, and heating hydrolysis generates metatitanic acid.The metatitanic acid that generates is washed down, dries, grinds, get 3g and insert and be warming up to 850 ℃ in the retort furnace, and be incubated 10 hours, gained rutile titanium dioxide, content are that 100%(sees Fig. 1).
Example 2
Get the titanyl sulfate solution 100ml identical, add FeCl with example 1 2.4H 2O 20g is through dissolving, the freezing FeSO that separates out that removes 4.7H 2Behind the O, add 6% rutilization nuclei, heating hydrolysis generates metatitanic acid, it is washed down, dries, get 3g and add crystal type promoting reagent ZnO, MgO each 1%, insert and be warming up to 800 ℃ in the retort furnace, and be incubated 10 hours, gained titanium dioxide rutile content is that 100%(sees Fig. 2).
Example 3
Get the titanyl sulfate solution 100ml identical, add FeCl with example 1 2.4H 2O 40g, below operation is with example 2, gained titanium dioxide rutile content is that 100%(sees Fig. 5).
Example 4
Get the titanyl sulfate solution 100ml identical, add FeCl with example 1 2.4H 2O 60g is through dissolving, the freezing FeSO that separates out that removes 4.7H 2O adds 6% crystal seeds of rutile, and heating hydrolysis becomes metatitanic acid.The metatitanic acid that generates is washed down, dries, add the ZnO.MgO crystal type promoting reagent each 1%, place to be warming up to 750 ℃ in the retort furnace, and be incubated 10 hours, gained titanium dioxide rutile content is that 100%(sees Fig. 4).
Example 5
Get the metatitanic acid of handling well that makes with example 1 same procedure, add crystal type promoting reagent ZnO, MgO each 1%, and grind to be mixed to be placed on and be warming up to 800 ℃ in the retort furnace, and be incubated 6 hours, gained titanium dioxide rutile content is 100%.(see figure 3)

Claims (2)

1, the metatitanic acid that obtains from hydrolysising titanium salt of a kind of calcining prepares the method for rutile titanium dioxide, the invention is characterized in to decompose in the titanyl sulfate solution of the removal of impurities that ilmenite obtains and introduce a certain amount of iron protochloride with sulfuric acid, add the crystal seeds of rutile that accounts for solution total amount 1-6% again, after the metatitanic acid that heating hydrolysis makes passes through washing, removal of impurities, drying, grinding again, adding (perhaps not adding) crystal type promoting reagent ZnO.MgO respectively 1% is mixed, calcining is 6-10 hour in 750-850 ℃ of temperature range, makes rutile titanium dioxide.
2,, it is characterized in that the weight ratio of the iron protochloride introduced is TiO according to the preparation method of the said rutile titanium dioxide of claim 1 2: FeCl 2.4H 2O=1: between the 0.97-3.88 scope.
CN 91108973 1991-09-14 1991-09-14 Preparation of rutile-type titanium dioxide by using of ferrous chloride Expired - Fee Related CN1029466C (en)

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CN 91108973 CN1029466C (en) 1991-09-14 1991-09-14 Preparation of rutile-type titanium dioxide by using of ferrous chloride

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Application Number Priority Date Filing Date Title
CN 91108973 CN1029466C (en) 1991-09-14 1991-09-14 Preparation of rutile-type titanium dioxide by using of ferrous chloride

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CN1071145A true CN1071145A (en) 1993-04-21
CN1029466C CN1029466C (en) 1995-08-09

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100368302C (en) * 2006-02-22 2008-02-13 攀钢集团攀枝花钢铁研究院 Rutile-type titanium white and its prepn process
CN102145295A (en) * 2011-01-27 2011-08-10 攀枝花学院 Method for preparing doped porous titanium dioxide
CN115400754A (en) * 2021-05-28 2022-11-29 四川大学 Preparation of high-dispersion iron-based NH 3 Method for SCR denitration catalyst
CN115417451A (en) * 2022-10-24 2022-12-02 攀钢集团研究院有限公司 Method for preparing rutile titanium dioxide

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100368302C (en) * 2006-02-22 2008-02-13 攀钢集团攀枝花钢铁研究院 Rutile-type titanium white and its prepn process
CN102145295A (en) * 2011-01-27 2011-08-10 攀枝花学院 Method for preparing doped porous titanium dioxide
CN102145295B (en) * 2011-01-27 2012-10-17 攀枝花学院 Method for preparing doped porous titanium dioxide
CN115400754A (en) * 2021-05-28 2022-11-29 四川大学 Preparation of high-dispersion iron-based NH 3 Method for SCR denitration catalyst
CN115417451A (en) * 2022-10-24 2022-12-02 攀钢集团研究院有限公司 Method for preparing rutile titanium dioxide
CN115417451B (en) * 2022-10-24 2023-11-24 攀钢集团研究院有限公司 Process for preparing rutile titanium dioxide

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