CN109987589A - Utilize the method for ferric trichloride concentration titanium white waste acid - Google Patents

Utilize the method for ferric trichloride concentration titanium white waste acid Download PDF

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Publication number
CN109987589A
CN109987589A CN201910334716.8A CN201910334716A CN109987589A CN 109987589 A CN109987589 A CN 109987589A CN 201910334716 A CN201910334716 A CN 201910334716A CN 109987589 A CN109987589 A CN 109987589A
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China
Prior art keywords
titanium white
waste acid
white waste
ferric trichloride
concentration
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Application number
CN201910334716.8A
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Chinese (zh)
Inventor
穆宏波
穆天柱
邓斌
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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Priority to CN201910334716.8A priority Critical patent/CN109987589A/en
Publication of CN109987589A publication Critical patent/CN109987589A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/69Sulfur trioxide; Sulfuric acid
    • C01B17/88Concentration of sulfuric acid

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of methods using ferric trichloride concentration titanium white waste acid, belong to chemical field, the following steps are included: titanium white waste acid and ferric trichloride are respectively placed in same closed container, the sulfuric acid for being 50~55% to get mass percentage concentration after the completion of to be concentrated.The method of the present invention completely avoids the use of boiler and evaporator, avoid the use of expensive resistant material, to reduce production cost, and operation it is at normal temperature or slightly hot under conditions of carry out, operating condition is significantly improved in this way, but also the economy of titanium white waste acid concentration is improved.

Description

Utilize the method for ferric trichloride concentration titanium white waste acid
Technical field
The invention belongs to chemical fields, and in particular to a method of titanium white waste acid is concentrated using ferric trichloride.
Background technique
Titanium White Production By Sulfuric Acid Process will generate Waste Sulfuric Acid (abbreviation titanium white waste acid) and the green vitriol containing 7 crystallizations water (FeSO4·7H2O), when using ilmenite concentrate, (main component is metatitanic acid iron FeTiO3, wherein TiO2Content be 45-50wt%) be When raw material, 1 ton of titanium dioxide is generally produced by seven inkstone of output 3.5-4 ton, while generating 7~8 tons and containing 17~20% sulfuric acid Titanium white waste acid.
Due to too big using the waste sulfuric acid solution quantum of output of method for producing gtitanium dioxide with sulphuric acid by-product, and contain a certain amount of sulphur It is sour ferrous, so that this waste sulfuric acid solution can not be utilized in other fields using dilute sulfuric acid.Lime is generallyd use at present In stone and generate calcium sulfate method titanium white waste acid is handled, however, obtained calcium sulfate there is no utility value and can only Stockpiling, this does not utilize raw material not only well, but also biggish pressure can be caused to environment.Positive method is first to lead to When crossing preliminary evaporation and concentration and improving the mass percentage concentration of sulfuric acid to 30%~40%, ferrous sulfate is isolated;Further Evaporation and concentration becomes 50% or more sulfuric acid, returns to acidolysis operation, uses for continuous acidolysis, to completely be utilized.But It is that the corrosivity of sulfuric acid solution at high temperature is extremely strong, it is desirable that be worth higher graphite material, while being concentrated by evaporation and needing large capacity Steam boiler so that the equipment investment of this method is high and production cost is also high.
Summary of the invention
The technical problem to be solved by the present invention is to it is existing concentration titanium white waste acid method it is big to equipment corrosion, it is at high cost.
The technical solution of present invention solution above-mentioned technical problem are as follows: provide a kind of utilization ferric trichloride concentration titanium white waste acid Method, comprising the following steps: titanium white waste acid and ferric trichloride are respectively placed in same closed container, after the completion of to be concentrated, The sulfuric acid for being 50~55% up to mass percentage concentration.
Wherein, the above-mentioned method using ferric trichloride concentration titanium white waste acid, the quality percentage of sulfuric acid in the titanium white waste acid Concentration is 17~20%.
Wherein, it is above-mentioned using ferric trichloride concentration titanium white waste acid method, the ferric trichloride be two aqueous ferric chlorides or Four aqueous ferric chlorides.
Wherein, the above-mentioned method stated using ferric trichloride concentration titanium white waste acid, the matter of the titanium white waste acid and ferric trichloride Amount is than being 1:1.66~10.
Wherein, the above-mentioned method using ferric trichloride concentration titanium white waste acid, the quality of the titanium white waste acid and ferric trichloride Than for 1:1.66~5.
Wherein, the above-mentioned method using ferric trichloride concentration titanium white waste acid, the temperature of the concentration are 10~38 DEG C.
Wherein, the above-mentioned method using ferric trichloride concentration titanium white waste acid, the time of the concentration are 3~7 days.
Compared with prior art, the beneficial effects of the present invention are:
The method of the present invention completely avoids the use of boiler and evaporator, avoids the use of expensive resistant material, To reduce production cost, and operate it is at normal temperature or slightly hot under conditions of carry out, significantly improve work in this way Condition, but also the economy of titanium white waste acid concentration is improved.
The raw material ferric trichloride that the present invention uses can recycle, and greatly reduce the cost of raw material.
Specific embodiment
Specifically, a kind of method using ferric trichloride concentration titanium white waste acid, comprising the following steps: by titanium white waste acid and three Iron chloride is respectively placed in same closed container, the sulfuric acid for being 50~55% to get mass percentage concentration after the completion of to be concentrated.
The mass percentage concentration of sulfuric acid is 17~20% in titanium white waste acid used in the method for the present invention.
In method of the invention, in the method for the present invention, ferric trichloride selection has hygroscopic two aqueous ferric chloride or four Better two aqueous ferric chloride of aqueous ferric chloride, preferably hygroscopicity.
In the method for the present invention, the dosage of ferric trichloride and the time of concentration are to be mutually related: the dosage of ferric trichloride is more, Then concentration time is short, and the dosage of ferric trichloride is few, then the time being concentrated is short.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention System is among the embodiment described range.
Embodiment 1
By 100 grams of Waste Sulfuric Acids, wherein the ferrous sulfate of sulfuric acid and 2~3wt% containing 20wt%.With 166 gram of two water trichlorine Change iron (FeCl3·2H2O it) is respectively placed in same closed container at normal temperature, (notices that two kinds of materials are separated, cannot mix It closes).Two kinds of materials are taken out after 7 days, liquid is the sulfuric acid of 50~55wt%, and solid is ferric chloride (FeCl36H2O) (FeCl3·6H2O), FeCl3·6H2The removing crystallization water is dried at 100~150 DEG C in O, becomes FeCl3·2H2O, which is returned, to be used.50~55wt%'s Sulfuric acid can return to acidolysis and use for continuous acidolysis.
Embodiment 2
By 100 grams of Waste Sulfuric Acids, wherein the ferrous sulfate of sulfuric acid and 2~3wt% containing 20wt%.With 332 gram of two water trichlorine Change iron (FeCl3·2H2O it) is respectively placed in same closed container at normal temperature, (notices that two kinds of materials are separated, cannot mix It closes).Two kinds of materials are taken out after 3.5 days, liquid is the sulfuric acid of 50~55wt%, and solid is four aqueous ferric chloride (FeCl3· 4H2O), FeCl3·4H2The removing crystallization water is dried at 100~150 DEG C in O, becomes FeCl3·2H2O, which is returned, to be used.50~ The sulfuric acid of 55wt% can return to acidolysis and use for continuous acidolysis.
Embodiment 3
In order to improve FeCl3·2H2The utilization rate of O can use the mode of operation of " adverse current ".
By the finally obtained solid phase FeCl of embodiment 23·4H2O continues to put respectively at normal temperature with 100 grams of new Waste Sulfuric Acids It is placed in same closed container, (notice that two kinds of materials are separated, cannot mix).Two kinds of materials are taken out after 7 days, liquid is The sulfuric acid of 50wt%, solid are ferric chloride (FeCl36H2O) (FeCl3·6H2O), the removing crystallization water is dried at 100~150 DEG C, Become FeCl3·2H2O, which is returned, to be used.
The sulfuric acid of 50wt% continues and FeCl3·2H2O is respectively placed at normal temperature in same closed container, (pays attention to two Kind material is separated, cannot mix).Two kinds of materials are taken out after 3.5 days, liquid is the sulfuric acid of 55wt%, returns to acidolysis for even Continuous acidolysis uses;Solid phase ferric trichloride still has the space of water suction, continues to act on new Waste Sulfuric Acid, until it is saturated and becomes FeCl3·6H2O is dried the removing crystallization water at 100~150 DEG C, becomes FeCl3·2H2O, which is returned, to be used;Liquid phase continues With new FeCl3·2H2O effect, until liquid concentration reaches 55wt% and stops.

Claims (7)

1. utilizing the method for ferric trichloride concentration titanium white waste acid, which comprises the following steps: by titanium white waste acid and trichlorine Change iron to be respectively placed in same closed container, the sulfuric acid for being 50~55% to get mass percentage concentration after the completion of to be concentrated.
2. utilizing the method for ferric trichloride concentration titanium white waste acid according to claim 1, it is characterised in that: the titanium white waste acid The mass percentage concentration of middle sulfuric acid is 17~20%.
3. utilizing the method for ferric trichloride concentration titanium white waste acid according to claim 1, it is characterised in that: the ferric trichloride For two aqueous ferric chlorides or four aqueous ferric chlorides.
4. utilizing the method for ferric trichloride concentration titanium white waste acid according to claim 1, it is characterised in that: the titanium white waste acid Mass ratio with ferric trichloride is 1:1.66~10.
5. utilizing the method for ferric trichloride concentration titanium white waste acid according to claim 4, it is characterised in that: the titanium white waste acid Mass ratio with ferric trichloride is 1:1.66~5.
6. utilizing the method for ferric trichloride concentration titanium white waste acid according to claim 1, it is characterised in that: the temperature of the concentration Degree is 10~38 DEG C.
7. according to claim 1 using ferric trichloride concentration titanium white waste acid method, it is characterised in that: the concentration when Between be 3~7 days.
CN201910334716.8A 2019-04-24 2019-04-24 Utilize the method for ferric trichloride concentration titanium white waste acid Withdrawn CN109987589A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004137118A (en) * 2002-10-18 2004-05-13 Galva Kogyo Mihara Kojo:Kk Method for recovering hydrochloric acid from waste iron-hydrochloric acid treatment liquid
CN1540036A (en) * 2003-04-23 2004-10-27 上海新芝电子有限公司 Method for regenerating etching waste fluid of iron protochloride of containing nickel
CN1566401A (en) * 2003-06-29 2005-01-19 上海新芝电子有限公司 Regeneration method for ferric chloride etching solution containing nickel
WO2011147426A1 (en) * 2010-05-24 2011-12-01 Mohammed Mohammed Mohammed Saad A process of production of concentrated ferric chloride solution from the waste hydrochloric acid pickle liquor
CN102910594A (en) * 2012-11-06 2013-02-06 黄正源 Method for concentrating waste sulfuric acid by utilizing waste heat of titanium dioxide calcinator
CN102923877A (en) * 2012-10-19 2013-02-13 常州北化智合化工工程技术有限公司 Treatment technology for mirabilite tailing wastewater
CN108275727A (en) * 2018-02-07 2018-07-13 宁波天大工程设计有限公司 A kind of spent acid treatment process and equipment

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004137118A (en) * 2002-10-18 2004-05-13 Galva Kogyo Mihara Kojo:Kk Method for recovering hydrochloric acid from waste iron-hydrochloric acid treatment liquid
CN1540036A (en) * 2003-04-23 2004-10-27 上海新芝电子有限公司 Method for regenerating etching waste fluid of iron protochloride of containing nickel
CN1566401A (en) * 2003-06-29 2005-01-19 上海新芝电子有限公司 Regeneration method for ferric chloride etching solution containing nickel
WO2011147426A1 (en) * 2010-05-24 2011-12-01 Mohammed Mohammed Mohammed Saad A process of production of concentrated ferric chloride solution from the waste hydrochloric acid pickle liquor
CN102923877A (en) * 2012-10-19 2013-02-13 常州北化智合化工工程技术有限公司 Treatment technology for mirabilite tailing wastewater
CN102910594A (en) * 2012-11-06 2013-02-06 黄正源 Method for concentrating waste sulfuric acid by utilizing waste heat of titanium dioxide calcinator
CN108275727A (en) * 2018-02-07 2018-07-13 宁波天大工程设计有限公司 A kind of spent acid treatment process and equipment

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
化学工业部天津化工研究院等编: "《化工产品手册》", 31 August 1983 *

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Application publication date: 20190709