CN1104999A

CN1104999A - Purified technology for ferrous sulfate of titanium white powder by-product

Info

Publication number: CN1104999A
Application number: CN 94105891
Authority: CN
Inventors: 王汉栋; 王学钦; 张永宏; 赵建国; 余武; 贾金平
Original assignee: YANGQUAN CITY MAGNETIC POWDER ENGINEERING PREPARING DEPT SHANXI PROV
Current assignee: YANGQUAN CITY MAGNETIC POWDER ENGINEERING PREPARING DEPT SHANXI PROV
Priority date: 1994-06-01
Filing date: 1994-06-01
Publication date: 1995-07-12

Abstract

The process for refining ferrous sulfate as by-product in production of titanium white powder includes such seps as hydrolysis, reduction and flocculation. The refined product has purity of ov er 99% and titanium content is 3.9 ppm (in 20% Fe account). The contents of other metals, non-metals and compounds are obviously reduced. The product may be directly used to make magnetic powder, high-purity iron oxide and others fields.

Description

Purified technology for ferrous sulfate of titanium white powder by-product

The invention belongs to the processing of titanium and compound thereof, be specifically related to a kind of refining purifying technique of byproduct ferrous sulfate of titanium dioxide.

The by-product ferrous sulfate during of production process of titanium pigment, its foreign matter content are between 25-10%, and wherein major part is titanium and compound thereof, free acid, water etc.Ferrous sulfate is again starting material of producing magnetic, high purity ferric oxide.Because magnetic, ferric oxide are very high to the purity requirement of raw material.Therefore byproduct ferrous sulfate of titanium dioxide needs to purify through refining.In the known technology, as Wuhan 824 factories acidleach purification process, removing the titanium result is 161PPm, and the clearance of other impurity is also undesirable, and the rate of recovery is low.The technical process of the purification titanium dioxide ferrous sulfate that Chemical Co., Ltd of Japanese for another example kingdom proposes promptly in copperas solution, adds alkali the titanium hydrolysis is separated out, and its technology needs through tens of refining repeatedly purifications.

The object of the present invention is to provide a kind of technology simple, refining effect is remarkable, the process for refining of the byproduct ferrous sulfate of titanium dioxide of turning waste into wealth.

Design of the present invention is based on such principle.Utilize Tl ⁴⁺Easily hydrolysis and generate the mechanism of insoluble titanium compound, under the certain temperature condition, insoluble titanium compound is separated out in hydrolysis, adds an amount of clean reduced iron powder simultaneously with reduction Fe wherein ³⁺With displace the part metals particle, as Pb ²⁺, Cu ²⁺, Nl ²⁺Deng.Along with iron powder consumes H in the solution ⁺Ion, pH value raises, when rising to certain value, termination reaction.Add treatment agent again and carry out sedimentation, filtration.

The present invention takes following technical scheme.

Process for refining follows these steps to carry out in turn.

With byproduct ferrous sulfate of titanium dioxide, hot water, in 0.8(kg): ratio 1(L) adds retort intensification stirring and dissolving successively, adds reduced iron powder, continues to be heated to 55-80 ℃, keeps temperature 2-3 hour, and at this moment, following reaction mainly takes place solution:

Vitriolic consumption raises pH value, half an hour approximately when invariable to pH value, cooling solution, termination reaction.

Add after 1% flocculant solution stirs 2-5 minute by molten heavy 0.01-0.05%, sedimentation is filtered and is promptly got light blue or the transparent copperas solution of blue-greenish colour, and this solution can be directly used in magnetic and high purity ferric oxide production.If with the solution crystallisation by cooling, filtering separation can get the ferrous sulfate crystal, and mother liquor can be recycled, the FeSo of gained ₄Crystal is used for fields such as medicine, chemical reagent.

Technological process of the present invention is simple, and refining effect is splendid, and it is as follows that simultaneous test detects data:

NO??Fe%??Ti??Zn??Mg??Ca??Mn??Si??P??Al(ug/g)

Y-0??19.06??4359??42.3??33.2??219.5??1498??0.5??987.1??0.3

Y-1??18.77??3.7??13.5??35.6??453.6??494??4.3??690.2??0.9

Y-5??18.93??161??35.3??31.8??392.2??1151??1.1??791.8??84.4

Y-6??19.02??8277??6.9??0.5??89.3??75??5.1??800.3??0.7

NO??Ti??Zn??Mg??Ca??Mn??Si??P??Al??Cu??Cr(ug/ml)

Y-2?0.3?23.1?22.4??204.1??496.3??0.2??136.9??5.9??4.4??7.7

Y-3??0.3??22.7??15.7??142.1??473.6

Y-4??0.5??21.8??7.9??59.8??453.4??0.1??147.4??6.2

Wherein, Y-O distributes for the byproduct ferrous sulfate of titanium dioxide foreign matter content; Y-1 is the refining crystallization ferrous sulfate; Y-2, Y-3, Y-4 distribute for adopting this technology POV ferrous iron solution foreign matter content; Y-5 is for trying to such an extent that 824 factories acidleach purification process makes the distribution of ferrous sulfate foreign matter content;

Find out that from verification result titanium Impurity removal effect can reach 0.9Pm and 3.9PPm(in 20%Fe).Other foreign matter content also obviously reduces, and the product that make also can be used for the requirement of medicine and other fields not only with the production of the high purity ferric oxide that satisfies magnetic.

The whole less investment of technology, loss is low, turns waste into wealth, and has obvious social and economic benefit.

Below in conjunction with embodiment the solution of the present invention is further described.

With byproduct ferrous sulfate of titanium dioxide, hot water, in 1(kg): ratio 1.25(1) adds molten device intensification stirring and dissolving successively.Wherein vitriol oil concentration is the 98%(analytical pure).Add Fe greater than 95%, insolubles is less than 0.2%, and granularity is heated to 55-80 ° less than the reduced iron powder K of 0.06mm, is preferably 60-75 ℃, be incubated about 2-3 hour, arrives pH value and cools off when invariable.The 0.01-0.05% that presses the ferrous sulfate gross weight adds 1% flocculation agent, and for example poly-propionyl acid amides stirred 2-3 minute, carries out sedimentation, filters and promptly get copperas solution.Or with the solution crystallisation by cooling, filtering separation makes the ferrous sulfate crystal.

Claims

1, a kind of process for refining of byproduct ferrous sulfate of titanium dioxide is characterized in that process for refining carries out according to the following steps successively:

A, by-product of white titanium pigment hot water, ferrous sulfate are added container intensification stirring and dissolving successively in the ratio of 1: 1.25 (L); Add the vitriol oil, its add-on is decided on the pH value of solution, generally is controlled at about 2.0.

B, add reduced iron powder, be heated to 55-80 ℃, kept temperature 2-3 hour with the 0.5-1% of ferrous sulfate weight, to pH value when invariable, cooling;

C1, the 0.01-0.05% that presses the ferrous sulfate gross weight add 1% flocculation agent and stirred 2-5% minute, carry out sedimentation, filter and promptly get copperas solution;

Or

c ₂: with the solution crystallisation by cooling, filtering separation makes the ferrous sulfate crystal.

2, the process for refining of byproduct ferrous sulfate of titanium dioxide as claimed in claim 1 is characterized in that the vitriol oil concentration that reaction process adds is the 98%(analytical pure).

3, the process for refining of byproduct ferrous sulfate of titanium dioxide as claimed in claim 1, the specification that it is characterized in that the reduced iron powder that adds in the reaction process for (chemical pure) Fe greater than 95%, insolubles is less than 0.2%, granularity is less than 0.06mm.

4, the process for refining of byproduct ferrous sulfate of titanium dioxide as claimed in claim 1 is characterized in that the flocculation agent that adds can be polyacrylamide.

5,, it is characterized in that the foreign matter content of byproduct ferrous sulfate of titanium dioxide can reach 25%-10% as the process for refining of claim 1,2,3 or 4 described casting white powder by-product ferrous sulfate durings.