CN1217298A

CN1217298A - Preparation of titanic-schorl type titanium white by hydrochloric -acid process

Info

Publication number: CN1217298A
Application number: CN 98113128
Authority: CN
Inventors: 谢亚汉; 谢炳元; 刘朴衡; 谢晓芳; 高国威
Original assignee: HUACHANG SCIENCE AND TECHNOLOGY DEVELOPMENT Co Ltd GUANGZHOU CITY
Current assignee: HUACHANG SCIENCE AND TECHNOLOGY DEVELOPMENT Co Ltd GUANGZHOU CITY
Priority date: 1998-02-24
Filing date: 1998-02-24
Publication date: 1999-05-26
Anticipated expiration: 2018-02-24
Also published as: CN1079374C

Abstract

The preparation method of rutile-type titanium white by using hydrochloric acid process includes the following steps: adding dilute hydrochloric acid in acid-resistant reaction still; in the presence of metatitanic acid hydrolytic seed crystal, simultaneously adding pulverized iserite and reduction agent; keeping temp. at 108-110 deg.C, and in all the processes of iserite decomposition and metatitanic acid hydrolysis, retaining the presence of micro quantity of reduction agent; after the decomposition and hydrolysis are completed, filtering and separating the metatitanic acid from mother liquor, and water-washing metatitanic acid; adopting gravity separation method to separate out the layer grain-size undecomposed mineral material from the metatitanic acid; then adding HF to remove SiO2 from metatitanic acid; bleaching metatitanic acid and making salt treatment, and calcining at 850-900 deg.C to obtain the invented product.

Description

Preparation of titanic-schorl type titanium white by hydrochloric-acid process

The invention belongs to the production method of titanium dioxide

In the reactor of salt tolerant acid, add dilute hydrochloric acid, in stirring, add metatitanic acid hydrolysis crystal seed (automatic growing crystal species), at a certain temperature, add reductive agent and ilmenite simultaneously through pulverizing.Ilmenite constantly is decomposed and the continuous hydrolysis of metatitanic acid, and in whole decomposition and hydrolytic process, reductive agent constantly is consumed, and needs constantly to replenish.The existence that in entire reaction course, must keep micro-reductive agent.After ilmenite decomposition and metatitanic acid hydrolysis end, after filtration, will contain chlorination ferrous spent acid mother liquor separately.Metatitanic acid is removed remaining iron protochloride through washing.It is thick slightly to isolate granularity through gravity concentration from metatitanic acid, the undecomposed mineral that proportion is big slightly.According to SiO in the metatitanic acid ₂Content add the HF of respective amount, will generate corresponding SiF ₄Gas and with SiO ₂Remove.Through routine bleaching with carry out salt according to different requirements and handle, produce the commodity Rutile type Titanium Dioxide through surface treatment and pulverizing more then then 850-900 ℃ of calcining.Iron protochloride spent acid mother liquor can adopt torch firing regeneration hydrochloric acid and ferric oxide, and regeneration hydrochloric acid retrieval system is decomposed ilmenite, and ferric oxide can be made the iron oxide pigment of low gear, and iron protochloride spent acid mother liquor also can be produced the raw material { 1} of red iron oxide as wet method.The surface treatment of iron protochloride spent acid mother liquor and titanium dioxide all has sophisticated technology, not at the row of the research of this paper.

Example: in the reactor of salt tolerant acid, add 19% dilute hydrochloric acid, when being raised to 100 ℃, temperature adds metatitanic acid hydrolysis crystal, add simultaneously through the ilmenite of pulverizing and the chloride soln of low price titanium, temperature maintains 108-110 ℃ always then, in the whole process of ilmenite decomposition and metatitanic acid hydrolysis, remaining at a low price, the content of titanium is that 0.3-0.5g/g decomposed in about 6 hours and hydrolysis finishes.Filtration separates metatitanic acid with iron protochloride spent acid mother liquor.Metatitanic acid is washed, and adopts the shale shaking table that the thick slightly big slightly undecomposed mineral of proportion of the granularity in the metatitanic acid are separated.After the metatitanic acid slurrying, according to SiO in the metatitanic acid ₂Content adds an amount of HF with SiO ₂Remove.Bleaching and salt are handled then, 850-900 ℃ of calcining about 1 hour, obtain not surface treated Rutile type Titanium Dioxide at last, and whiteness is near the Rutile type Titanium Dioxide of inward.

{ the technology CN85-105994 technical process of 1} Xie Yahan production of iron red product from iron-containing waste liquid sees that the hydrochloric acid legal system gets rutile titanium white powder craft general flow chart to reference.

Claims

1: it is characterized in that salt tolerant acid has in the reactor of stirring, add dilute hydrochloric acid, in the presence of the metatitanic acid hydrolysis crystal seed, be warmed up to certain temperature, add reductive agent and ilmenite simultaneously through pulverizing.Hydrolysis simultaneously went out metatitanic acid when hydrochloric acid decomposed ilmenite.In the process of continuous decomposition of ilmenite and metatitanic acid hydrolysis, reductive agent constantly consumes the existence that must constantly replenish and keep micro-reductive agent in whole process.When ilmenite decomposes and the metatitanic acid hydrolysis finishes, after filtration metatitanic acid is separated with iron protochloride spent acid mother liquor.Metatitanic acid adopts gravity concentration that the big slightly undecomposed mineral of the thick slightly proportion of contained granularity in the metatitanic acid are separated after washing.Then will be according to SiO in the metatitanic acid ₂Content add HF and remove SiO ₂Then through routine bleaching with carry out salt according to different requirements and handle, 850-900 ℃ of calcining about 1 hour, obtain not surface treated Rutile type Titanium Dioxide at last, whiteness near or suitable inward Rutile type Titanium Dioxide.

2: the reductive agent of indication in the technology is characterized in that referring to the ferric iron in the solution can be reduced to ferrous material immediately, as the muriate of titanous or the vitriol of titanous etc.

3: the gravity beneficiation equipment of indication in the technology is characterized in that referring to that the mineral that the are not decomposed granularity in the metatitanic acid is thick slightly and that proportion is big slightly separate, as hydrocyclone and shale shaking table.