CN106086478A - A kind of method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material - Google Patents
A kind of method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material Download PDFInfo
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- CN106086478A CN106086478A CN201610446708.9A CN201610446708A CN106086478A CN 106086478 A CN106086478 A CN 106086478A CN 201610446708 A CN201610446708 A CN 201610446708A CN 106086478 A CN106086478 A CN 106086478A
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- iron powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1209—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material, comprise the following steps: join reducing agent fixed carbon in the concentrated ilmenite of (1) Yunnan and add additive, binding agent and fully moisten mill and process and improve material activity；(2) pelletizing, oven drying at low temperature are made after profit mill；(3) dried pelletizing carries out solid state reduction；(4) the metallized pellet mill choosing obtained obtains reduced iron powder and tailings respectively；(5) reduced iron powder obtained adds a small amount of reducing agent moistening dries under cryogenic；Tailings oxygen pressure acidleach in autoclave pressure removes the impurity beyond titanium, improves grade of titanium dioxide in rich-titanium material.The present invention is from raw material to reduced iron powder and rich-titanium material, and the full Iron grade of reduced iron powder is more than 94%, and ferrum yield is more than 86%, and in rich-titanium material, content of titanium dioxide is more than 75%, and titanium yield is more than 88%.This technological process is simple, and low cost, environmental friendliness, prospects for commercial application is good.
Description
Technical field
The invention belongs to rare metal production technical field, be specifically related to one and utilize Yunnan ilmenite concentrate to produce reduction
The method of iron powder coproduction rich-titanium material.
Background technology
There is abundant ilmenite resource in Yunnan Province, in many counties and cities as rich people, Lu advise, Lufeng, Wuding County, natural resources, Mouding,
Building the area such as water, Muller and have been found that the ilmenite resource that reserves are bigger, the mining of these resources is easy, and ore dressing is simple, produces into
This is relatively low.According to incompletely statistics, ilmenite exploitation is engaged in Yunnan and the producer managed is more, it has also become the titanium material that China is main
One of grown place.Additionally, Yunnan ilmenite is "dead", of high grade, iron titanium oxide total amount reaches 96 ~ 97% in ore deposit, non-ferra
Matter particularly sial impurity content is relatively low, and calcium and content of magnesium are low more than the sefstromite concentrate on the ground such as Flos Bombacis Malabarici and Chengde, and sulfur, phosphorus contain
Measuring the lowest, Yunnan ilmenite concentrate is a kind of quality raw materials first-selection producing titanium white and high titanium slag.
At present, the route that Yunnan concentrated ilmenite uses is generally Production By Sulfuric Acid Process titanium white, electro-smelting production titanium slag etc. two
Plant main method.Wherein there is the problems such as seriously polluted, cost is high, resource utilization is low in Production By Sulfuric Acid Process titanium white；Electric furnace refines
, there is power consumption height, high in cost of production problem in titanium slag.Existing method is as follows:
To sum up, Yunnan concentrated ilmenite uses dispensing profit mill, briquetting, cold drying, solid state reduction, mill choosing to obtain iron powder and tail respectively
Slag, iron powder cold drying, tailings pressure leaching obtain rich-titanium material.At inspection information, the method shows that there is not been reported.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material.
The object of the present invention is achieved like this, comprises the following steps:
(1) join in the concentrated ilmenite of Yunnan reducing agent fixed carbon and add additive, binding agent fully moisten mill process improve material live
Property；
(2) pelletizing, oven drying at low temperature are made after profit mill；
(3) dried pelletizing carries out solid state reduction；
(4) the metallized pellet mill choosing obtained obtains reduced iron powder and tailings respectively；
(5) reduced iron powder obtained adds a small amount of reducing agent moistening dries under cryogenic；Tailings is the acidleach of oxygen pressure in autoclave pressure
Remove the impurity beyond titanium, improve grade of titanium dioxide in rich-titanium material.
The present invention is from raw material to reduced iron powder and rich-titanium material, and the full Iron grade of reduced iron powder is more than 94%, and ferrum yield is more than 86%,
In rich-titanium material, content of titanium dioxide is more than 75%, and titanium yield is more than 88%.This technological process is simple, and ferrotianium is utilized effectively, also
Former iron powder can be used for the reducing agent of hydrometallurgy, and rich-titanium material can be as producing titanium white chloride raw material, low cost, environmental friendliness, work
Industry application prospect is good.
Advantages of the present invention essentially consists in:
(1) dispensing profit mill, briquetting, cold drying, it is to avoid activity disappears；
(2) mill choosing have employed rotary spiral chute, substantially increases reduced iron powder quality and yield；
(2) reduced iron powder uses and adds reducing agent and avoid secondary oxidation in cold drying；
(3) tailings uses pressurized acid leaching remove impurity to obtain high-grade rich-titanium material.
Accompanying drawing explanation
Fig. 1 is present invention process flow chart.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but is any limitation as the present invention never in any form,
Based on present invention teach that any conversion or improvement made, each fall within protection scope of the present invention.
Method of the present invention comprises the following steps:
(1) join in the concentrated ilmenite of Yunnan reducing agent fixed carbon and add additive, binding agent fully moisten mill process improve material live
Property；
(2) pelletizing, oven drying at low temperature are made after profit mill；
(3) dried pelletizing carries out solid state reduction；
(4) the metallized pellet mill choosing obtained obtains reduced iron powder and tailings respectively；
(5) reduced iron powder obtained adds a small amount of reducing agent moistening dries under cryogenic；Tailings is the acidleach of oxygen pressure in autoclave pressure
Remove the impurity beyond titanium, improve grade of titanium dioxide in rich-titanium material.
Step (1) will join reducing agent fixed carbon and additional additive, binding agent fully moisten mill and process in the concentrated ilmenite of Yunnan
Improving material activity, wherein profit mill equipment is planetary ball mill, tumbling ball mill or kolleroang, and additive is lithium carbonate, carbonic acid
One or more in sodium, sodium hydroxide.
Making pelletizing, oven drying at low temperature after step (2) profit mill, wherein cold drying is vacuum drying, and temperature is 50-80 DEG C.
Step (3) dried pelletizing carries out solid state reduction, and reduction temperature is 1100 ~ 1200 DEG C, recovery time 1-5h.
Mill optional equipment in step (4) is shaking table, magnetic separator or rotary spiral chute.
In step (5), reducing agent is one or more in hydrazine hydrate, sodium borohydride, sodium sulfite.
In the pressure acidleach of step (6) oxygen, acid is sulphuric acid or hydrochloric acid, and pressure 0.8 ~ 1.6MPa, temperature is 110 ~ 160 DEG C, and the time is
1~4h。
Embodiment 1
Condition: reducing agent is coke powder, reducing agent proportioning 7%, additive 6.0%, binding agent 1%, use planetary ball mill profit mill, system
Become pelletizing, at 60 DEG C of oven drying at low temperature 5h, reduction temperature 1180 DEG C, recovery time 3h；After reduction, logical protective atmosphere is cooled to room temperature,
Pulverize, carry out mill choosing, pulp density 60%, Ball-milling Time 2.0h, use magnetic separator magnetic separation, magnetic separation strength 800Oe, it is thus achieved that magnetic
Select iron powder and tailings；Iron powder adds employing hydrazine hydrate moistening 70 DEG C of dry 4h in a vacuum furnace, uses acid pressurization remove impurity, and technique is joined
Number: sulfuric acid concentration 10%, liquid-solid ratio 4:1, temperature are 120 DEG C, time 2h, oxygen pressure is 1.2MPa, mixing speed is 250rpm.?
Under these process conditions, the full ferrum of reduced iron powder is 95.12%, and in rich-titanium material, content of titanium dioxide is 76.14%.
Embodiment 2
Condition: reducing agent is coke powder, reducing agent proportioning 7%, sodium hydroxide 8.0%, binding agent 1%, use planetary ball mill profit mill,
Make pelletizing, at 80 DEG C of oven drying at low temperature 3h, reduction temperature 1150 DEG C, recovery time 3h；After reduction, logical protective atmosphere is cooled to room
Temperature, pulverizes, and carries out mill choosing, pulp density 60%, Ball-milling Time 2.0h, uses rotary spiral chute to carry out gravity treatment, it is thus achieved that also
Former iron powder and tailings；Iron powder adds employing sodium borohydride moistening 60 DEG C of dry 4h in a vacuum furnace, the pressurization remove impurity of tailings acid adding, technique
Parameter: sulfuric acid concentration 15%, liquid-solid ratio 4:1, temperature are 130 DEG C, time 2h, oxygen pressure is 1.5MPa, mixing speed is 250rpm.
Under these process conditions, the full ferrum of reduced iron powder is 96.18%, and in rich-titanium material, content of titanium dioxide is 77.01%.
Embodiment 3
Condition: reducing agent is coke powder, reducing agent proportioning 10%, sodium carbonate 8.0%, binding agent 1%, use tumbling ball mill profit mill, system
Become pelletizing, at 80 DEG C of oven drying at low temperature 3h, reduction temperature 1170 DEG C, recovery time 3h；After reduction, logical protective atmosphere is cooled to room temperature,
Pulverize, carry out mill choosing, pulp density 60%, Ball-milling Time 2.0h, use rotary spiral chute carry out gravity treatment, it is thus achieved that reduction
Iron powder and tailings；Iron powder adds employing sodium sulfite moistening 60 DEG C of dry 4h in a vacuum furnace, and the pressurization remove impurity of tailings acid adding, technique is joined
Number: concentration of hydrochloric acid 8%, liquid-solid ratio 5:1, temperature are 130 DEG C, time 2h, oxygen pressure is 1.4MPa, mixing speed is 250rpm.At this
Under process conditions, the full ferrum of reduced iron powder is 96.33%, and in rich-titanium material, content of titanium dioxide is 77.32%.
Embodiment 4
Condition: reducing agent is coke powder, reducing agent proportioning 8%, sodium carbonate 5.0%, sodium hydroxide 4%, binding agent 1%, use kolleroang
Profit mill, makes pelletizing, at 70 DEG C of oven drying at low temperature 3h, reduction temperature 1180 DEG C, recovery time 3h；Logical protective atmosphere cooling after reduction
To room temperature, pulverize, carry out mill choosing, pulp density 60%, Ball-milling Time 2.0h, use rotary spiral chute to carry out gravity treatment, it is thus achieved that
Reduced iron powder and tailings；Iron powder add employing sodium sulfite moistening 60 DEG C of dry 4h in a vacuum furnace, tailings acid adding pressurization remove impurity,
Technological parameter: concentration of hydrochloric acid 12%, liquid-solid ratio 4:1, temperature are 140 DEG C, time 2h, oxygen pressure is 1.6MPa, mixing speed is
250rpm.Under these process conditions, the full ferrum of reduced iron powder is 95.13%, and in rich-titanium material, content of titanium dioxide is 77.71%.
Embodiment 5
Condition: reducing agent is coke powder, reducing agent proportioning 11%, lithium carbonate 0.5%, sodium carbonate 6%, binding agent 1%, use roller ball mill
Machine profit mill, makes pelletizing, at 70 DEG C of oven drying at low temperature 3h, reduction temperature 1200 DEG C, recovery time 3h；After reduction, logical protective atmosphere is cold
But arriving room temperature, pulverize, carry out mill choosing, pulp density 60%, Ball-milling Time 2.0h, first use magnetic separator sorting, magnetic separation strength is
600Oe, magnetic concentrate uses rotary spiral chute to carry out gravity treatment again, it is thus achieved that reduced iron powder and tailings；Iron powder adds employing water
Closing hydrazine moistening 60 DEG C of dry 4h in a vacuum furnace, magnetic separation tailings and gravity treatment tailings merge into final tailings, and tailings uses acid adding to add
Pressure remove impurity, technological parameter: concentration of hydrochloric acid 10%, liquid-solid ratio 4:1, temperature are 140 DEG C, time 3h, oxygen pressure is 1.6MPa, stirring speed
Degree is 250rpm.Under these process conditions, the full ferrum of reduced iron powder is 96.77%, and in rich-titanium material, content of titanium dioxide is 77.35%.
Claims (7)
1. one kind utilizes the method that Yunnan ilmenite concentrate produces reduced iron powder coproduction rich-titanium material, it is characterised in that include following step
Rapid:
(1) join in the concentrated ilmenite of Yunnan reducing agent fixed carbon and add additive, binding agent fully moisten mill process improve material live
Property；
(2) pelletizing, oven drying at low temperature are made after profit mill；
(3) dried pelletizing carries out solid state reduction；
(4) the metallized pellet mill choosing obtained obtains reduced iron powder and tailings respectively；
(5) reduced iron powder obtained adds a small amount of reducing agent moistening dries under cryogenic；Tailings is the acidleach of oxygen pressure in autoclave pressure
Remove the impurity beyond titanium, improve grade of titanium dioxide in rich-titanium material.
The method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material the most according to claim 1, it is special
Levy and be that step (1) will join reducing agent fixed carbon and additional additive, binding agent fully moisten mill and process and carry in the concentrated ilmenite of Yunnan
High material activity, wherein profit mill equipment be planetary ball mill, tumbling ball mill or kolleroang, additive be lithium carbonate, sodium carbonate,
One or more in sodium hydroxide.
The method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material the most according to claim 1, it is special
Levying and make pelletizing after being step (2) profit mill, oven drying at low temperature, wherein cold drying is vacuum drying, and temperature is 50-80 DEG C.
The method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material the most according to claim 1, it is special
Levying and be that step (3) dried pelletizing carries out solid state reduction, reduction temperature is 1100 ~ 1200 DEG C, recovery time 1-5h.
The method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material the most according to claim 1, it is special
Levying the mill optional equipment being in step (4) is shaking table, magnetic separator or rotary spiral chute.
The method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material the most according to claim 1, it is special
Levy and be in step (5) that reducing agent is one or more in hydrazine hydrate, sodium borohydride, sodium sulfite.
The method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material the most according to claim 1, it is special
Levy and be that in the pressure acidleach of step (6) oxygen, acid is for sulphuric acid or hydrochloric acid, pressure 0.8 ~ 1.6MPa, temperature is 110 ~ 160 DEG C, the time is 1 ~
4h。
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| CN201610446708.9A CN106086478A (en) | 2016-06-21 | 2016-06-21 | A kind of method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110735032A (en) * | 2019-09-03 | 2020-01-31 | 昆明禾丰环境研究所 | vanadium-titanium-iron paragenetic ore treatment process |
| CN115532169A (en) * | 2022-10-13 | 2022-12-30 | 成都天屿新磷科技有限公司 | Method and system for preparing special pellets for yellow phosphorus by enriching ground phosphate rock |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110735032A (en) * | 2019-09-03 | 2020-01-31 | 昆明禾丰环境研究所 | vanadium-titanium-iron paragenetic ore treatment process |
| CN110735032B (en) * | 2019-09-03 | 2021-04-06 | 昆明禾丰环境研究所 | Vanadium-titanium-iron paragenetic ore treatment process |
| CN115532169A (en) * | 2022-10-13 | 2022-12-30 | 成都天屿新磷科技有限公司 | Method and system for preparing special pellets for yellow phosphorus by enriching ground phosphate rock |
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Application publication date: 20161109 |