CN111744556B - Catalyst for accelerating reduction of titanium concentrate and preparation method thereof - Google Patents
Catalyst for accelerating reduction of titanium concentrate and preparation method thereof Download PDFInfo
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- C22B34/10—Obtaining titanium, zirconium or hafnium
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Abstract
The invention relates to a catalyst for accelerating the reduction of titanium concentrate and a preparation method thereof, belonging to the technical field of metallurgy. The catalyst for accelerating the reduction of the titanium concentrate comprises ferrous oxide, magnesium oxide, PVA, cyclic ester halide and coal; the mass ratio of the ferrous oxide to the magnesium oxide to the PVA to the cyclic ester halide is (2.5-3.5); the ferrous oxide: the mass ratio of the magnesium oxide is 4-7: 6 to 7; the mass ratio of the sum of the ferrous oxide, the magnesium oxide, the PVA and the cyclic ester halide to the coal is 400. The catalyst can accelerate the reaction efficiency and speed, and solves the problems of low reduction efficiency, large tailing amount and the like caused by fusion and agglomeration of the titanium concentrate in the reduction process in the prior art.
Description
Technical Field
The invention relates to a catalyst for accelerating the reduction of titanium concentrate and a preparation method thereof, belonging to the technical field of metallurgy.
Background
In the traditional process of ferrotitanium production, the contact area of titanium concentrate and a reducing agent is small, and the titanium concentrate is easy to melt and agglomerate in the reduction process, so that the reduction efficiency is low, and the tailings are large in quantity.
Zhang Kai titanium concentrate solid phase reduction strengthening method research [ D ]. Chongqing university, 2014 discloses that Panzhihua titanium concentrate is used as a research object, two experimental methods of isothermal reduction and non-isothermal reduction are adopted, the influence laws of two strengthening modes of mechanical activation and additive (catalyst) on the reduction process are respectively compared, and the catalyst is borax and sodium carbonate.
Research on the process and mechanism of preparing titanium-rich material by reduction-grinding method of titanium concentrate (Guoyupang, jiangzao, etc.) [ J ]]The 2008 non-blast furnace iron-making annual meeting collection of the Chinese society for metals, 2008, discloses a product titanium concentrate obtained by sorting vanadium titano-magnetite in Panxi area of China, and effective separation of Fe/Ti is realized by adopting a reduction-grinding separation method. Compared with the traditional methodCompared with the original grinding and selecting method, the novel process adopts the novel additive KS as a catalyst in the reduction process, so that the proper reduction temperature of the titanium concentrate is reduced to 1100 ℃ from the usual 1250-1280 ℃. The research on the mechanism shows that the additive KS has the function of strengthening solid phase diffusion and reducing impurity ions Mg in the titanium concentrate 2+ For Fe 2 TiO 5 The stabilizing effect of (1). The reduction of iron oxide in the titanium concentrate and the growth of metal iron grains can be realized at a lower temperature, and the grinding, separation and separation efficiency is improved.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a novel catalyst for accelerating the reduction of the titanium concentrate.
In order to solve the first technical problem, the catalyst for accelerating the reduction of the titanium concentrate comprises ferrous oxide, magnesium oxide, PVA, cyclic ester halide and coal; the mass ratio of the ferrous oxide to the magnesium oxide to the PVA to the cyclic ester halide is 2.5-3.5; the mass ratio of the sum of the masses of the ferrous oxide, the magnesium oxide, the PVA and the cyclic ester halide to the coal is 400.
In one embodiment, the cyclic ester halide is a cyclic ester chloride, a cyclic ester bromide, a cyclic ester iodide.
In one specific embodiment, the ferrous oxide and the magnesium oxide are prepared by the following method: mixing iron powder, magnesium powder and water according to the mass ratio of 5-8 ^-2 Pa, pumping dry air, cooling for 1-2 h, and grinding into powder with the particle size of 10-60 meshes.
In one embodiment, the PVA is prepared by the following process: stirring 100 volume parts of polyethylene with the polymerization degree of 500-2000 and the alcoholysis degree of 75-99 mo1% and 200-400 volume parts of mixed solvent of dimethyl sulfoxide and water at 80-120 ℃ and-0.01-0.08 MPa for 3-4 hours to obtain spinning solution, filtering, defoaming, spinning by dry-wet method and post-treating to obtain water-soluble polyvinyl alcohol, concentrating and drying to obtain PVA.
In one embodiment, the ratio of dimethylsulfoxide in the mixed solvent of dimethylsulfoxide/water: 70-90: 10-30 of water.
In one embodiment, the cyclic ester halide is a cyclic ester chloride.
In one embodiment, the cyclic ester chloride is prepared by the following method: reacting the cyclic ester with chlorine gas at 230-300 ℃ for 2-3 h to obtain cyclic ester chloride, and drying.
In one embodiment, the method for preparing the catalyst for accelerating the reduction of the titanium concentrate comprises the following steps: uniformly mixing ferrous oxide, magnesium oxide powder, PVA powder and cyclic ester chloride powder to obtain a mixture; and then mixing the mixture with the coal powder according to the mass ratio of 400:100, and drying for 0.5 to 1.5 hours at the temperature of between 100 and 120 ℃ to obtain a finished product.
The second technical problem to be solved by the invention is to provide a preparation method of the catalyst for accelerating the reduction of the titanium concentrate.
In order to solve the second technical problem of the present invention, the method for preparing the catalyst for accelerating the reduction of the titanium concentrate comprises:
A. the preparation of ferrous oxide and magnesium oxide powder is carried out by mixing iron powder, magnesium powder and water according to the mass ratio of 5-8 ^-2 Pa, pumping dry air, drying, cooling for 1-2 h, and grinding into powder with the granularity of 10-60 meshes;
B. preparing composite organic component powder PVA, namely stirring 100 parts of polyethylene with the polymerization degree of 500-2000 and the alcoholysis degree of 75-99 mo1% and 200-400 parts of mixed solvent of dimethyl sulfoxide and water at 80-120 ℃ and-0.01-0.08 MPa for 3-4 hours to obtain spinning solution, filtering, defoaming, spinning by a dry-wet method and post-treating to obtain water-soluble polyvinyl alcohol, concentrating and drying to obtain PVA;
C. preparing compound organic component powder, namely reacting cyclic ester with halogen to obtain cyclic ester chloride, and drying; preferably, the halogen is chlorine, and the reaction is carried out for 2 to 3 hours at a temperature of between 230 and 300 ℃;
D. mixing organic components and inorganic powder, namely uniformly mixing ferrous oxide, magnesium oxide powder, PVA powder and cyclic ester chloride powder to obtain a mixture; and then mixing the mixture with the coal powder according to the mass ratio of 400:100, and drying for 0.5 to 1.5 hours at the temperature of between 100 and 120 ℃ to obtain a finished product.
In one embodiment, the ratio of dimethylsulfoxide in the mixed solvent of dimethylsulfoxide/water: 70-90: 10-30 of water.
Has the beneficial effects that:
the catalyst can accelerate the reaction efficiency and speed, and solves the problems of low reduction efficiency, large tailing amount and the like caused by fusion and agglomeration of the titanium concentrate in the reduction process in the prior art.
The catalyst is a new high-efficiency metallurgical catalyst technology which is independently researched and developed, can efficiently modify and reduce the titanium concentrate and tailings after the titanium concentrate is smelted, provides an integral solution for improving the productivity, reducing the energy consumption, reducing the pollution and the like, breaks through the barrier of the traditional metallurgical production technology, effectively improves the utilization rate of raw materials, and is compared with the laggard technology, the catalyst product is prepared by the following steps: the requirements of high efficiency, high quality, low energy consumption and the like of production are really met.
The gas components generated by decomposition after the catalyst of the invention is added are reacted into the reaction among the raw material, the reducing gas and the coal powder, the reducing gas is uniformly diffused in the tailings and has high flowing speed, the reducing gas can permeate into the solidified raw material, and the reaction module is opened, so that the reaction is rapidly and deeply carried out, the product quality is stable, and the problems of rapid reduction and product quality improvement are solved.
Detailed Description
In order to solve the first technical problem, the catalyst for accelerating the reduction of the titanium concentrate comprises ferrous oxide, magnesium oxide, PVA, cyclic ester halide and coal; the mass ratio of the ferrous oxide to the magnesium oxide to the PVA to the cyclic ester halide is (2.5-3.5); the mass ratio of the sum of the ferrous oxide, the magnesium oxide, the PVA and the cyclic ester halide to the coal is 400.
In one embodiment, the cyclic ester halide is a cyclic ester chloride, a cyclic ester bromide, a cyclic ester iodide.
In one specific embodiment, the ferrous oxide and the magnesium oxide are prepared by the following method: iron powder, magnesium powder and water are mixed according to the mass ratio of 5-8: 4 to 9, heating for 2 to 3 hours at the temperature of between 500 and 600 ℃, and keeping the vacuum degree at 1 to 8 x 10 ^-2 Pa, pumping dry air, cooling for 1-2 h, and grinding into powder with the granularity of 10-60 meshes.
In one embodiment, the PVA is prepared by the following process: 100 parts by volume of polyethylene with the polymerization degree of 500-2000 and the alcoholysis degree of 75-99 mo1% and 200-400 parts by volume of mixed solvent of dimethyl sulfoxide/water are stirred for 3-4 hours at 80-120 ℃ and-0.01-0.08 MPa to obtain spinning solution, water-soluble polyvinyl alcohol is obtained after filtration, deaeration, dry-wet spinning and post-treatment, and the PVA is obtained after concentration and drying.
In one embodiment, the ratio of dimethylsulfoxide in the mixed solvent of dimethylsulfoxide/water: 70-90: 10-30 of water.
In one embodiment, the cyclic ester halide is a cyclic ester chloride.
In one embodiment, the cyclic ester chloride is prepared by the following method: the cyclic ester and chlorine react for 2 to 3 hours at a temperature of between 230 and 300 ℃ to obtain cyclic ester chloride, and the cyclic ester chloride is dried.
In one embodiment, the method for preparing the catalyst for accelerating the reduction of the titanium concentrate comprises the following steps: uniformly mixing ferrous oxide, magnesium oxide powder, PVA powder and cyclic ester chloride powder to obtain a mixture; and then mixing the mixture with the coal powder according to the mass ratio of 400:100, and drying at 100-120 ℃ for 0.5-1.5 h to obtain the finished product.
In order to solve the second technical problem of the present invention, the method for preparing the catalyst for accelerating the reduction of the titanium concentrate comprises the following steps:
A. the preparation of ferrous oxide and magnesium oxide powder is carried out by mixing iron powder, magnesium powder and water according to the mass ratio of 5-8 ^-2 Pa, pumping dry air and drying, cooling for 1-2 h, and grinding into powder with the particle size of 10-60 meshes;
B. preparing composite organic component powder PVA by stirring 100 parts of polyethylene with the polymerization degree of 500-2000 and the alcoholysis degree of 75-99 mo1% and 200-400 parts of mixed solvent of dimethyl sulfoxide/water at 80-120 ℃ and-0.01-0.08 MPa for 3-4 hours to obtain spinning solution, filtering, defoaming, spinning by a dry-wet method and post-treating to obtain water-soluble polyvinyl alcohol, concentrating and drying to obtain PVA;
C. preparing compound organic component powder, namely reacting cyclic ester with halogen to obtain cyclic ester chloride, and drying; preferably, the halogen is chlorine, and the reaction is carried out for 2 to 3 hours at a temperature of between 230 and 300 ℃;
D. mixing organic components and inorganic powder, namely uniformly mixing ferrous oxide, magnesium oxide powder, PVA powder and cyclic ester chloride powder to obtain a mixture; and then mixing the mixture with the coal powder according to the mass ratio of 400:100, and drying at 100-120 ℃ for 0.5-1.5 h to obtain the finished product.
In one embodiment, the ratio of dimethylsulfoxide in the mixed solvent of dimethylsulfoxide/water: 70-90: 10-30 of water.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the invention to the embodiments described.
Example 1
1. Preparation of ferrous oxide and magnesium oxide powder
Iron powder and magnesium powder are mixed according to the mass ratio of 3:2 mixing the components, weighing 300g, charging into vacuum furnace (ZY-Q), mixing with 160g water, heating at 550 deg.C for 2.5h with vacuum degree of 10 ^-2 And Pa, pumping air, cooling and drying for 1h to obtain a mixture of ferrous oxide and magnesium oxide. Then ground into powder with the granularity of 20 meshes by a mechanical grinder.
2. Preparing composite organic component powder PVA, namely adding 100 parts of polyethylene with the polymerization degree of 1000 and the alcoholysis degree of 99mo1% into a stainless steel dissolving kettle by using 400 parts of mixed solvent with the dimethyl sulfoxide/water = 70: 30, dissolving for 3 hours at the temperature of 100 ℃ and the pressure of-0.01 MPa under stirring to prepare spinning solution, filtering, defoaming, spinning by a dry-wet method and post-treating to obtain water-soluble polyvinyl alcohol (PVA), concentrating, and drying in an electrothermal blowing drying box to obtain PVA powder.
3. Preparing composite organic component powder X: reacting 400g of cyclic ester powder with chlorine gas in a reaction kettle at the normal pressure of 265 ℃ for 2h to obtain cyclic ester chloride X, and drying in an electrothermal blowing drying oven to obtain cyclic ester chloride X powder.
4. Mixing organic components with inorganic powder: uniformly mixing the ferrous oxide and magnesium oxide mixture powder prepared in the step 1, the PVA powder prepared in the step 2 and the cyclic ester chloride X powder prepared in the step 3 according to the mass ratio of 3. And then mixing the mixture according to the mass ratio of 400:100, adding coal powder, mixing, and drying at 110 ℃ for 0.5h to obtain the finished catalyst for accelerating the reduction of the titanium concentrate.
Example 2
Similar to example 1, the only difference is that the preparation temperature of the compound organic component cyclic ester chloride powder X is 250 ℃.
Example 3
Similar to example 1, the only difference is that the mass ratio of iron powder to magnesium powder is 6.
Example 4
Similar to example 1, the only difference is that the mixture of ferrous oxide and magnesium oxide has a 60 mesh grind size.
The finished product of the catalyst for accelerating the reduction of the titanium concentrate prepared in the example is added into raw ore of the titanium concentrate, and 10kg of the catalyst is added into 1 ton of the raw ore.
The catalyst is used up to now in 12 th of the year 2019, the tailings are recycled efficiently and comprehensively, the average value of the recycling rate is 74.36% after being measured for many times, and the recycling rate is 77.48% when the furnace condition is good.
The gas in the metallurgical process is tested and analyzed for many times, and the gas components are not obviously changed before the catalyst is used. Most of the catalyst components are used as nucleating agents in ferrotitanium and accelerate the reaction.
The average production time of ferrotitanium in each furnace can be reduced by 3.5 hours through multiple tests, and compared with the average production time of ferrotitanium in the prior furnace of 18 hours, the production efficiency of the invention is greatly improved. The data show that the catalyst is green and pollution-free and can be used in the whole ferrotitanium smelting process.
The titanium and iron of 15 days and 19 batches of the catalyst are sampled and detected, the titanium content is in the previous standard range, and the impurity content is strictly controlled in the qualified range. Therefore, the catalyst does not affect the product quality. The industrial application can be further expanded.
The catalyst prepared in the example 1 is respectively added into raw ore of titanium concentrate and tailings, 1 part by weight of catalyst is added into 100 parts by weight of raw ore of titanium concentrate, 3 parts by weight of catalyst is added into 100 parts by weight of tailings, secondary roasting is carried out, ferrotitanium can be formed at a low temperature of 1150 ℃, organic matter components in the catalyst are decomposed after being heated, the vaporization of a reducing agent is promoted, the reaction rate is accelerated, and the reduction effect is stable after long-term use.
Claims (11)
1. The catalyst for accelerating the reduction of the titanium concentrate is characterized by comprising ferrous oxide, magnesium oxide, PVA, cyclic ester halide and coal; the mass ratio of the ferrous oxide to the magnesium oxide to the PVA to the cyclic ester halide is 2.5-3.5; the ferrous oxide: the mass ratio of the magnesium oxide is 4-7: 6 to 7; the mass ratio of the sum of the ferrous oxide, the magnesium oxide, the PVA and the cyclic ester halide to the pulverized coal is 400.
2. The catalyst for accelerating the reduction of titanium concentrate according to claim 1, wherein the cyclic ester halide is cyclic ester chloride, cyclic ester bromide, cyclic ester iodide.
3. The catalyst for accelerating the reduction of titanium concentrate according to claim 1 or 2, wherein the ferrous oxide and the magnesium oxide are prepared by the following method: iron powder, magnesium powder and water are mixed according to the mass ratio of 5-8: 4 to 9, heating for 2 to 3 hours at the temperature of between 500 and 600 ℃ and the vacuum degree of 1 multiplied by 10 -2 Pa～8×10 -2 Pa, pumping dry air, cooling for 1-2 h, and grinding into powder with the particle size of 10-60 meshes.
4. The catalyst for accelerating the reduction of titanium concentrate according to claim 3, wherein said PVA is prepared by the following method: stirring 100 volume parts of polyethylene with the polymerization degree of 500-2000 and the alcoholysis degree of 75-99 mo1% and 200-400 volume parts of mixed solvent of dimethyl sulfoxide and water at 80-120 ℃ and-0.01-0.08 MPa for 3-4 hours to obtain spinning solution, filtering, defoaming, spinning by dry-wet method and post-treating to obtain water-soluble polyvinyl alcohol, concentrating and drying to obtain PVA.
5. The catalyst for accelerating the reduction of titanium concentrate according to claim 4, wherein the ratio of dimethyl sulfoxide to water in the mixed solvent of dimethyl sulfoxide and water is as follows: the volume ratio of water is 70-90: 10-30.
6. Catalyst for accelerating the reduction of titanium concentrates according to claim 1 or 2, characterized in that the cyclic ester halide is a cyclic ester chloride.
7. The catalyst for accelerating the reduction of titanium concentrate according to claim 6, wherein the cyclic ester chloride is prepared by the following method: reacting the cyclic ester with chlorine gas at 230-300 ℃ for 2-3 h to obtain cyclic ester chloride powder, and drying.
8. The catalyst for accelerating the reduction of titanium concentrate according to claim 1 or 2, wherein the preparation method of the catalyst for accelerating the reduction of titanium concentrate comprises: uniformly mixing ferrous oxide, magnesium oxide powder, PVA powder and cyclic ester chloride powder to obtain a mixture; and then mixing the mixture and the coal powder according to the mass ratio of 400:100, and drying at 100-120 ℃ for 0.5-1.5 h to obtain the finished product.
9. A method for preparing a catalyst for accelerating reduction of titanium concentrate, the method comprising:
A. the preparation of ferrous oxide and magnesium oxide powder is carried out by mixing iron powder, magnesium powder and water according to mass ratio of 5-8 -2 Pa～8×10 -2 Pa, pumping to dryAir drying, cooling for 1-2 h, and grinding into powder with the particle size of 10-60 meshes;
B. preparing composite organic component powder PVA, namely stirring 100 parts of polyethylene with the polymerization degree of 500-2000 and the alcoholysis degree of 75-99 mo1% and 200-400 parts of mixed solvent of dimethyl sulfoxide and water at 80-120 ℃ and-0.01-0.08 MPa for 3-4 hours to obtain spinning solution, filtering, defoaming, spinning by a dry-wet method and post-treating to obtain water-soluble polyvinyl alcohol, concentrating and drying to obtain PVA;
C. preparing compound organic component powder, namely reacting cyclic ester with halogen to obtain cyclic ester chloride, and drying;
D. mixing organic components and inorganic powder, namely uniformly mixing ferrous oxide, magnesium oxide powder, PVA powder and cyclic ester chloride powder to obtain a mixture; and then mixing the mixture and the coal powder according to the mass ratio of 400:100, and drying for 0.5 to 1.5 hours at the temperature of between 100 and 120 ℃ to obtain a finished product.
10. The method for preparing the catalyst for accelerating the reduction of titanium concentrate according to claim 9, wherein the halogen is chlorine in the step C, and the reaction is performed at 230 to 300 ℃ for 2 to 3 hours.
11. The method of claim 9, wherein the ratio of dimethylsulfoxide in the mixed solvent of dimethylsulfoxide and water: 70-90: 10-30 of water.
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| NZ252568A (en) * | 1992-05-21 | 1996-11-26 | Du Pont | Beneficiating titanium-bearing material which contains iron by reduction in the presence of carbonaceous material |
| CN103555974B (en) * | 2013-10-24 | 2016-03-09 | 攀枝花学院 | Magnalium method produces high ferrotitanium alloy |
| CN108910942A (en) * | 2018-10-09 | 2018-11-30 | 龙蟒佰利联集团股份有限公司 | A method of synthetic rutile is prepared by high calcium magnesium titanium slag |
| CN109338124A (en) * | 2018-11-23 | 2019-02-15 | 宜宾天原集团股份有限公司 | A method of chlorination rich-titanium material is prepared using high silicon-calcium-magnesium ilmenite concentrate |
| CN110606506A (en) * | 2019-09-17 | 2019-12-24 | 河南佰利联新材料有限公司 | Method for producing titanium slag and titanium white chloride by using Panzhihua ilmenite |
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