CN115353146A - Treatment method of titanium tetrachloride dust collection slag - Google Patents
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Abstract
The invention discloses a method for treating titanium tetrachloride dust collecting slag, which comprises the following steps: s1, spraying titanium tetrachloride dust collecting slag to obtain water-containing dust collecting slag; s2, roasting the water-containing dust-collecting slag at 500-900 ℃ for 0.5-5 h to obtain a roasted solid phase and roasted tail gas; s3, mixing the roasted solid phase with the Panzhihua titanium concentrate according to the mass ratio of 1:2-4, and then smelting titanium slag in an electric furnace to obtain a smelting product; and S4, using the smelting product as acid-soluble titanium slag of the sulfuric acid method titanium dioxide production process. The advantages are that: (1) the slag discharging site environment of the chlorination furnace is obviously improved; (2) The resource utilization of the titanium tetrachloride dust collecting slag is completely realized; (3) the treatment cost of the titanium tetrachloride dust collection slag is obviously reduced; and (4) the industrial popularization is easy.
Description
Technical Field
The invention relates to a titanium dioxide production technology, in particular to a technology for treating a byproduct in titanium dioxide production by a chlorination process.
Background
In recent years, the high-end titanium industry in China is rapidly developed, and according to statistics, the capacity of titanium dioxide produced by the chlorination process in China is increased to 40 ten thousand tons/year by 2020 and 5 months; the capacity of the titanium sponge exceeds 15 ten thousand tons, and the titanium sponge is the first in the world. In the production process of titanium dioxide or titanium sponge by chlorination process, chlorine and titanium-rich materials (high titanium slag, natural rutile, artificial rutile or UGS slag) are required to be subjected to chlorination reaction at high temperature to obtain titanium tetrachloride, the production process comprises two methods of boiling chlorination and molten salt chlorination, and due to the advantages of the quality of the obtained products, the emission of wastes, the length of the process flow and the productivity of equipment, the boiling chlorination is the mainstream process adopted at home and abroad at present.
After the boiling titanium white chloride is carbonized and chlorinated, metal compounds of titanium, iron, calcium, magnesium and the like in the titanium-rich material react with chlorine at high temperature to form metal chloride which overflows out of a chlorination furnace, and the metal chloride is cooled and refined to obtain titanium tetrachloride. Because titanium tetrachloride is carried in the dust-collecting slag, hydrolysis reaction occurs immediately when the dust-collecting slag meets water in the air in the deslagging process, acid mist is formed, and the field operation environment is influenced. In the process of producing titanium tetrachloride by boiling chlorination, 50-120 kg of dust collecting slag is generated when 1 ton of crude titanium tetrachloride is produced (different according to the grade difference of the used raw materials).
The titanium tetrachloride dust-collecting slag contains a large amount of easily soluble metal chloride, which is very easy to absorb moisture or hydrolyze in water to generate hydrochloric acid and metal oxide, and meanwhile, when the titanium tetrachloride dust-collecting slag is discharged out of equipment, titanium tetrachloride is very easy to combine with moisture in the air to generate hydrochloric acid mist, so that the environment is polluted, and serious accidents such as soil acidification, heavy metal ion pollution and the like are caused if the titanium tetrachloride dust-collecting slag is directly discharged into the environment. Therefore, foreign related enterprises generally adopt a lime neutralization and filter residue landfill mode for treatment, and a chlorination process titanium dioxide maximum production enterprise-American Kemu company adopts a lime neutralization method and also adopts a treatment mode of pulping waste residues, injecting the waste residues into a stratum through a high-pressure deep well, neutralizing the waste residues, and adding cement sand stone to prepare and produce building materials, namely the Guanyin stone. Most domestic enterprises adopt a mode of directly pulping with industrial water, neutralizing and filtering, discharging sewage, and conveying filter residues to a slag yard for stacking, so that secondary environmental pollution is easily caused by treatment.
With the strictness of the national environmental protection policy, in order to solve the problems, domestic enterprises and scientific research institutes develop a great deal of research and development work on a new technology for treating the collected dust slag in a reduction, harmless and recycling manner, for example, the invention patent CN104030344A provides a comprehensive treatment method of the titanium tetrachloride collected dust slag, and valuable components such as titanium slag, petroleum coke, hydrochloric acid, iron and the like are respectively recovered through size mixing, filtering, reselection, filtrate conversion and roasting. The principle is mainly based on the characteristic that the dust collecting slag contains ferric chloride and ferrous chloride with high proportion and the characteristic that hydrochloric acid is easy to volatilize, sulfuric acid is added for conversion, then hydrochloric acid is recovered through evaporation, and chloride is converted into sulfate which is difficult to volatilize. And roasting the sulfate, decomposing metal sulfates such as iron and the like into metal oxides, decomposing the sulfate into sulfur dioxide, and collecting tail gas. The method has the advantages of easily controlled process, zero discharge of production sewage and the like, but has longer flow and high waste residue treatment cost.
The invention patent CN101746816A discloses a titanium tetrachloride dust-collecting slag treatment process, which comprises the steps of adding water into titanium tetrachloride dust-collecting slag to prepare slurry, leading steam and part of hydrogen chloride gas generated in the pulping process to chlorination tail gas for neutralization treatment, conveying the prepared slurry to a drum filter by a mortar pump for filtration and liquid-solid separation, using the generated filter cake as a road cushion or conveying the filter cake to a slag yard for disposal, conveying the filtrate to a sewage treatment system for standard discharge, wherein a large amount of washing water is needed for washing waste slag generated by the treatment method, secondary pollution is caused, meanwhile, solid phase materials are not thoroughly washed, and soluble chlorine remained in the solid phase materials is leaked out under the action of rainwater soaking, so that the environmental protection is directly influenced.
The invention discloses a method for recovering hydrochloric acid by hydrolyzing titanium tetrachloride dust-collecting slag through steam neutrality, which is disclosed by CN106586962A and comprises the steps of adding the titanium tetrachloride dust-collecting slag into a rotary kiln at a constant speed, continuously introducing mixed gas of tail gas of a boiling chlorination furnace and water vapor into the rotary kiln, enabling a solid phase and a gas phase in the rotary kiln to form countercurrent contact, hydrolyzing an acid chloride and a neutral chloride in the titanium tetrachloride dust-collecting slag in steam, enabling the gas to form hydrochloric acid through a gas condenser, recovering iron of a hydrolyzed solid-phase product through weak magnetic separation, and recovering petroleum coke through flotation.
The invention patent CN105836862A discloses a titanium tetrachloride dust collecting slag treatment method, which comprises the following steps of (1) absorbing dust collecting ash with water, and obtaining solid slag and mixed liquid through solid-liquid separation; (2) Adding excessive iron powder into the mixed solution, removing heavy metal ions through a displacement reaction, and filtering to obtain a pre-heavy metal removal filtrate; (3) Removing vanadium and manganese from the pre-heavy metal removal filtrate by extraction to obtain extraction tail liquid; (4) Oxidizing the extraction tail liquid by adding an oxidant, evaporating, concentrating, cooling and crystallizing to obtain the composite flocculant-polyaluminum ferric chloride. And (2) carrying out flotation and classification treatment on the solid slag obtained in the step (1) to respectively obtain petroleum coke, quartz sand and rutile. The method realizes the comprehensive recycling of petroleum coke, rutile, quartz sand, polyaluminum ferric chloride, vanadate and heavy metal slag, does not generate wastewater and waste gas in the treatment process, and realizes the reduction and harmless comprehensive treatment of solid wastes.
The invention patent CN100998914A discloses a method for treating titanium tetrachloride dust collecting slag, which has the following principle: after metal chloride generated in the titanium tetrachloride production process is discharged in the form of dust collection slag, the dust collection slag directly enters a pulping tank for pulping, pulping liquid is recycled, when the chlorine content of the circulating slurry reaches 5-30%, the circulating slurry is pumped into a neutralization reaction tank, lime is used for neutralization reaction while stirring, and the value of the neutralization liquid is controlled to be pH 6-9; then, the mixed slurry is filtered in a filter, the filtrate is calcium chloride solution, the calcium chloride solution can be sold as a commodity after being evaporated and concentrated to reach the required concentration, a filter cake is washed by fresh water, all the calcium chloride solution is washed out and is supplemented into a pulping tank, the iron content of the filter cake is prepared by iron ore concentrate after being washed by water, the iron content of the filter cake reaches the sintering ore component required by iron making, coal coke powder and coal powder are added, the prepared filter cake is sintered at the temperature of 1000-1025 ℃, and the obtained sintering ore is the raw material required by iron making. The invention has the advantages that valuable products are formed after treatment, and all chlorine radicals are recycled, thereby completely meeting the requirements of circular economy and harmless discharge.
The invention patent CN106745308A discloses a treatment method of titanium tetrachloride dust collection slag, which comprises the following steps: (1) Adding water into titanium tetrachloride dust-collecting slag, and mixing until chloride is dissolved in a liquid phase to obtain slurry; (2) Filtering the obtained slurry to obtain a first filtrate and a first filter residue; (3) Separating the first filter residue by gravity to obtain titanium slag and petroleum coke; (4) Adding lime milk into the obtained first filtrate until the pH value is between 7 and 8 to obtain second filtrate; (5) Standing the obtained second filtrate for 2-3 h, and then filtering to obtain a calcium chloride solution and second filter residue; (6) Roasting the obtained second filter residue at 700-800 ℃ to obtain the iron oxide powder. The invention provides a titanium tetrachloride dust collection slag treatment method which improves the comprehensive utilization rate of resources and reduces environmental pollution. The invention patents CN110961430A and CN111545551A of Panzhihua steel group also disclose two treatment methods of chlorination residues, and mainly invent a special device. The device is utilized to decompose titanium tetrachloride dust-collecting slag by adding water to obtain an aqueous solution, the aqueous solution reacts with hypochlorite-containing wastewater generated by a chlorination production tail gas treatment system and then is filtered to obtain iron-containing slag and brine, the iron-containing slag can be stockpiled and utilized, the brine can be evaporated, crystallized and recycled to obtain salt, the treatment method is simple, the titanium tetrachloride dust-collecting slag and the hypochlorite-containing wastewater are comprehensively treated and utilized, and the environmental protection problem caused by the existing titanium tetrachloride dust-collecting slag treatment mode is better solved.
In addition, some documents also mention the treatment method of titanium tetrachloride dust-collecting slag, for example, the materials of northeast university and the 2013 level of Master research institute Yao Quan research two methods, one is the preparation method of calcium chloride by using lime neutralization method, and the other is the preparation method of similar guanyin stone.
From the recent research situation in China. At present, the titanium tetrachloride dust collecting slag is treated basically in a wet mode, reduction and harmlessness are mainly adopted in the treatment process, various treatment process flows are long, equipment requirements are strict, the cost is high, and no report of industrial popularization and application is found; the comprehensive utilization of resources is rarely reported except that the CN100998914A patent is used for blending iron ore into filter cakes for sintering pellets.
As can be seen, there is still a lack of economically viable treatment methods available in the art for titanium tetrachloride dust collecting slag.
Disclosure of Invention
The invention provides a method for treating titanium tetrachloride dust-collecting slag, which aims to solve the problems that the titanium tetrachloride dust-collecting slag is difficult to treat and the treatment cost is high.
The technical scheme adopted by the invention is as follows: the method for treating the titanium tetrachloride dust collecting slag comprises the following steps:
s1, spraying titanium tetrachloride dust collecting slag to obtain water-containing dust collecting slag;
s2, roasting the water-containing dust-collecting slag at 500-900 ℃ for 0.5-5 h to obtain a roasted solid phase and roasted tail gas;
s3, mixing the roasted solid phase with the Panzhihua titanium concentrate according to a mass ratio of 1:2-4, and then smelting titanium slag in an electric furnace to obtain a smelting product;
and S4, using the smelting product as acid-soluble titanium slag of the sulfuric acid method titanium dioxide production process.
As a further improvement of the invention, the method also comprises the step of spraying and absorbing the roasting tail gas to obtain by-product hydrochloric acid.
As a further improvement of the invention, the equipment used for calcination in step S2 is a rotary kiln or a fluidized bed. More preferably, the fuel used for calcination is natural gas, heavy oil or solid fuel.
As a further improvement of the invention, the amount of water used for spraying in the step S1 is 1-20% of the mass of the titanium tetrachloride dust-collecting slag.
The beneficial effects of the invention are:
(1) Improving the slag discharge site environment of the chlorination furnace: titanium tetrachloride dust-collecting slag generated by the boiling titanium dioxide in the chlorination process is discharged from a chlorination furnace and collected by a cyclone dust collector, titanium tetrachloride is inevitably carried in the formed dust-collecting slag, and once the dust-collecting slag meets moisture contained in air in the deslagging process, hydrolysis reaction is immediately carried out on the titanium tetrachloride to form white smoke containing hydrogen chloride, so that the field operation environment is influenced; on the other hand, due to the addition of water, the temperature of the dust collection slag material is reduced, the generation of acid mist is reduced, and the aim of obviously improving the field environment is fulfilled.
(2) The resource utilization of the titanium tetrachloride dust collection slag is completely realized: experiments show that the smelted product obtained by smelting titanium slag in an electric furnace after the roasted solid phase and the Panzhihua titanium concentrate are mixed according to the mass ratio of 1:2-4 can completely meet the index requirement of the acid-soluble titanium slag, and can be used as the acid-soluble titanium slag of the production process of titanium dioxide by a sulfuric acid method. The dust collection slag contains a large amount of chloride, the chlorine in the material can be pyrolyzed to form hydrogen chloride when the material contains moisture, hydrochloric acid can be obtained after the hydrogen chloride is absorbed by water and sold, and an outlet is found for utilizing the chlorine. Therefore, the chloride ions and the metal compounds in the titanium tetrachloride dust collecting slag can be completely recycled, and the requirement standard of circular economy is completely met.
(3) The treatment cost of the titanium tetrachloride dust collection slag is remarkably reduced: the invention has the advantages of simple process, short flow, low energy consumption, low cost and the like; and the titanium tetrachloride dust collection slag is ingeniously utilized to contain more unreacted petroleum coke powder, the petroleum coke is oxidized to emit a large amount of heat during roasting, and the roasting of the dust collection slag can be completed by using the heat emitted by oxidation or adding a heat source properly, so that the process energy consumption is greatly reduced. Experiments show that the cost of treating each ton of titanium tetrachloride dust collecting slag by adopting the method is only about 15 yuan; is far superior to the prior titanium tetrachloride dust-collecting slag recovery process.
(4) Easy industrialized popularization: the invention belongs to combined innovation of cross-industry and cross-field, does not relate to new equipment and materials, has smaller technical risk and is easy for industrialized popularization.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The first embodiment is as follows:
the method comprises the following steps of:
(1) Separating the chlorinated tail gas by cyclone to obtain titanium tetrachloride dust-collecting slag, collecting the dust-collecting slag into a slag tank, spraying water in a proportion of 7.5 percent of the slag amount in the collecting process, and cooling the material to 70 ℃ to obtain water-containing dust-collecting slag for roasting.
(2) Transferring the water-containing dust-collecting slag into a rotary kiln preheated to 850 ℃, controlling the temperature of the rotary kiln to be stabilized at 850 ℃ by controlling the introduction amount of natural gas used for combustion of the rotary kiln, roasting the material for 2 hours, then discharging the roasted material into a slag cooler, cooling the material to ensure that the temperature of the material is less than or equal to 80 ℃, and obtaining a roasted solid phase and roasted tail gas; the obtained roasting tail gas is absorbed by water to obtain hydrochloric acid with the mass concentration of 32%, and the hydrochloric acid is sold.
Sampling and detecting the roasted solid phase, wherein the chemical components are shown in the table 1:
table 1 example solid phase chemical composition after calcination
| Item | TiO 2 | FeO | Fe 2 O 3 | C | CaO | MgO | SiO 2 | Al 2 O 3 |
| W/％ | 36.53 | 2.56 | 30.79 | 25.32 | 0.96 | 1.18 | 3.43 | 1.07 |
Solid phase particle size after calcination is as in table 2:
table 2 example solid phase particle size composition after calcination
| Particle size (mm) | 10～20 | 1～10 | 0.1～1 | ＜0.1 |
| W/％ | 3.5 | 93.2 | 2.7 | 0.6 |
(3) The roasted solid phase and Panzhihua titanium concentrate with the grade of 46.7 percent are mixed according to the mass ratio of 1:2 for smelting titanium slag in an electric furnace, and the component detection of the obtained smelting product is shown in a table 3:
table 3: example A chemical composition of a smelting product
| Item | TiO 2 | FeO | CaO | MgO | SiO 2 |
| W/％ | 74.6 | 9.52 | 1.31 | 6.04 | 6.82 |
As can be seen from Table 3, the obtained smelting product can completely meet the index requirements of the acid-soluble titanium slag, and can be used as the acid-soluble titanium slag of the titanium dioxide production process by the sulfuric acid method.
Example two:
the method is adopted for treating the titanium tetrachloride dust collecting slag:
(1) And (3) obtaining titanium tetrachloride dust collecting slag after the chlorination tail gas is subjected to cyclone separation, collecting the dust collecting slag into a slag tank, spraying water in a proportion of 5% of the slag amount in the collecting process, and obtaining water-containing dust collecting slag for roasting when the material is cooled to 65 ℃.
(2) Transferring the water-containing dust-collecting slag into a rotary kiln preheated to 750 ℃, controlling the temperature of the rotary kiln to be 750 ℃ by controlling the introduction amount of natural gas used for combustion of the rotary kiln, roasting the material for 4 hours, then discharging the roasted material into a slag cooler, cooling the material to ensure that the temperature of the material is less than or equal to 75 ℃, and obtaining a roasted solid phase and roasted tail gas; the obtained roasting tail gas is absorbed by water to obtain hydrochloric acid with the mass concentration of 17%, and the hydrochloric acid is sold.
Sampling and detecting the solid phase after roasting, wherein the chemical components are shown in the table 4:
table 4 example two solid phase chemical composition after firing
| Item | TiO 2 | FeO | Fe 2 O 3 | C | CaO | MgO | SiO 2 | Al 2 O 3 |
| W/％ | 33.49 | 2.37 | 29.86 | 27.98 | 1.13 | 1.21 | 3.86 | 1.27 |
Solid phase particle size after calcination is as in table 5:
TABLE 5 example two solid phase particle size composition after calcination
| Particle size (mm) | 10～20 | 1～10 | 0.1～1 | ＜0.1 |
| W/％ | 2.9 | 92.7 | 3.8 | 0.6 |
(3) The roasted solid phase and Panzhihua titanium concentrate with the grade of 46.3 percent are mixed according to the mass ratio of 1:3 for smelting titanium slag in an electric furnace, and the component detection of the obtained smelting product is shown in Table 6:
table 6: EXAMPLE II smelting of product chemistry
| Item | TiO 2 | FeO | CaO | MgO | SiO 2 |
| W/％ | 72.5 | 10.27 | 1.53 | 6.85 | 7.13 |
As can be seen from Table 6, the obtained smelting product can completely meet the index requirements of the acid-soluble titanium slag, and can be used as the acid-soluble titanium slag of the titanium dioxide production process by the sulfuric acid method.
Example three:
the method is adopted for treating the titanium tetrachloride dust collecting slag:
(1) And (3) obtaining titanium tetrachloride dust collecting slag after the chlorination tail gas is subjected to cyclone separation, collecting the dust collecting slag into a slag tank, spraying water in a proportion of 10% of the slag amount in the collecting process, and obtaining water-containing dust collecting slag for roasting when the material is cooled to 65 ℃.
(2) Transferring the water-containing dust-collecting slag into a rotary kiln preheated to 800 ℃, controlling the temperature of the rotary kiln to be stabilized at 800 ℃ by controlling the introduction amount of natural gas used for combustion of the rotary kiln, roasting the material for 2.5 hours, then discharging the roasted material into a slag cooler, cooling the material to ensure that the temperature of the material is less than or equal to 70 ℃, and obtaining a roasted solid phase and roasted tail gas; the obtained calcination tail gas is absorbed by water to obtain hydrochloric acid with the mass concentration of 27%, and the hydrochloric acid is sold.
Sampling and detecting the solid phase after roasting, wherein the chemical components are shown in the table 7:
TABLE 7 examples solid phase chemical composition after triple calcination
| Item | TiO 2 | FeO | Fe 2 O 3 | C | CaO | MgO | SiO 2 | Al 2 O 3 |
| W/％ | 34.67 | 2.49 | 28.67 | 26.85 | 1.05 | 1.31 | 3.79 | 1.21 |
Solid phase particle size after calcination is as in table 8:
TABLE 8 examples solid phase particle size composition after triple calcination
| Particle size (mm) | 10～20 | 1～10 | 0.1～1 | ＜0.1 |
| W/％ | 3.4 | 92.4 | 3.4 | 0.8 |
(3) The roasted solid phase and the Panzhihua titanium concentrate with the grade of 45.9 percent are mixed according to the mass ratio of 1:4 for smelting titanium slag in an electric furnace, and the component detection of the obtained smelting product is shown in a table 9:
table 9: EXAMPLE III smelting of product chemistry
| Item | TiO 2 | FeO | CaO | MgO | SiO 2 |
| W/％ | 73.6 | 9.97 | 1.45 | 6.76 | 6.81 |
As can be seen from Table 9, the obtained smelting product can completely meet the index requirements of the acid-soluble titanium slag, and can be used as the acid-soluble titanium slag of the titanium dioxide production process by the sulfuric acid method.
Claims (5)
1. The method for treating the titanium tetrachloride dust collecting slag is characterized by comprising the following steps:
s1, spraying titanium tetrachloride dust collecting slag to obtain water-containing dust collecting slag;
s2, roasting the water-containing dust-collecting slag at 500-900 ℃ for 0.5-5 h to obtain a roasted solid phase and roasted tail gas;
s3, mixing the roasted solid phase with the Panzhihua titanium concentrate according to a mass ratio of 1:2-4, and then smelting titanium slag in an electric furnace to obtain a smelting product;
and S4, using the smelting product as acid-soluble titanium slag of the sulfuric acid method titanium dioxide production process.
2. The method for treating titanium tetrachloride dust-collecting slag according to claim 1, wherein: and the method also comprises the step of spraying and absorbing the roasting tail gas to obtain a byproduct hydrochloric acid.
3. The method for treating titanium tetrachloride dust-collecting slag according to claim 1, wherein: the equipment used for roasting in the step S2 is a rotary kiln or a fluidized bed.
4. The method for treating titanium tetrachloride dust-collecting slag according to claim 3, wherein: the fuel used for roasting is natural gas, heavy oil or solid fuel.
5. The method for treating titanium tetrachloride dust-collecting slag according to claim 1, wherein: in the step S1, the amount of water used for spraying is 1-20% of the mass of the titanium tetrachloride dust-collecting slag.
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| CN117488104A (en) * | 2023-11-02 | 2024-02-02 | 聚挪机械科技(上海)有限公司 | Method for preparing high-vanadium slag by treating vanadium-containing slurry by fluidized bed |
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