CN107188127B - Method for preparing titanium dioxide seed crystal by using chlorination waste acid - Google Patents
Method for preparing titanium dioxide seed crystal by using chlorination waste acid Download PDFInfo
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- CN107188127B CN107188127B CN201710524170.3A CN201710524170A CN107188127B CN 107188127 B CN107188127 B CN 107188127B CN 201710524170 A CN201710524170 A CN 201710524170A CN 107188127 B CN107188127 B CN 107188127B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
Abstract
The invention discloses a method for preparing titanium dioxide seed crystals by using chlorination waste acid, and belongs to the technical field of titanium dioxide seed crystal preparation. The operation of preparing the titanium dioxide seed crystal is divided into three parts of concentration of waste hydrochloric acid, preparation of hydrochloric acid for the seed crystal and preparation of the titanium dioxide seed crystal, the pesticide waste hydrochloric acid is purified and absorbed to obtain a concentrated hydrochloric acid solution, then the industrial hydrochloric acid and the concentrated hydrochloric acid solution are mixed and prepared according to a certain proportion, and the obtained hydrochloric acid for the seed crystal is prepared to be used in an acid dissolving process of preparing the titanium dioxide seed crystal. The invention uses the by-product waste hydrochloric acid of the pesticide, the price is low, not only the cost of treating waste acid by a pesticide manufacturer is reduced, but also the cost of purchasing industrial hydrochloric acid by a titanium dioxide manufacturer is reduced, and the equipment cost is lower, the corrosion resistance is strong, and the service life is long.
Description
Technical Field
The invention relates to the technical field of titanium dioxide seed crystal preparation, in particular to a method for preparing titanium dioxide seed crystal by using chlorination waste acid. The invention concentrates the pesticide waste acid and uses the concentrated pesticide waste acid to perform acid dissolution to obtain the titanium dioxide seed crystal, thereby achieving the purpose of reducing the production cost of pesticide manufacturers and titanium dioxide manufacturers.
Background
Titanium dioxide is an important white pigment and porcelain glaze, and compared with other white pigments, the titanium dioxide has superior whiteness, tinting strength, covering power, weather resistance, heat resistance and chemical stability, and particularly has no toxicity. The titanium dioxide production process belongs to the fine chemical engineering range, the production process is continuously optimized, the production cost of the titanium dioxide is reduced to the maximum extent under the condition of not influencing the yield and the quality of the titanium dioxide, and the titanium dioxide production process is always the target pursued by titanium dioxide manufacturers.
In the preparation process of pesticides such as dimethoate, glyphosate and the like, the most produced by-product is waste hydrochloric acid with acid content of about 15-18%, and the waste hydrochloric acid cannot be directly discharged due to strong acid content, and a large amount of alkali is generally required for neutralization when a pesticide manufacturer treats the by-product waste hydrochloric acid. And the waste hydrochloric acid contains a large amount of NaCl and other impurities, so that the waste hydrochloric acid cannot be directly utilized in other application fields. Therefore, except for the alkali neutralization, the current pesticide manufacturers ask the relevant manufacturers for help in treatment, and the treatment cost of the waste hydrochloric acid is undoubtedly high for the pesticide manufacturers.
Aiming at the problem of treatment of waste acid in the pesticide by-product, the patent number is CN200810233979.1, and the invention creation name is: a process for recovering waste acid in glyphosate production uses 15-20% of condensed waste acid in glyphosate production as raw material, and the condensed waste acid is concentrated into 31% hydrochloric acid by a two-stage falling film absorption tower of a two-in-one device of a chlor-alkali production system, and then returned to an acidification post of a glyphosate dehydrogenation section and a condensation section (a phosphorous acid method) of a pesticide production system for use, so as to achieve the purposes of reducing production cost and reducing environmental protection pressure. The application realizes the recycling of waste acid resources, and is a good scheme for cost reduction and efficiency improvement, but if a pesticide manufacturer needs to be matched with an online waste acid recovery system to realize the scheme, not all pesticide manufacturers can bear or are willing to bear the extra expense.
The patent number is CN201510938229.4, and the invention creation name is: a method for producing titanium dioxide by a waste acid self-circulation non-blast furnace titanium slag sulfuric acid method; the application takes non-blast furnace smelting titanium slag of vanadium titano-magnetite as a raw material, waste acid produced in the titanium dioxide production process is mixed with the non-blast furnace titanium slag to obtain pre-treated titanium slag containing low iron, aluminum and magnesium, the pre-treated titanium slag is subjected to acidolysis curing by concentrated sulfuric acid, then the titanium dioxide is produced by the procedures of water leaching, concentration, hydrolysis, roasting and the like, and the waste acid after hydrolysis is returned for recycling. The application is mainly characterized in that titanium white waste acid is adopted to pretreat titanium slag, so that most of aluminum and magnesium impurities in the titanium slag are removed, the influence of the aluminum, magnesium and other impurities in the titanium slag on titanium white production is eliminated, the process of sulfuric acid process purification of ilmenite is simplified, and a foundation is laid for producing high-quality titanium white; meanwhile, the direct recycling of titanium white hydrolysis waste acid is realized, but the application firstly utilizes non-blast furnace smelting titanium slag to produce titanium white, is relatively limited in the actual production process, and the process for preparing the titanium white cannot become a mainstream.
The patent with the application number of CN201510818825.9 discloses a method for applying the waste acid chloride to the coating of titanium dioxide, wherein the waste acid chloride is used for preparing titanium dioxide; according to the application, crude hydrochloric acid recovered by washing chlorinated tail gas is subjected to standing, precipitation and impurity removal, then is diluted, and is subjected to process adjustment in the titanium dioxide coating process, so that other impurities are prevented from being deposited on the titanium dioxide, and a titanium dioxide coated product with excellent quality is obtained. The application applies the industrially recycled crude hydrochloric acid to the titanium dioxide coating process, which is a good waste recycling scheme, but how to develop other utilization values of the industrial waste acid in the titanium dioxide manufacturing process, such as the preparation of titanium dioxide seed crystals by using the waste hydrochloric acid, no effective scheme is found through retrieval, and further research is still needed.
Disclosure of Invention
1. Technical problem to be solved by the invention
The invention aims to solve the problems that in the prior art, waste hydrochloric acid which is a byproduct in pesticide production is seriously wasted and cannot be well recycled, and provides a method for preparing titanium dioxide seed crystals by using waste acid from chlorination; by adopting the technical scheme provided by the invention, the waste hydrochloric acid which is a byproduct in pesticide production is concentrated and absorbed to reach the concentration of 20-22%, and then is prepared into hydrochloric acid with the concentration of 25-28% with industrial hydrochloric acid for preparing titanium dioxide seed crystals; the hydrochloric acid can greatly reduce the production cost of the titanium dioxide; the production system provided by the invention has the advantages of corrosion resistance, long service time, simple maintenance and low cost.
2. Technical scheme
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the invention discloses a method for preparing titanium dioxide seed crystals by using chlorinated waste acid, which comprises the following operation steps of concentrating waste hydrochloric acid, preparing seed crystals by using hydrochloric acid and preparing the titanium dioxide seed crystals, purifying and absorbing pesticide waste hydrochloric acid to obtain a concentrated hydrochloric acid solution, mixing industrial hydrochloric acid and the concentrated hydrochloric acid solution according to the proportion of 1:1-2:1, and preparing the obtained seed crystals by using the hydrochloric acid for an acid dissolving process of preparing the titanium dioxide seed crystals.
Furthermore, the production system for preparing the titanium dioxide seed crystal comprises a waste hydrochloric acid concentration unit, a seed crystal hydrochloric acid configuration unit and a titanium dioxide seed crystal preparation unit, wherein the waste hydrochloric acid concentration unit is connected with the seed crystal hydrochloric acid configuration unit, the waste hydrochloric acid concentration unit purifies and absorbs the pesticide waste hydrochloric acid and inputs the purified and absorbed pesticide waste hydrochloric acid into the seed crystal hydrochloric acid configuration unit, an output pipeline of the seed crystal hydrochloric acid configuration unit is connected with an acid dissolving pot of the titanium dioxide seed crystal preparation unit, and the configured hydrochloric acid of the seed crystal is input into the acid dissolving pot.
Furthermore, the waste hydrochloric acid concentration unit comprises a waste hydrochloric acid storage tank, an evaporator, a gas-liquid separator, an absorption tower and a hydrochloric acid storage tank, wherein the waste hydrochloric acid storage tank is connected with the evaporator, the top of the evaporator is connected with the gas-liquid separator, the upper part of the gas-liquid separator is connected with the absorption tower, and the bottom of the absorption tower is connected with the hydrochloric acid storage tank.
Furthermore, the horizontal position of the evaporator is higher than that of the waste hydrochloric acid storage tank, and the bottom of the evaporator is connected with a pipeline to the waste hydrochloric acid storage tank; the bottom of the gas-liquid separator is also connected with a pipeline to a waste hydrochloric acid storage tank.
Furthermore, the crystal seed hydrochloric acid preparation unit comprises a hydrochloric acid preparation tank, an industrial hydrochloric acid storage tank and a crystal seed hydrochloric acid storage tank, wherein the hydrochloric acid storage tank is connected with the hydrochloric acid preparation tank, the industrial hydrochloric acid storage tank is also connected with the hydrochloric acid preparation tank, and the lower end of the hydrochloric acid preparation tank is connected with the crystal seed hydrochloric acid storage tank.
Furthermore, the titanium dioxide seed crystal preparation unit comprises an acid dissolving pot, an acid dissolving filter press, an acid dissolving pulping tank, a metatitanic acid storage tank, a metatitanic acid metering tank, an alkali dissolving pot, an alkali dissolving filter press and an alkali dissolving pulping tank; according to the conveying direction of the materials, a metatitanic acid storage tank, a metatitanic acid metering tank, an alkali dissolving pot, an alkali dissolving filter press, an alkali dissolving pulping tank, an acid dissolving pot, an acid dissolving filter press and an acid dissolving pulping tank are sequentially connected, and a hydrochloric acid storage tank for seed crystals is connected with the acid dissolving pot through a hydrochloric acid metering tank for seed crystals.
Furthermore, the concrete process of the concentration of the pesticide waste hydrochloric acid and the preparation of the hydrochloric acid for the seed crystal comprises the following steps:
step one, starting an evaporator, and controlling the negative pressure of the evaporator to be between 300 and 400 KPa.
And step two, starting a material transferring pump of the waste hydrochloric acid storage tank to supply the waste hydrochloric acid to the evaporator.
Step three, after supplying acid for a period of time, the evaporator starts to supply mixed gas of HCl and water vapor to the gas-liquid separator;
step four, the evaporator supplies steam to the gas-liquid separator, then the absorption tower is opened, and after the steam is supplied for a period of time, the liquid of the gas-liquid separator is separated out and transferred to a waste hydrochloric acid storage tank; and after the gas-liquid separator supplies steam to the absorption tower for a period of time, transferring the concentrated hydrochloric acid absorbed by the absorption tower to a hydrochloric acid storage tank.
Step five, the volume of the concentrated hydrochloric acid in the hydrochloric acid storage tank reaches 50m3Rotate 30m later3To a hydrochloric acid preparation tank; then the industrial hydrochloric acid storage tank is rotated by 30m3-60m3Preparing industrial hydrochloric acid into a hydrochloric acid preparation tank, stirring for a period of time, and measuring the concentration of the hydrochloric acid; transferring the crystal seeds to a hydrochloric acid storage tank for later use when the concentration reaches 25-31%.
Furthermore, the specific process for preparing the titanium dioxide seed crystal comprises the following steps:
step one, transferring the prepared metatitanic acid from a metatitanic acid storage tank to a metatitanic acid metering tank, and heating to 60-80 ℃;
secondly, adding liquid caustic soda with a certain volume mass percentage concentration of 49% into an alkali dissolving pot, and heating to 75-95 ℃;
step three, transferring the metatitanic acid heated in the metatitanic acid metering tank into an alkali dissolving pot, heating to 108 ℃, and aging for 2 hours;
step four, adding desalted water with the same volume as the metatitanic acid into an alkali dissolving pot, reducing the temperature, adding sand into a jacket of the alkali dissolving pot, filtering water, and cooling the slurry to 60-70 ℃;
transferring the slurry after the alkali dissolution in the alkali dissolving pot into an alkali dissolving filter press, washing with deionized water until the NaOH content in the filtrate is less than 5g/L, and transferring the filtrate into a filtrate tank;
step six, transferring the slurry in the alkali-dissolving filter press into an alkali-dissolving slurry making tank, wherein the mass ratio of water to the slurry in the alkali-dissolving slurry making tank is 7:1, and continuously stirring for a period of time;
step seven, transferring the slurry in the alkali dissolving slurry tank to an acid dissolving pot, adding dilute hydrochloric acid from the seed crystal to the acid dissolving pot by using a hydrochloric acid metering tank, adjusting the pH to be less than 3.1, stirring for a period of time, adding dilute hydrochloric acid to ensure that the pH is less than 3.1, and heating to 40-50 ℃;
step eight, heating the slurry in the acid dissolving pot to 60-65 ℃, and adding hydrochloric acid again to adjust the pH value to 0-1.0; continuously heating to 100 ℃ and 110 ℃, and aging for 120 minutes;
transferring the slurry prepared by the acid dissolving pot to an acid dissolving filter press, and washing with deionized water until the NaCl content in the filtrate is lower than 1 g/L;
step ten, blanking by an acid-soluble filter press, pulping in an acid-soluble pulping tank, and controlling the total titanium concentration to be 110-120g/L to obtain the titanium dioxide rutile seed crystal.
Furthermore, in the acid dissolution process, the temperature is raised to 110 ℃ with the temperature rise range of 1 ℃/min until the acid dissolution temperature is 100-.
Furthermore, after the acid dissolution process is completed, the rutile conversion rate R is required to be more than 98.5%, and the total titanium concentration is 110-120g/L, and then the slurry is transferred to an acid dissolution filter press.
3. Advantageous effects
Compared with the prior art, the technical scheme provided by the invention has the following remarkable effects:
(1) the invention relates to a method for preparing titanium dioxide seed crystals by using chlorinated waste acid, wherein the waste hydrochloric acid is evaporated by an evaporator, the evaporated gas is subjected to gas-liquid separation by a gas-liquid separator, the separated HCl gas is transferred to an absorption tower, the absorption tower uses deionized water without any impurities as an absorbent, and hydrochloric acid with higher purity can be obtained by simple concentration, purification and absorption, only a small amount of NaCl can be contained, but the NaCl impurities do not influence the preparation of the titanium dioxide seed crystals, do not influence the activity of the titanium dioxide seed crystals, and can be completely used for preparing the titanium dioxide seed crystals;
(2) according to the method for preparing the titanium dioxide seed crystal by using the chlorination waste acid, the concentration of the concentrated hydrochloric acid can only reach 20% -22% and cannot meet the requirement of the seed crystal preparation on the concentration of the hydrochloric acid, and the concentrated hydrochloric acid is further processed, so that the required cost is high, the process is complex, and the cost performance is not high; instead of completely utilizing the concentrated hydrochloric acid, a crystal seed hydrochloric acid preparation unit is arranged, and the industrial hydrochloric acid and the concentrated hydrochloric acid are mixed to obtain the hydrochloric acid suitable for preparing the titanium dioxide crystal seed, so that the cost for preparing the titanium dioxide crystal seed is further reduced;
(3) according to the method for preparing the titanium dioxide seed crystal by using the chlorination waste acid, the hydrochloric acid suitable for preparing the titanium dioxide seed crystal can be obtained by simply concentrating, purifying, absorbing and mixing the pesticide waste hydrochloric acid, and the process is simple; the pesticide waste hydrochloric acid can be obtained from a pesticide manufacturer at a lower price even without any cost, so that the raw material purchasing cost of a titanium dioxide manufacturer is reduced, the liquid caustic soda used by the pesticide manufacturer for neutralization and discharge is reduced, and the pesticide production cost is greatly reduced;
(4) the production system for preparing the titanium dioxide seed crystal by using the chlorination waste acid is simple in structure, and is convenient to control by conveying materials through the material transferring pump; the evaporator and the gas-liquid separator are provided with reflux devices, so that the environment is protected and the materials are recycled; the waste hydrochloric acid storage tank, the evaporator, the gas-liquid separator and the like are concentrated and purified by adopting graphite as the internal material, so that the corrosion can be avoided, and the service life of the equipment is prolonged.
Drawings
FIG. 1 is a schematic structural diagram of a production system for preparing titanium dioxide seed crystals by using pesticide waste hydrochloric acid in the invention;
FIG. 2 is a flow chart of preparing titanium dioxide seed crystals by using chlorinated waste acid in the invention.
1. A waste hydrochloric acid storage tank; 2. an evaporator; 3. a gas-liquid separator; 4. an absorption tower; 5. a hydrochloric acid storage tank; 6. a hydrochloric acid preparation tank; 7. an industrial hydrochloric acid storage tank; 8. a hydrochloric acid storage tank for the crystal seeds; 9. a hydrochloric acid metering tank is used for the seed crystal; 10. an acid dissolution pot; 11. acid-soluble filter press; 12. acid-soluble pulping tank; 13. a metatitanic acid storage tank; 14. a metatitanic acid metering tank; 15. an alkali dissolving pot; 16. an alkali-soluble filter press; 17. alkali dissolving pulping tank; 18. a deionized water storage tank.
Detailed Description
For a further understanding of the invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings and examples.
Example 1
According to the production system for preparing the titanium dioxide seed crystal by adopting the pesticide waste hydrochloric acid, the pesticide waste acid is concentrated, the purification and the absorption are included, impurities in the waste hydrochloric acid are removed, the concentration of the waste hydrochloric acid can be improved, and the preparation condition of the titanium dioxide seed crystal is achieved; not only can reduce the cost of treating the waste hydrochloric acid in a pesticide factory, but also can reduce the cost of purchasing industrial hydrochloric acid in a titanium dioxide factory. The concentration principle of the waste hydrochloric acid is as follows: the vapor pressure is adjusted to achieve the transition of hydrogen chloride gas from liquid phase to gas phase.
Referring to fig. 1, the production system of this embodiment specifically includes a waste hydrochloric acid storage tank 1, an evaporator 2, a gas-liquid separator 3, an absorption tower 4, a hydrochloric acid storage tank 5, a hydrochloric acid preparation tank 6, an industrial hydrochloric acid storage tank 7, a seed crystal hydrochloric acid storage tank 8, a seed crystal hydrochloric acid metering tank 9, an acid dissolution pot 10, an acid dissolution filter press 11, an acid dissolution pulping tank 12, a metatitanic acid storage tank 13, a metatitanic acid metering tank 14, an alkali dissolution pot 15, an alkali dissolution filter press 16, an alkali dissolution pulping tank 17, and a deionized water storage tank 18.
The side end of the waste hydrochloric acid storage tank 1 is directly connected with the evaporator 2 by a pump, the horizontal position of the evaporator 2 is higher than that of the waste hydrochloric acid storage tank 1, the bottom of the evaporator 2 is connected with a pipeline to the waste hydrochloric acid storage tank 1, and dilute hydrochloric acid containing a small amount of HCl is transferred into the waste hydrochloric acid storage tank 1 through the pipeline at the bottom of the evaporator 2 under the action of gravity after the evaporator 2 finishes evaporation. The top of the evaporator 2 is connected with the gas-liquid separator 3, the gas of the evaporator 2 is transferred to the gas-liquid separator 3 through a pipeline, the upper part of the gas-liquid separator 3 is connected with the absorption tower 4, and the HCl gas separated from the gas-liquid separator 3 is transferred to the absorption tower 4 from the upper part of the gas-liquid separator 3. The bottom of the gas-liquid separator 3 is connected with a pipeline to the waste hydrochloric acid storage tank 1, and liquid flows out from the pipeline at the bottom of the gas-liquid separator 3 to the waste hydrochloric acid storage tank 1 under the action of gravity.
The solvent of the absorption tower 4 is deionized water, the deionized water is added through a deionized water storage tank 18 at the upper part of the absorption tower 4, and the deionized water is supplied to the absorption tower 4 as an absorbent without bringing any impurities. The bottom of the absorption tower 4 is connected with a hydrochloric acid storage tank 5, and the absorbed hydrochloric acid is transferred to the hydrochloric acid storage tank 5. The absorbed hydrochloric acid, namely the hydrochloric acid solution with the HCl concentration of about 20% -22% in the hydrochloric acid storage tank 5, contains a small amount of water vapor which carries a small amount of NaCl, namely the absorbed hydrochloric acid contains a small amount of NaCl.
It is worth to be noted here that the preparation of the seed crystal of titanium dioxide requires the use of a large amount of hydrochloric acid, requiring HCl concentrations of 25% to 31%. In the process of preparing the titanium dioxide seed crystal, a large amount of liquid alkali can be remained in the first step of alkali dissolution, a small amount of liquid alkali can exist after washing, and the liquid alkali can react with hydrochloric acid to produce NaCl with higher concentration during acid dissolution, namely the absorbed hydrochloric acid contains a small amount of NaCl and does not influence the preparation of the seed crystal. In the embodiment, the titanium dioxide seed crystal is prepared by using the pesticide waste hydrochloric acid, the pesticide waste hydrochloric acid can be obtained from a pesticide manufacturer at a lower price even without any cost, but the recovered waste hydrochloric acid is insufficient in concentration, contains a certain amount of NaCl and cannot be directly used, and the waste hydrochloric acid is further treated to improve the concentration of the waste hydrochloric acid and reduce the content of the NaCl, so that the titanium dioxide seed crystal is suitable for preparing the titanium dioxide seed crystal.
The hydrochloric acid storage tank 5 is connected with the hydrochloric acid preparation tank 6, a pump is arranged between the hydrochloric acid storage tank 5 and the hydrochloric acid preparation tank 6, and the low-concentration hydrochloric acid in the hydrochloric acid storage tank 5 is transferred to the hydrochloric acid preparation tank 6 through the pump. The hydrochloric acid preparation tank 6 is simultaneously connected with the industrial hydrochloric acid storage tank 7, a pump is also arranged between the hydrochloric acid preparation tank 6 and the industrial hydrochloric acid storage tank 7, the industrial hydrochloric acid in the industrial hydrochloric acid storage tank 7 is transferred to the hydrochloric acid preparation tank 6 through the pump, a stirrer is arranged inside the hydrochloric acid preparation tank 6 and used for preparing hydrochloric acid with proper crystal seed preparation concentration, and the hydrochloric acid for crystal seeds is prepared by mixing the industrial hydrochloric acid and the concentrated hydrochloric acid according to the proportion of 1:1-2:1 in the embodiment.
The lower end of the hydrochloric acid preparation tank 6 is connected with a crystal seed hydrochloric acid storage tank 8, a pump is arranged between the hydrochloric acid preparation tank 6 and the crystal seed hydrochloric acid storage tank 8, prepared hydrochloric acid with proper concentration is transferred to the crystal seed hydrochloric acid storage tank 8 for standby, and the preparation of the crystal seed hydrochloric acid is completed. In this embodiment, the waste hydrochloric acid storage tank 1, the evaporator 2, the gas-liquid separator 3, the absorption tower 4, the hydrochloric acid storage tank 5, the hydrochloric acid preparation tank 6, the industrial hydrochloric acid storage tank 7, and the seed crystal hydrochloric acid storage tank 8 are made of graphite, so as to prevent corrosion.
According to the material conveying direction, a metatitanic acid storage tank 13, a metatitanic acid metering tank 14, an alkali dissolving pot 15, an alkali dissolving filter press 16, an alkali dissolving pulp making tank 17, an acid dissolving pot 10, an acid dissolving filter press 11 and an acid dissolving pulp making tank 12 are connected in sequence, and a seed crystal hydrochloric acid storage tank 8 is connected with the acid dissolving pot 10 through a seed crystal hydrochloric acid metering tank 9. A steam pipe is arranged in the alkali dissolving pot 15 and used for steam heating, and the alkali dissolving pot 15 is provided with a jacket and can be used for steam heating or sand filtration water cooling and is provided with stirring. The internal materials of the hydrochloric acid metering tank 9 and the acid dissolving pot 10 for the crystal seeds are graphite, and the acid dissolving pot 10 is stirred. The metatitanic acid storage tank 13 transfers the prepared metatitanic acid to a metatitanic acid metering tank 14, the metatitanic acid metering tank 14 transfers the metatitanic acid to an alkali dissolving pot 15 in a specified time period according to actual needs, and the alkali dissolving pot 15 transfers the slurry after the alkali dissolution is completed to an alkali dissolving filter press 16. Feeding the alkali-soluble filter press 16 to an alkali-soluble pulp making tank 17, transferring the pulp to an acid dissolving pot 10 by the alkali-soluble pulp making tank 17, and simultaneously adding dilute hydrochloric acid into the acid dissolving pot 10 by a seed crystal hydrochloric acid metering tank 9; and transferring the prepared slurry to an acid-soluble filter press 11 by an acid-soluble pot 10, discharging the material by the acid-soluble filter press 11, and pulping in an acid-soluble pulping tank 12 to obtain the rutile seed crystal.
By using the production system provided by the embodiment, the specific process for preparing the titanium dioxide seed crystal by using the pesticide waste hydrochloric acid is as follows:
step one, starting the evaporator 2, and controlling the negative pressure of the evaporator 2 within the range of 370-380 Kpa.
And step two, starting a material transferring pump of the waste hydrochloric acid storage tank 1 to supply the waste hydrochloric acid to the evaporator 2.
After 5min, the evaporator 2 starts to supply the mixed gas of HCl and water vapor to the gas-liquid separator 3; a small amount of dilute hydrochloric acid containing HCl is discharged to the waste hydrochloric acid storage tank 1 at the bottom of the evaporator 2.
And step four, after the evaporator 2 supplies steam to the gas-liquid separator 3, the absorption tower 4 is started, after 10min of steam supply, liquid of the gas-liquid separator 3 is separated and transferred to the waste hydrochloric acid storage tank 1, and after 30min of steam supply to the absorption tower 4, the gas-liquid separator 3 transfers the concentrated hydrochloric acid absorbed by the absorption tower 4 to the hydrochloric acid storage tank 5.
Step five, the volume of the hydrochloric acid in the hydrochloric acid storage tank 5 reaches 50m3Rotate 30m later3To a hydrochloric acid preparation tank 6; then the industrial hydrochloric acid storage tank 7 is rotated to 55m3Industrial hydrochloric acid to hydrochloric acid preparation tank 6, stirring for 10min, and measuring the concentration; after the concentration reaches 27.5%, transferring to a hydrochloric acid storage tank 8 for seed crystal for standby.
Step six, the prepared volume is 7.5m3Metatitanic acid (A) is transferred from a metatitanic acid storage tank (13) to a metatitanic acid metering tank (14), and the temperature is raised to 76 ℃.
Step seven, adding 5.2m of alkali dissolving pot 153And (3) heating liquid caustic soda with the mass percent of 49% to 90 ℃.
And eighthly, transferring the heated metatitanic acid in the metatitanic acid metering tank 14 into an alkali dissolving pot 15 (with a jacket) within 30min, heating to 108 ℃, and aging for 2 h.
Step nine, adding desalted water with the same volume as the metatitanic acid into the alkali dissolving pot 15, reducing the temperature, adding sand into the jacket for filtering water, and reducing the temperature of the slurry to 68 ℃.
And step ten, transferring the slurry after the alkali dissolution in the alkali dissolution pot 15 is finished into an alkali dissolution filter press 16, washing until the NaOH content in the filtrate is 3.5g/L, and transferring the filtrate into a filtrate tank.
Step eleven, feeding the materials to an alkali-soluble pulp tank 17, wherein the mass ratio of water to the pulp in the alkali-soluble pulp tank 17 is 7:1, and stirring for 30 min.
Step twelve, the slurry in the alkali-dissolving slurry tank 17 is transferred to 15m3Adding into an acid dissolving pot 10, adding 1.2m hydrochloric acid from a seed crystal metering tank 93Adding dilute hydrochloric acid into acid dissolving pot 10, adjusting pH to 3.0, stirring for 10min, adding dilute hydrochloric acid 0.1m3The pH was measured to be 2.9, and the temperature was raised to 48 ℃.
Thirteen, heating the slurry in the acid dissolving pot 10 to 60 ℃, adding hydrochloric acid again, wherein the hydrochloric acid is about 1.9m3Adjusting the pH value to 0.9; opening a steam valve, continuously heating to 107 ℃ for boiling, heating at the speed of 1 ℃/min, and aging for 120 minutes.
Fourteen, measuring 99.2% and the total titanium concentration is 116 g/L.
And a fifteenth step of transferring the slurry prepared by the acid dissolution pot 10 to an acid dissolution filter press 11, washing to remove unreacted hydrochloric acid, NaCl brought by concentrated hydrochloric acid and NaCl generated by the reaction of NaOH and hydrochloric acid after alkali dissolution, until the NaCl content in the filtrate is 0.6 g/L.
Sixthly, blanking by an acid-soluble filter press 11, pulping in an acid-soluble pulping tank 12, wherein the total titanium concentration is 115g/L, and obtaining the titanium dioxide rutile seed crystal.
The rutile seed crystal obtained by pulping in the embodiment is deionized and can be directly added to a salt treatment process, so that the energy consumption caused by the fact that the seed crystal is added to a hydrolysis process in the traditional process and needs to be subjected to subsequent multi-process production is saved, and the cost is reduced. The addition amount of the obtained titanium dioxide rutile seed crystal in the salt treatment process is 4-7%.
Example 2
The production system for preparing titanium dioxide seed crystals by using pesticide waste hydrochloric acid in the embodiment is basically the same as that in embodiment 1, and the specific process for preparing titanium dioxide seed crystals by using pesticide waste hydrochloric acid in the embodiment is as follows:
step one, the waste hydrochloric acid storage tank 1 supplies waste hydrochloric acid to the evaporator 2 through a material transfer pump, and the negative pressure of the evaporator 2 fluctuates between 350-360 KPa.
Step two, the evaporator 2 supplies the gas-liquid separator 3 with the mixed gas of HCl and water vapor; a small amount of dilute hydrochloric acid containing HCl is discharged to the waste hydrochloric acid storage tank 1 at the bottom of the evaporator 2.
And step three, opening the absorption tower 4 after the gas-liquid separator 3 supplies gas, separating liquid from the gas-liquid separator 3, transferring the liquid to the waste hydrochloric acid storage tank 1, supplying gas to the absorption tower by the gas-liquid separator 3, and transferring the concentrated hydrochloric acid absorbed by the absorption tower 4 to the hydrochloric acid storage tank 5.
Step four, the volume of the hydrochloric acid in the hydrochloric acid storage tank 5 reaches 50m3Rotate 30m later3To a hydrochloric acid preparation tank 6; then the industrial hydrochloric acid storage tank 7 is rotated for 58m3Industrial hydrochloric acid to hydrochloric acid preparation tank 6, stirring for 10min, and measuring the concentration; after the concentration reaches 28%, transferring to a hydrochloric acid storage tank 8 for seed crystal for standby.
Step five, preparing the prepared 7.5m3Metatitanic acid is transferred from a metatitanic acid storage tank 13 to a metatitanic acid metering tank 14, and the temperature is raised to 76 ℃.
Step six, adding 5.2m into an alkali dissolving pot 153Liquid caustic soda with the mass percent of 49 percent is heated to 90 ℃.
And seventhly, transferring the heated metatitanic acid in the metatitanic acid metering tank 14 into an alkali dissolving pot 15 (with a jacket) within 30min, heating to 108 ℃, and aging for 2 h.
Step eight, adding desalted water with the same volume as the metatitanic acid into the alkali dissolving pot 15, reducing the temperature, adding sand filter water into the jacket, and reducing the temperature of the slurry to 65 ℃.
And step nine, transferring the slurry after the alkali dissolution in the alkali dissolution pot 15 is finished into an alkali dissolution filter press 16, washing until the NaOH content in the filtrate is measured to be 2.3g/L, and transferring the filtrate into a filtrate tank.
And step ten, blanking to an alkali-soluble pulp tank 17, wherein the mass ratio of water to the pulp in the alkali-soluble pulp tank 17 is 7:1, and stirring for 30 min.
Step eleven, transferring the slurry in the alkali-dissolving slurry tank 17 to 15m3Adding into an acid dissolving pot 10, adding 1.3m hydrochloric acid from a seed crystal metering tank 93Adding dilute hydrochloric acid into acid dissolving pot 10, adjusting pH to 2.5, stirring for 10min, measuring pH to 2.8, and heating to 46 deg.C.
Step twelve, heating the slurry in the acid dissolution pot 10 to 60 ℃, and adding hydrochloric acid 2.0m again3Adjusting the pH value to 0.7; opening a steam valve, continuously heating to 106 ℃ for boiling, heating at the speed of 1 ℃/min, and aging for 120 minutes.
Step thirteen, the conversion rate R is measured to be 99.5 percent, and the total titanium concentration is measured to be 115 g/L.
And step fourteen, transferring the slurry prepared by the acid dissolution pot 10 to an acid dissolution filter press 11, and washing until the NaCl content in the filtrate is 0.4 g/L.
And step fifteen, blanking by an acid-soluble filter press 11, pulping in an acid-soluble pulping tank 12, wherein the total titanium concentration is 116g/L, and obtaining the titanium dioxide rutile seed crystal.
Example 3
The production system for preparing titanium dioxide seed crystals by using pesticide waste hydrochloric acid in the embodiment is basically the same as that in embodiment 1, and the specific process for preparing titanium dioxide seed crystals by using pesticide waste hydrochloric acid in the embodiment is as follows:
step one, the waste hydrochloric acid storage tank 1 supplies waste hydrochloric acid to the evaporator 2 through a material transfer pump, and the negative pressure of the evaporator 2 fluctuates between 300 and 400 KPa.
Step two, the evaporator 2 supplies the gas-liquid separator 3 with the mixed gas of HCl and water vapor; a small amount of dilute hydrochloric acid containing HCl is discharged to the waste hydrochloric acid storage tank 1 at the bottom of the evaporator 2.
And step three, opening the absorption tower 4 after the gas-liquid separator 3 supplies gas, separating liquid from the gas-liquid separator 3, transferring the liquid to the waste hydrochloric acid storage tank 1, supplying gas to the absorption tower by the gas-liquid separator 3, and transferring the concentrated hydrochloric acid absorbed by the absorption tower 4 to the hydrochloric acid storage tank 5.
Step four, the volume of the hydrochloric acid in the hydrochloric acid storage tank 5 reaches 50m3Rotate 30m later3To a hydrochloric acid preparation tank 6; then the industrial hydrochloric acid storage tank 7 is rotated for 30m3Industrial hydrochloric acid to hydrochloric acid preparation tank 6, stirring for 10min, and measuring the concentration; after the concentration reaches 25%, transferring to a hydrochloric acid storage tank 8 for seed crystal for standby.
Step five, preparing the prepared 7.5m3Metatitanic acid is transferred from a metatitanic acid storage tank 13 to a metatitanic acid metering tank 14, and the temperature is raised to 80 ℃.
Step six, adding 5.2m into an alkali dissolving pot 153Liquid caustic soda with the mass percent of 49 percent is heated to 95 ℃.
And seventhly, transferring the heated metatitanic acid in the metatitanic acid metering tank 14 into an alkali dissolving pot 15 (with a jacket) within 30min, heating to 108 ℃, and aging for 2 h.
Step eight, adding desalted water with the same volume as the metatitanic acid into the alkali dissolving pot 15, reducing the temperature, adding sand into the jacket for filtering water, and reducing the temperature of the slurry to 60 ℃.
And step nine, transferring the slurry after the alkali dissolution in the alkali dissolution pot 15 is finished into an alkali dissolution filter press 16, washing until the NaOH content in the filtrate is measured to be 2.8g/L, and transferring the filtrate into a filtrate tank.
And step ten, blanking to an alkali-soluble pulp tank 17, wherein the mass ratio of water to the pulp in the alkali-soluble pulp tank 17 is 7:1, and stirring for 30 min.
Step eleven, transferring the slurry in the alkali-dissolving slurry tank 17 to 15m3Adding into an acid dissolving pot 10, adding 1.3m hydrochloric acid from a seed crystal metering tank 93Adding dilute hydrochloric acid into acid dissolving pot 10, adjusting pH to 2.5, stirring for 10min, measuring pH to 2.8, and heating to 46 deg.C.
Step twelve, heating the slurry in the acid dissolution pot 10 to 65 ℃, and adding hydrochloric acid 1.2m again3Adjusting the pH value to 1.0; and opening a steam valve, continuously heating to 110 ℃ for boiling, heating at the speed of 1 ℃/min, and aging for 120 minutes.
Step thirteen, the conversion rate R is measured to be 98.7 percent, and the total titanium concentration is measured to be 110 g/L.
And step fourteen, transferring the slurry prepared by the acid dissolution pot 10 to an acid dissolution filter press 11, and washing until the NaCl content in the filtrate is 0.2 g/L.
And step fifteen, blanking by an acid-soluble filter press 11, pulping in an acid-soluble pulping tank 12, wherein the total titanium concentration is 113g/L, and obtaining the titanium dioxide rutile seed crystal.
Example 4
The production system for preparing titanium dioxide seed crystals by using pesticide waste hydrochloric acid in the embodiment is basically the same as that in embodiment 1, and the specific process for preparing titanium dioxide seed crystals by using pesticide waste hydrochloric acid in the embodiment is as follows:
step one, the waste hydrochloric acid storage tank 1 supplies waste hydrochloric acid to the evaporator 2 through a material transfer pump, and the negative pressure of the evaporator 2 fluctuates between 320 and 350 KPa.
Step two, the evaporator 2 supplies the gas-liquid separator 3 with the mixed gas of HCl and water vapor; a small amount of dilute hydrochloric acid containing HCl is discharged to the waste hydrochloric acid storage tank 1 at the bottom of the evaporator 2.
And step three, opening the absorption tower 4 after the gas-liquid separator 3 supplies gas, separating liquid from the gas-liquid separator 3, transferring the liquid to the waste hydrochloric acid storage tank 1, supplying gas to the absorption tower by the gas-liquid separator 3, and transferring the concentrated hydrochloric acid absorbed by the absorption tower 4 to the hydrochloric acid storage tank 5.
Step four, the volume of the hydrochloric acid in the hydrochloric acid storage tank 5 reaches 50m3Rotate 30m later3To a hydrochloric acid preparation tank 6; then the industrial hydrochloric acid storage tank 7 is rotated for 60m3Industrial hydrochloric acid to hydrochloric acid preparation tank 6, stirring for 10min, and measuring the concentration; after the concentration reaches 31%, transferring to a hydrochloric acid storage tank 8 for seed crystal for standby.
Step five, preparing the prepared 7.5m3Metatitanic acid is transferred from a metatitanic acid storage tank 13 to a metatitanic acid metering tank 14, and the temperature is raised to 60 ℃.
Step six, adding 5.2m into an alkali dissolving pot 15349 percent of liquid caustic soda by mass percent, and heating to 75 ℃.
And seventhly, transferring the heated metatitanic acid in the metatitanic acid metering tank 14 into an alkali dissolving pot 15 (with a jacket) within 30min, heating to 108 ℃, and aging for 2 h.
Step eight, adding desalted water with the same volume as the metatitanic acid into the alkali dissolving pot 15, reducing the temperature, adding sand into the jacket for filtering water, and reducing the temperature of the slurry to 70 ℃.
And step nine, transferring the slurry after the alkali dissolution in the alkali dissolution pot 15 is finished into an alkali dissolution filter press 16, washing until the NaOH content in the filtrate is 3.8g/L, and transferring the filtrate into a filtrate tank.
And step ten, blanking to an alkali-soluble pulp tank 17, wherein the mass ratio of water to the pulp in the alkali-soluble pulp tank 17 is 7:1, and stirring for 30 min.
Step eleven, transferring the slurry in the alkali-dissolving slurry tank 17 to 15m3To an acid dissolution pot 10, a hydrochloric acid metering tank 9 for seed crystalAdding 1.3m3Adding dilute hydrochloric acid into acid dissolving pot 10, adjusting pH to 2.5, stirring for 10min, measuring pH to 2.8, and heating to 46 deg.C.
Step twelve, heating the slurry in the acid dissolution pot 10 to 60 ℃, and adding hydrochloric acid again to adjust the pH value to 0.6; opening a steam valve, continuously heating to 100 ℃ for boiling, heating at the speed of 1 ℃/min, and aging for 120 minutes.
Step thirteen, the conversion rate R is measured to be 99.1 percent, and the total titanium concentration is measured to be 114 g/L.
And step fourteen, transferring the slurry prepared by the acid dissolution pot 10 to an acid dissolution filter press 11, and washing until the NaCl content in the filtrate is 0.2 g/L.
And step fifteen, blanking by an acid-soluble filter press 11, pulping in an acid-soluble pulping tank 12, wherein the total titanium concentration is 115g/L, and obtaining the titanium dioxide rutile seed crystal.
The present invention and its embodiments have been described above schematically, without limitation, and what is shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.
Claims (1)
1. A method for preparing titanium dioxide seed crystals by using chlorination waste acid is characterized by comprising the following steps: the operation comprises three parts of concentration of waste hydrochloric acid, preparation of hydrochloric acid for seed crystals and preparation of titanium dioxide seed crystals, the pesticide waste hydrochloric acid is purified and absorbed to obtain a concentrated hydrochloric acid solution, the industrial hydrochloric acid and the concentrated hydrochloric acid solution are mixed and prepared according to the proportion of 1:1-2:1, and the obtained hydrochloric acid for the seed crystals is prepared to be used in an acid dissolving process of the preparation of the titanium dioxide seed crystals; the production system for preparing the titanium dioxide seed crystal comprises a waste hydrochloric acid concentration unit, a seed crystal hydrochloric acid configuration unit and a titanium dioxide seed crystal preparation unit, wherein the waste hydrochloric acid concentration unit is connected with the seed crystal hydrochloric acid configuration unit, the waste hydrochloric acid concentration unit purifies and absorbs pesticide waste hydrochloric acid and inputs the pesticide waste hydrochloric acid into the seed crystal hydrochloric acid configuration unit, an output pipeline of the seed crystal hydrochloric acid configuration unit is connected with an acid dissolving pot (10) of the titanium dioxide seed crystal preparation unit, and the seed crystal hydrochloric acid configured by the seed crystal hydrochloric acid configuration unit is input into the acid dissolving pot (10);
the waste hydrochloric acid concentration unit comprises a waste hydrochloric acid storage tank (1), an evaporator (2), a gas-liquid separator (3), an absorption tower (4) and a hydrochloric acid storage tank (5), wherein the waste hydrochloric acid storage tank (1) is connected with the evaporator (2), the top of the evaporator (2) is connected with the gas-liquid separator (3), the upper part of the gas-liquid separator (3) is connected with the absorption tower (4), and the bottom of the absorption tower (4) is connected with the hydrochloric acid storage tank (5); the horizontal position of the evaporator (2) is higher than the waste hydrochloric acid storage tank (1), and the bottom of the evaporator (2) is connected with a pipeline to the waste hydrochloric acid storage tank (1); the bottom of the gas-liquid separator (3) is also connected with a pipeline to the waste hydrochloric acid storage tank (1);
the hydrochloric acid preparation unit for the seed crystal comprises a hydrochloric acid preparation tank (6), an industrial hydrochloric acid storage tank (7) and a hydrochloric acid storage tank (8) for the seed crystal, wherein the hydrochloric acid storage tank (5) is connected with the hydrochloric acid preparation tank (6), the industrial hydrochloric acid storage tank (7) is also connected with the hydrochloric acid preparation tank (6), and the lower end of the hydrochloric acid preparation tank (6) is connected with the hydrochloric acid storage tank (8) for the seed crystal;
the titanium dioxide seed crystal preparation unit comprises an acid dissolving pot (10), an acid dissolving filter press (11), an acid dissolving pulping tank (12), a metatitanic acid storage tank (13), a metatitanic acid metering tank (14), an alkali dissolving pot (15), an alkali dissolving filter press (16) and an alkali dissolving pulping tank (17); according to the conveying direction of materials, a metatitanic acid storage tank (13), a metatitanic acid metering tank (14), an alkali dissolving pot (15), an alkali dissolving filter press (16), an alkali dissolving pulping tank (17), an acid dissolving pot (10), an acid dissolving filter press (11) and an acid dissolving pulping tank (12) are sequentially connected, and a crystal seed is connected with the acid dissolving pot (10) through a crystal seed hydrochloric acid storage tank (8) and a crystal seed hydrochloric acid metering tank (9);
the concentration of the pesticide waste hydrochloric acid and the preparation of the hydrochloric acid for the seed crystal comprise the following specific processes:
step one, starting an evaporator (2), and controlling the negative pressure of the evaporator (2) to be between 300 and 400 KPa;
step two, starting a material transferring pump of the waste hydrochloric acid storage tank (1) to supply waste hydrochloric acid to the evaporator (2);
step three, after supplying acid for a period of time, the evaporator (2) starts to supply the mixed gas of HCl and water vapor to the gas-liquid separator (3);
step four, the evaporator (2) supplies steam to the gas-liquid separator (3), then the absorption tower (4) is opened, and after the steam is supplied for a period of time, the liquid of the gas-liquid separator (3) is separated out and transferred to the waste hydrochloric acid storage tank (1); after the gas-liquid separator (3) supplies steam to the absorption tower (4) for a period of time, transferring the concentrated hydrochloric acid absorbed by the absorption tower (4) to a hydrochloric acid storage tank (5);
step five, the volume of the concentrated hydrochloric acid in the hydrochloric acid storage tank (5) reaches 50m3Rotate 30m later3To a hydrochloric acid preparation tank (6); then the industrial hydrochloric acid storage tank (7) is rotated by 30m3-60m3Preparing the industrial hydrochloric acid into a hydrochloric acid preparation tank (6), and measuring the concentration of the hydrochloric acid after stirring for a period of time; transferring the crystal seeds to a hydrochloric acid storage tank (8) when the concentration reaches 25-31% for later use;
the specific process for preparing the titanium dioxide seed crystal comprises the following steps:
step one, transferring the prepared metatitanic acid from a metatitanic acid storage tank (13) to a metatitanic acid metering tank (14), and heating to 60-80 ℃;
secondly, adding liquid alkali with a certain volume mass percentage concentration of 49% into an alkali dissolving pot (15), and heating to 75-95 ℃;
step three, transferring the heated metatitanic acid in the metatitanic acid metering tank (14) into an alkali dissolving pot (15), heating to 108 ℃, and aging for 2 hours;
step four, adding desalted water with the same volume as the metatitanic acid into an alkali dissolving pot (15), reducing the temperature, adding sand into a jacket of the alkali dissolving pot (15) to filter water, and reducing the temperature of the slurry to 60-70 ℃;
transferring the slurry after the alkali dissolution in the alkali dissolution pot (15) to an alkali dissolution filter press (16), washing with deionized water until the NaOH content in the filtrate is less than 5g/L, and transferring the filtrate to a filtrate tank;
step six, transferring the slurry in the alkali-soluble filter press (16) into an alkali-soluble slurry making tank (17), wherein the mass ratio of water to the slurry in the alkali-soluble slurry making tank (17) is 7:1, and continuously stirring for a period of time;
step seven, transferring the slurry in the alkali dissolving slurry tank (17) to an acid dissolving pot (10), adding dilute hydrochloric acid from a crystal seed hydrochloric acid metering tank (9) to the acid dissolving pot (10), adjusting the pH to be less than 3.1, stirring for a period of time, then adding dilute hydrochloric acid to ensure that the pH is less than 3.1, and heating to 40-50 ℃;
step eight, heating the slurry in the acid dissolving pot (10) to 60-65 ℃, and adding hydrochloric acid again to adjust the pH value to 0-1.0; continuously heating to 100 ℃ and 110 ℃, and aging for 120 minutes; heating to the acid dissolution temperature of 100 ℃ and 110 ℃ at the temperature rise range of 1 ℃/min in the acid dissolution process to be in a boiling state;
step nine, measuring the rutile conversion rate R to be more than 98.5 percent and the total titanium concentration to be 110-120g/L, transferring the slurry prepared by the acid-soluble pot (10) to an acid-soluble filter press (11), and washing with deionized water until the NaCl content in the filtrate is lower than 1 g/L;
step ten, blanking by an acid-soluble filter press (11), pulping in an acid-soluble pulping tank (12), and controlling the total titanium concentration to be 110-.
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| CN108516582B (en) * | 2018-04-28 | 2020-09-18 | 南京钛白化工有限责任公司 | Preparation method of high-weather-resistance nano rutile titanium dioxide |
| CN113120863A (en) * | 2021-04-22 | 2021-07-16 | 南通三圣石墨设备科技股份有限公司 | Hydrochloric acid method for recycling titanium dioxide hydrochloric acid |
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| CN202193614U (en) * | 2011-08-08 | 2012-04-18 | 常州化工设备有限公司 | Processing equipment for concentrating and recycling hydrochloric acid |
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Denomination of invention: A method for preparing titanium dioxide crystal seed by using chlorinated waste acid Effective date of registration: 20210924 Granted publication date: 20200505 Pledgee: China Co. truction Bank Corp Ma'anshan branch Pledgor: ANHUI VENUS TITANIUM DIOXIDE (Group) Co.,Ltd. Registration number: Y2021980009723 |
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Date of cancellation: 20221024 Granted publication date: 20200505 Pledgee: China Co. truction Bank Corp Ma'anshan branch Pledgor: Anhui Venus Titanium Dioxide (Group) Co.,Ltd. Registration number: Y2021980009723 |