CN112723411A - Production process of titanium dioxide by sulfuric acid process - Google Patents
Production process of titanium dioxide by sulfuric acid process Download PDFInfo
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- CN112723411A CN112723411A CN202011616151.1A CN202011616151A CN112723411A CN 112723411 A CN112723411 A CN 112723411A CN 202011616151 A CN202011616151 A CN 202011616151A CN 112723411 A CN112723411 A CN 112723411A
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- titanium
- sulfuric acid
- liquid
- titanium dioxide
- titanium liquid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
- C01G23/0534—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts in the presence of seeds
Abstract
The invention discloses a production process of titanium dioxide by a sulfuric acid method, which comprises the following raw material components of concentrated sulfuric acid with the concentration of 98%, titanium concentrate with the purity of 45-48% and high-titanium slag with the purity of 70-75%, wherein the raw material components are 65-70% of concentrated sulfuric acid, 13-17% of titanium concentrate and 13-17% of titanium concentrate respectively. The invention relates to a production process of titanium dioxide by a sulfuric acid method, which comprises the steps of preheating titanium liquid, injecting the titanium liquid into a half of a seed crystal, adding the titanium liquid into a hydrolysis pot gradually, stirring continuously, improving the hydrolysis efficiency of the titanium liquid, heating the titanium liquid again through external steam until the titanium liquid is boiled after the titanium liquid is added, further improving the hydrolysis efficiency of the titanium liquid, absorbing, dedusting and cooling waste gas generated in the acidolysis process through an alkaline water spray tower, spraying and absorbing through venturi clear water, treating through deodorization equipment and a demisting tower, discharging after reaching the standard, and reducing the pollution of the waste gas generated in the acidolysis process to air.
Description
Technical Field
The invention particularly relates to a production process of titanium dioxide by a sulfuric acid method.
Background
Titanium dioxide is an important inorganic chemical pigment, and the main component is titanium dioxide. The production process of titanium dioxide comprises two process routes of a sulfuric acid method and a chlorination method. The titanium dioxide has important application in the industries of paint, ink, paper making, plastic rubber, chemical fiber, ceramic and the like, the relative density of the titanium dioxide is the smallest in common white pigment, the surface area of the titanium dioxide is the largest and the pigment volume is the highest in white pigment with the same mass, and the titanium dioxide has excellent electrical property due to higher dielectric constant.
In the existing technology for producing titanium dioxide by a sulfuric acid method, certain waste gas is generated in the acidolysis and calcination processes, the waste gas is directly discharged to cause certain pollution, and the hydrolysis efficiency is low in the hydrolysis process of titanium liquid. Therefore, we improve the technology and propose a production technology of titanium dioxide by a sulfuric acid method.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a production process of titanium dioxide by a sulfuric acid method.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention relates to a production process of titanium dioxide by a sulfuric acid method, which comprises the following raw material components of concentrated sulfuric acid with the concentration of 98%, titanium concentrate with the purity of 45-48% and high-titanium slag with the purity of 70-75%, wherein the raw material components are 65-70% of concentrated sulfuric acid, 13-17% of titanium concentrate and 13-17% of titanium concentrate respectively.
The invention relates to a production process of titanium dioxide by a sulfuric acid method, which comprises the following steps:
s1: grinding the titanium concentrate and the high titanium slag through a ball mill to obtain titanium concentrate and high titanium slag powder;
s2: conveying the powder obtained in the step S1 to an acidolysis tank to be mixed with concentrated sulfuric acid for acidolysis, and heating and welding the acidolysis tank through steam to obtain titanium liquid;
s3: adding a flocculating agent into the titanium liquid obtained in the step S2 for precipitation, and then performing precipitation treatment through a multistage sedimentation tank to obtain a supernatant;
s4: hydrolyzing the supernatant obtained in the step S3 to obtain metatitanic acid;
s5: filtering the metatitanic acid obtained in the step S4 by a liquid filter to remove iron;
s6: adding salt into the titanium liquid subjected to iron removal in the step S4;
s7: calcining and dehydrating the titanium liquid treated in the step S6 through a rotary kiln to obtain a primary titanium dioxide product, and rolling and grinding to obtain powdery titanium dioxide;
s8: and (5) drying the titanium dioxide obtained in the step (S7) by using drying equipment, and then packaging to obtain a titanium dioxide finished product.
As a preferred technical scheme of the invention, the raw material composition ratio is 68% of concentrated sulfuric acid, 16% of titanium concentrate and 16% of titanium concentrate respectively.
As a preferred technical scheme of the invention, the waste gas generated in the acidolysis process of the step S2 is treated by firstly absorbing, dedusting and cooling through an alkaline water spray tower, then spraying and absorbing through venturi clear water, finally treating through deodorization equipment and a demisting tower, and discharging after reaching the standard.
As a preferred technical solution of the present invention, the step of hydrolyzing the supernatant of step S3 comprises:
1. preheating the titanium liquid to 85 ℃, then gradually adding the titanium liquid into a hydrolysis pot, and continuously stirring the titanium liquid through stirring equipment;
2. when the titanium liquid is added by half, seed crystal titanyl sulfate is added into the titanium liquid, the concentration of the seed crystal is 75-85g/L, and the addition amount is 1.5-2% of the titanium liquid;
3. and after the titanium liquid is completely added, continuously heating the hydrolysis kettle by steam until the titanium liquid is heated to be boiling, and then keeping for 3-4h to complete hydrolysis.
As a preferred technical scheme of the invention, the salts added in the step S6 are phosphoric acid, potassium hydroxide and aluminum sulfate, and the color phase and the looseness of the titanium dioxide are increased by adding the phosphoric acid, the potassium hydroxide and the aluminum sulfate.
As a preferred technical scheme of the invention, the tail gas generated by calcining in the step S7 is treated, large-particle materials are recovered by settling through a settling box, small materials are recovered by cyclone dust removal, dust removal and temperature reduction are performed by primary and secondary venturi spraying, then absorption is performed through a lime water spraying tower, and finally fine adjustment is performed through a weak alkali absorption tower, and the tail gas is discharged after reaching the standard.
The invention has the beneficial effects that: the production process of the titanium dioxide by the sulfuric acid method comprises the following steps:
1. waste gas generated in the acidolysis process is firstly absorbed, dedusted and cooled by an alkaline water spray tower, then is sprayed and absorbed by venturi clear water, and finally is treated by deodorization equipment and a demisting tower, and is discharged after reaching the standard, so that the pollution of the waste gas generated in the acidolysis process to air can be reduced;
2. the tail gas that will calcine the production subsides the material of retrieving great granule through the setting bin earlier, and the less material is retrieved in the dust removal of rethread cyclone, and rethread one-level and second grade venturi spray and remove dust and cool down, then absorb through the lime water spray column, and the light alkali absorption tower of rethread is fine setting at last, discharges after up to standard again, can reduce the pollution of the waste gas that the calcination process produced to the air.
3. The titanium liquid is preheated firstly, then the titanium liquid is injected into a half of the hydrolysis kettle, the seed crystal is added, the titanium liquid is gradually added into the hydrolysis kettle and is continuously stirred, the hydrolysis efficiency of the titanium liquid can be improved, and after the titanium liquid is added, the titanium liquid is heated again through external steam until boiling, so that the hydrolysis efficiency of the titanium liquid can be further improved.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example (b): the invention relates to a production process of titanium dioxide by a sulfuric acid method, which comprises the following raw material components of concentrated sulfuric acid with the concentration of 98%, titanium concentrate with the purity of 46% and high-titanium slag with the purity of 73%, wherein the raw material components are respectively 68% of the concentrated sulfuric acid, 16% of the titanium concentrate and 16% of the titanium concentrate.
The invention relates to a production process of titanium dioxide by a sulfuric acid method, which comprises the following steps:
s1: grinding the titanium concentrate and the high titanium slag through a ball mill to obtain titanium concentrate and high titanium slag powder;
s2: conveying the powder obtained in the step S1 to an acidolysis tank to be mixed with concentrated sulfuric acid for acidolysis, and heating and welding the acidolysis tank through steam to obtain titanium liquid;
s3: adding a flocculating agent into the titanium liquid obtained in the step S2 for precipitation, and then performing precipitation treatment through a multistage sedimentation tank to obtain a supernatant;
s4: hydrolyzing the supernatant obtained in the step S3 to obtain metatitanic acid;
s5: filtering the metatitanic acid obtained in the step S4 by a liquid filter to remove iron;
s6: adding salt into the titanium liquid subjected to iron removal in the step S4;
s7: calcining and dehydrating the titanium liquid treated in the step S6 through a rotary kiln to obtain a primary titanium dioxide product, and rolling and grinding to obtain powdery titanium dioxide;
s8: and (5) drying the titanium dioxide obtained in the step (S7) by using drying equipment, and then packaging to obtain a titanium dioxide finished product.
Wherein, to the waste gas treatment that the acidolysis process of step S2 produced, absorb, remove dust and cool down through the buck spray tower earlier, rethread venturi clear water sprays the absorption, and at last rethread deodorization equipment and defogging tower are handled, discharge after reaching standard again.
Wherein, the step of hydrolyzing the supernatant in the step S3 comprises the following steps:
1. preheating the titanium liquid to 85 ℃, then gradually adding the titanium liquid into a hydrolysis pot, and continuously stirring the titanium liquid through stirring equipment;
2. when the titanium liquid is added by half, seed crystal titanyl sulfate is added into the titanium liquid, the concentration of the seed crystal is 75-85g/L, and the addition amount is 1.5-2% of the titanium liquid;
3. and after the titanium liquid is completely added, continuously heating the hydrolysis kettle by steam until the titanium liquid is heated to be boiling, and then keeping for 3-4h to complete hydrolysis.
Wherein, the salt added in the step S6 is phosphoric acid, potassium hydroxide and aluminum sulfate, and the color phase and the looseness of the titanium dioxide are increased by adding the phosphoric acid, the potassium hydroxide and the aluminum sulfate.
Wherein, to the tail gas processing of step S7 calcination production, subside the material of retrieving great granule through the setting bin earlier, the rethread whirlwind removes dust and retrieves less material, and rethread one-level and second grade venturi spray and remove dust and cool down, then absorb through the lime water spray column, at last rethread light alkali absorption tower fine setting, discharge after reaching standard again.
Waste gas generated in the acidolysis process is firstly absorbed, dedusted and cooled by an alkaline water spray tower, then is sprayed and absorbed by venturi clear water, and finally is treated by deodorization equipment and a demisting tower, and is discharged after reaching the standard, so that the pollution of the waste gas generated in the acidolysis process to air can be reduced;
the tail gas generated by calcination is firstly settled through a settling tank to recover large-particle materials, then is dedusted through cyclone to recover small-particle materials, is dedusted and cooled through primary and secondary venturi spraying, is absorbed through a lime water spraying tower, is finely adjusted through a weak base absorption tower, is discharged after reaching the standard, and can reduce the pollution of the waste gas generated in the calcination process to the air;
the titanium liquid is preheated firstly, then the titanium liquid is injected into a half of the hydrolysis kettle, the seed crystal is added, the titanium liquid is gradually added into the hydrolysis kettle and is continuously stirred, the hydrolysis efficiency of the titanium liquid can be improved, and after the titanium liquid is added, the titanium liquid is heated again through external steam until boiling, so that the hydrolysis efficiency of the titanium liquid can be further improved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The production process of titanium dioxide by a sulfuric acid method is characterized in that raw material components comprise 98% concentrated sulfuric acid, 45-48% titanium concentrate and 70-75% high-titanium slag, and the raw material components respectively comprise 65-70% concentrated sulfuric acid, 13-17% titanium concentrate and 13-17% titanium concentrate.
2. The production process of titanium dioxide by sulfuric acid process according to claim 1, characterized by comprising the steps of:
s1: grinding the titanium concentrate and the high titanium slag through a ball mill to obtain titanium concentrate and high titanium slag powder;
s2: conveying the powder obtained in the step S1 to an acidolysis tank to be mixed with concentrated sulfuric acid for acidolysis, and heating and welding the acidolysis tank through steam to obtain titanium liquid;
s3: adding a flocculating agent into the titanium liquid obtained in the step S2 for precipitation, and then performing precipitation treatment through a multistage sedimentation tank to obtain a supernatant;
s4: hydrolyzing the supernatant obtained in the step S3 to obtain metatitanic acid;
s5: filtering the metatitanic acid obtained in the step S4 by a liquid filter to remove iron;
s6: adding salt into the titanium liquid subjected to iron removal in the step S4;
s7: calcining and dehydrating the titanium liquid treated in the step S6 through a rotary kiln to obtain a primary titanium dioxide product, and rolling and grinding to obtain powdery titanium dioxide;
s8: and (5) drying the titanium dioxide obtained in the step (S7) by using drying equipment, and then packaging to obtain a titanium dioxide finished product.
3. The process according to claim 1, wherein the raw material composition ratio is 68% of concentrated sulfuric acid, 16% of titanium concentrate and 16% of titanium concentrate.
4. The process of claim 2, wherein the waste gas generated in the acidolysis step S2 is treated by absorption, dust removal and temperature reduction in an alkaline water spray tower, venturi clean water spray absorption, deodorization and demisting tower, and is discharged after reaching standards.
5. The process for producing titanium dioxide by a sulfuric acid process according to claim 2, wherein the step of hydrolyzing the supernatant of the step S3 is:
1. preheating the titanium liquid to 85 ℃, then gradually adding the titanium liquid into a hydrolysis pot, and continuously stirring the titanium liquid through stirring equipment;
2. when the titanium liquid is added by half, seed crystal titanyl sulfate is added into the titanium liquid, the concentration of the seed crystal is 75-85g/L, and the addition amount is 1.5-2% of the titanium liquid;
3. and after the titanium liquid is completely added, continuously heating the hydrolysis kettle by steam until the titanium liquid is heated to be boiling, and then keeping for 3-4h to complete hydrolysis.
6. The process for producing titanium dioxide by the sulfuric acid process according to claim 2, wherein the salts added in step S6 are phosphoric acid, potassium hydroxide and aluminum sulfate, and the color phase and the degree of crunchiness of titanium dioxide are increased by adding phosphoric acid, potassium hydroxide and aluminum sulfate.
7. The process for producing titanium dioxide by a sulfuric acid process according to claim 2, wherein the tail gas generated by calcining in step S7 is treated by settling and recovering large-particle materials through a settling tank, dedusting and recovering small materials through cyclone, dedusting and cooling through primary and secondary venturi spraying, absorbing through a lime water spray tower, fine-adjusting through a weak alkali absorption tower, and discharging after reaching the standard.
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Citations (5)
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| JP2003277055A (en) * | 2002-03-25 | 2003-10-02 | Tayca Corp | Method for purifying sulfuric acid digesting solution of iron titanate |
| CN106186054A (en) * | 2016-06-30 | 2016-12-07 | 广西金茂钛业有限公司 | A kind of method preparing ceramic pigment titanium dioxide |
| CN106241868A (en) * | 2016-08-31 | 2016-12-21 | 攀枝花大互通钛业有限公司 | A kind of titanium dioxide and preparation method thereof |
| CN107413149A (en) * | 2017-06-26 | 2017-12-01 | 哥乐巴环保科技(上海)有限公司 | A kind of MDF dries the modified technique and processing system of tail gas biochemical processing method |
| CN108423710A (en) * | 2018-05-04 | 2018-08-21 | 广西金茂钛业有限公司 | A kind of sulfuric acid process colorant enamel grade titanium dioxide powder, preparation method thereof |
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2020
- 2020-12-30 CN CN202011616151.1A patent/CN112723411A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003277055A (en) * | 2002-03-25 | 2003-10-02 | Tayca Corp | Method for purifying sulfuric acid digesting solution of iron titanate |
| CN106186054A (en) * | 2016-06-30 | 2016-12-07 | 广西金茂钛业有限公司 | A kind of method preparing ceramic pigment titanium dioxide |
| CN106241868A (en) * | 2016-08-31 | 2016-12-21 | 攀枝花大互通钛业有限公司 | A kind of titanium dioxide and preparation method thereof |
| CN107413149A (en) * | 2017-06-26 | 2017-12-01 | 哥乐巴环保科技(上海)有限公司 | A kind of MDF dries the modified technique and processing system of tail gas biochemical processing method |
| CN108423710A (en) * | 2018-05-04 | 2018-08-21 | 广西金茂钛业有限公司 | A kind of sulfuric acid process colorant enamel grade titanium dioxide powder, preparation method thereof |
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