CN115432733A - Method for preparing metatitanic acid with narrow particle size distribution - Google Patents
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- CN115432733A CN115432733A CN202211273287.6A CN202211273287A CN115432733A CN 115432733 A CN115432733 A CN 115432733A CN 202211273287 A CN202211273287 A CN 202211273287A CN 115432733 A CN115432733 A CN 115432733A
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- seed crystal
- particle size
- metatitanic acid
- size distribution
- hydrolysis
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- 239000002245 particle Substances 0.000 title claims abstract description 70
- 239000002253 acid Substances 0.000 title claims abstract description 42
- 238000009826 distribution Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 71
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 61
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 230000007062 hydrolysis Effects 0.000 claims abstract description 51
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000010936 titanium Substances 0.000 claims abstract description 45
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000002270 dispersing agent Substances 0.000 claims abstract description 32
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 26
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 235000010981 methylcellulose Nutrition 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000001556 precipitation Methods 0.000 abstract description 5
- 230000006399 behavior Effects 0.000 abstract description 3
- 238000004220 aggregation Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000004886 process control Methods 0.000 description 5
- 230000001186 cumulative effect Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- IXQWNVPHFNLUGD-UHFFFAOYSA-N iron titanium Chemical compound [Ti].[Fe] IXQWNVPHFNLUGD-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for preparing metatitanic acid with narrow particle size distribution, belonging to the technical field of titanium dioxide manufacturing. The method may comprise the steps of: preparing hydrolysis seed crystal: adding a seed crystal dispersing agent into a solution with the titanium dioxide concentration of 120-150 g/L to prepare a seed crystal solution, wherein the addition amount of the seed crystal dispersing agent is 0.30kg/m 3 ～1.20kg/m 3 (ii) a Preheating industrial titanium liquid with the concentration of 180-210 g/L to 94-100 ℃; adding 1.5-3.0% of seed crystal solution into the preheated industrial titanium liquid, and then performing hydrolysis according to the control conditions of the conventional hydrolysis process until the hydrolysis reaction is finished to obtain the metatitanic acid with narrow particle size distribution. The method for preparing the metatitanic acid with narrow particle size distribution by adjusting the hydrolysis conditions effectively controls the precipitation and aggregation behaviors of the metatitanic acid in the hydrolysis process, and the prepared metatitanic acid has the advantages of small particle size, narrow particle size distribution, simple process, convenience in operation and wide popularization and application.
Description
Technical Field
The invention relates to a method for preparing metatitanic acid with narrow particle size distribution, belonging to the technical field of titanium dioxide manufacturing.
Background
The sulfuric acid method titanium dioxide process is one of the main methods for industrially preparing titanium dioxide, and is in the leading position in China at present. The hydrolysis process in the titanium dioxide production process by the sulfuric acid method directly influences the composition, structure and particle size distribution of the hydrolyzed metatitanic acid, and finally influences the structure and performance of the titanium dioxide product. The hydrolysis process and the precipitation of metatitanic acid are influenced by hydrolysis conditions such as the number of hydrolysis seed crystals, and the precipitation process and the particle size distribution of the hydrolyzed metatitanic acid are determined. The hydrolysis seed crystal particles are fine and are easy to adsorb and agglomerate, so that the activity of the hydrolysis seed crystal is reduced, a good induction effect on the hydrolysis process cannot be achieved, and the composition structure and the particle size distribution of the hydrolysis metatitanic acid are influenced. The titanium dioxide product prepared by the sulfuric acid process has the expected particle size of the titanium dioxide product in a proper range, and the narrower the particle size, the better the particle size, which is beneficial to improving the structure and the application performance of the titanium dioxide product.
CN103086425A discloses a method for producing titanium dioxide by using titanium liquid with low total titanium and high iron-titanium ratio, which comprises the following steps: hydrolyzing titanium liquid with seed crystal to prepare metatitanic acid; treating according to a conventional method to obtain titanium dioxide, wherein the total titanium concentration of the titanium liquid is TiO 2 The content of (B) is 160-185 g/L, and the weight ratio of iron to titanium is 0.31-0.45. The method has the following defects: although the production cost is saved, the seed crystal dispersing ability is poor due to no adoption of a seed crystal dispersing agent, and metatitanic acid with small particle size and narrow particle size distribution cannot be obtained.
Disclosure of Invention
The invention aims to provide a method for preparing metatitanic acid with narrow particle size distribution.
A method for preparing metatitanic acid with narrow particle size distribution comprises the following steps:
a. preparing seed crystals: adding a seed crystal dispersing agent into a solution with the titanium dioxide concentration of 120-150 g/L to prepare a seed crystal solution; wherein the addition amount of the seed crystal dispersing agent is 0.30kg/m 3 ～1.20kg/m 3 (ii) a The seed crystal dispersing agent is polyvinylpyrrolidone (PVP), carboxymethyl cellulose (CMC), methyl Cellulose (MC) and/or polyvinyl alcohol (PVA);
b. preheating industrial titanium liquid with the concentration of 180-210 g/L to 94-100 ℃;
c. adding the seed crystal solution prepared in the step a into the preheated industrial titanium solution in the step b, and then performing hydrolysis according to the control conditions of the conventional hydrolysis process until the hydrolysis reaction is finished; wherein the addition amount of the seed crystal solution is 1.5-3.0% of the weight of the industrial titanium liquid.
Preferably, the concentration of the titanium dioxide in the solution in the step a is 135-145 g/L.
Preferably, the seed crystal dispersing agent in the step a is polyvinylpyrrolidone.
Preferably, in the step a, a seed crystal dispersing agent is added into the solution with the titanium dioxide concentration of 120-150 g/L, and the adding amount of the seed crystal dispersing agent is 0.50kg/m 3 ～0.90kg/m 3 。
Preferably, the concentration of the industrial titanium liquid in the step b is 186 g/L-195 g/L.
Preferably, the preheating temperature of the industrial titanium liquid in the step b is 96-98 ℃.
Preferably, the addition amount of the seed crystal solution in the step c is 2.0-2.5% of the weight of the industrial titanium liquid.
In the step a, the seed crystal dispersing agent mainly has the function of increasing the surface charge of the seed crystal by utilizing the performance of a surfactant of the seed crystal dispersing agent so as to improve the dispersing capacity of the seed crystal and facilitate the induction of the subsequent hydrolysis process;
in the step b, the concentration of the industrial titanium liquid is controlled to regulate and control the precipitation behavior of metatitanic acid during hydrolysis, and when the concentration of the titanium liquid is lower than 180g/L, the precipitated metatitanic acid hydrolyzed particles are coarse and have wide particle size distribution; when the concentration is higher than 210g/L, a large amount of energy is consumed for concentrating the titanium liquid, the hydrolysis rate is low, the yield of titanium is influenced, and the titanium liquid is not suitable for cost, economy, environmental protection and the like. The preheating temperature of the titanium liquid is too low, which affects the heating and boiling process time of the titanium liquid, so that the operation time is long, and bad crystals are easily formed, thereby affecting the hydrolysis process and the particle size distribution of the metatitanic acid; the preheating temperature of the titanium liquid is too high, so that the early hydrolysis of the titanium liquid is easily caused, and the particle size distribution of the separated metatitanic acid is further influenced;
in the step c, when the adding amount of the seed crystal solution is small, the hydrolysis induction of the titanium liquid is insufficient, and irregular crystal centers are easily formed to widen the particle size distribution of the metatitanic acid; when the seed crystal solution is added in an excessive amount, metatitanic acid particles are easy to grow rapidly, and the metatitanic acid particles are too coarse and have widened particle size distribution, so that the structure and the pigment performance of a titanium dioxide product are influenced.
The invention has the beneficial effects that:
1. according to the method for preparing the metatitanic acid with narrow particle size distribution, provided by the invention, the seed crystal dispersing agent is added to promote the dispersion of hydrolysis seed crystals and induce the benign progress of hydrolysis, and the concentration of the seed crystals, the concentration and preheating temperature of titanium liquid, the addition amount of the seed crystals and the like are regulated and controlled, so that the precipitation and aggregation behaviors of the metatitanic acid in the hydrolysis process are controlled, and the hydrolyzed metatitanic acid with small particle size and narrow particle size distribution is obtained.
2. The method for preparing the metatitanic acid with narrow particle size distribution provided by the invention has the characteristics of simple process, convenience in operation and narrow particle size distribution of the metatitanic acid.
Detailed Description
Embodiments of the present invention are described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples were carried out under conventional conditions without specifying the specific conditions.
Example 1
Adding a seed crystal dispersing agent into a solution with the titanium dioxide concentration of 144g/L, wherein the adding amount of the seed crystal dispersing agent is 0.90kg/m 3 (ii) a Wherein the seed crystal dispersing agent is polyvinylpyrrolidone (PVP); preheating 193g/L industrial titanium liquid to 96 ℃; adding 2.2% of seed crystal solution into the preheated industrial titanium solution, and then performing hydrolysis according to the conventional hydrolysis process control conditions until the hydrolysis reaction is finished. After completion of the hydrolysis, the particle size distribution of the metatitanic acid was measured by a laser particle sizer, and the results are shown in example 1 of Table 1, in which the average particle size was 1.857. Mu.m and the pitch ratio was 1.271.
Example 2
Adding seed crystal dispersing agent into the solution with the titanium dioxide concentration of 136g/L, wherein the adding amount of the seed crystal dispersing agent is 0.88kg/m 3 (ii) a Wherein the seed crystal dispersing agent is polyvinylpyrrolidone (PVP); preheating industrial titanium liquid with the concentration of 195g/L to 98 ℃; adding 2.1% of seed crystal solution into the preheated industrial titanium liquid, and then performing hydrolysis according to the conventional hydrolysis process control conditions until the hydrolysis reaction is finished. After completion of the hydrolysis, the particle size distribution of the metatitanic acid produced was measured by a laser particle sizer, and the results are shown in example 2 of Table 1, in which the average particle size was 1.984 μm and the track pitch ratio was 1.336.
Example 3
Adding seed crystal dispersing agent into the solution with the titanium dioxide concentration of 137g/L, wherein the adding amount of the seed crystal dispersing agent is 0.65kg/m 3 (ii) a Wherein the seed crystal dispersing agent is polyvinylpyrrolidone (PVP); preheating industrial titanium liquid with the concentration of 193g/L to 97 ℃; adding 2.5 percent of seed crystal solution into the preheated industrial titanium liquid, and then performing hydrolysis according to the control conditions of the conventional hydrolysis process until the hydrolysis reaction is finished. After completion of the hydrolysis, the particle size distribution of the resulting metatitanic acid was measured by a laser particle sizer, and the results are shown in example 3 of Table 1, in which the average particle size was 2.016. Mu.m and the pitch ratio was 1.357.
Comparative example 1
Preparing hydrolysis seed crystals, wherein the concentration of titanium dioxide in the hydrolysis seed crystals is 115g/L; preheating industrial titanium liquid with the concentration of 178g/L to 92 ℃; adding 1.4% of seed crystal solution into the preheated industrial titanium liquid, and then performing hydrolysis according to the conventional hydrolysis process control conditions until the hydrolysis reaction is finished. After the hydrolysis was completed, the particle size distribution of the resulting metatitanic acid was measured by a laser particle sizer, and the results are shown in comparative example 1 of Table 1, in which the average particle size was 2.432. Mu.m and the pitch ratio was 1.457.
Comparative example 2
Preparing hydrolysis seed crystals, wherein the concentration of titanium dioxide in the hydrolysis seed crystals is 115g/L; preheating industrial titanium liquid with the concentration of 190g/L to 97 ℃; adding 2.3 percent of seed crystal solution into the preheated industrial titanium liquid, and then performing hydrolysis according to the control conditions of the conventional hydrolysis process until the hydrolysis reaction is finished. After completion of the hydrolysis, the particle size distribution of the metatitanic acid produced was measured by a laser particle sizer, and the results are shown in comparative example 2 of Table 1, in which the average particle size was 2.338 μm and the pitch ratio was 1.440.
Comparative example 3
Adding seed crystal dispersing agent into the solution with the titanium dioxide concentration of 144g/L, wherein the adding amount of the seed crystal dispersing agent is 0.90kg/m 3 (ii) a Wherein the seed crystal dispersing agent is polyvinylpyrrolidone (PVP); preheating industrial titanium liquid with the concentration of 178g/L to 90 ℃; adding 2.1% of seed crystal solution into the preheated industrial titanium liquid, and then performing hydrolysis according to the conventional hydrolysis process control conditions until the hydrolysis reaction is finished. After completion of the hydrolysis, the particle size distribution of the metatitanic acid produced was measured by a laser particle sizer, and the results are shown in comparative example 3 of Table 1, in which the average particle size was 2.277 μm and the pitch ratio was 1.493.
Comparative example 4
Adding a seed crystal dispersing agent into a solution with the titanium dioxide concentration of 144g/L, wherein the adding amount of the seed crystal dispersing agent is 0.90kg/m 3 (ii) a Wherein the seed crystal dispersing agent is polyvinylpyrrolidone (PVP); preheating 193g/L industrial titanium liquid to 97 ℃; adding 3.2% of seed crystal solution into the preheated industrial titanium solution, and then performing hydrolysis according to the conventional hydrolysis process control conditions until the hydrolysis reaction is finished. After the hydrolysis was completed, the particle size distribution of the resulting metatitanic acid was measured by a laser particle sizer, and the results are shown in comparative example 4 of Table 1, in which the average particle size was 2.185. Mu.m and the pitch ratio was 1.485.
Watch 1
| Sample name | D 10 (μm) | D 50 (μm) | D 90 (μm) | D AV (μm) | Radial to pitch ratio |
| Example 1 | 0.726 | 1.862 | 3.005 | 1.857 | 1.271 |
| Example 2 | 0.734 | 1.881 | 3.247 | 1.984 | 1.336 |
| Example 3 | 0.741 | 1.896 | 3.314 | 2.016 | 1.357 |
| Comparative example 1 | 0.665 | 2.394 | 4.153 | 2.432 | 1.457 |
| Comparative example 2 | 0.689 | 2.357 | 4.082 | 2.338 | 1.440 |
| Comparative example 3 | 0.705 | 2.238 | 4.046 | 2.277 | 1.493 |
| Comparative example 4 | 0.668 | 2.194 | 3.926 | 2.185 | 1.485 |
Wherein, D in the table 10 Particle diameter representing a cumulative particle distribution of 10%, D 50 Particle diameter representing a cumulative particle distribution of 50%, D 90 A particle diameter representing 90% of the cumulative particle distribution; d AV Represents the average particle diameter of the particles; radius-distance ratio = (D) 90 -D 10 )/D 50 The smaller the numerical value of the radius ratio, the narrower the particle size distribution of the particles.
The present embodiments are to be considered as illustrative and not restrictive, and modifications and improvements on the basis of the present invention may be made by those skilled in the art after reading the present specification without departing from the scope of the invention as defined by the appended claims.
Claims (7)
1. A method for preparing metatitanic acid with narrow particle size distribution is characterized by comprising the following steps:
a. preparing seed crystals: adding a seed crystal dispersing agent into a solution with the titanium dioxide concentration of 120-150 g/L to prepare a seed crystal solution; wherein, the seed crystal dispersing agentThe addition amount is 0.30kg/m 3 ～1.20kg/m 3 (ii) a The seed crystal dispersing agent is polyvinylpyrrolidone, carboxymethyl cellulose, methyl cellulose and/or polyvinyl alcohol;
b. preheating industrial titanium liquid with the concentration of 180-210 g/L to 94-100 ℃;
c. adding the seed crystal solution prepared in the step a into the preheated industrial titanium solution in the step b, and then performing hydrolysis according to the control conditions of the conventional hydrolysis process until the hydrolysis reaction is finished; wherein the addition amount of the seed crystal solution is 1.5-3.0% of the weight of the industrial titanium liquid.
2. The method for preparing metatitanic acid with narrow particle size distribution as claimed in claim 1, wherein: the concentration of the titanium dioxide in the solution in the step a is 135-145 g/L.
3. The method for preparing metatitanic acid with narrow particle size distribution of claim 1, wherein: the seed crystal dispersing agent in the step a is polyvinylpyrrolidone.
4. The method for preparing metatitanic acid with narrow particle size distribution as claimed in claim 1, wherein: in the step a, seed crystal dispersing agent is added into the solution with the titanium dioxide concentration of 120-150 g/L, and the adding amount of the seed crystal dispersing agent is 0.50kg/m 3 ～0.90kg/m 3 。
5. The method for preparing metatitanic acid with narrow particle size distribution as claimed in claim 1, wherein: the concentration of the industrial titanium liquid in the step b is 186 g/L-195 g/L.
6. The method for preparing metatitanic acid with narrow particle size distribution as claimed in claim 1, wherein: the preheating temperature of the industrial titanium liquid in the step b is 96-98 ℃.
7. The method for preparing metatitanic acid with narrow particle size distribution as claimed in claim 1, wherein: the addition amount of the seed crystal solution in the step c is 2.0-2.5% of the weight of the industrial titanium liquid.
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