CN112194177A - Preparation method of high-water-dispersion titanium dioxide - Google Patents
Preparation method of high-water-dispersion titanium dioxide Download PDFInfo
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Abstract
The invention discloses a preparation method of high-water-dispersion titanium dioxide, which comprises the following steps: s1 preparation of raw materials: preparing titanium liquid, hydrolyzing S2: adding sulfuric acid into the titanium liquid for hydrolysis to obtain metatitanic acid, and bleaching by S3: adding the hydrolyzed metatitanic acid into trivalent titanium for bleaching, and performing S4 salt treatment: adding a phosphorus salt, an anti-caking agent and a salt treating agent into the bleached metatitanic acid solution for salt treatment, and S5 squeezing: air compressing and pressing the metatitanic acid qualified in treatment, and calcining and cooling S6: the method can effectively avoid that divalent iron ions in the metatitanic acid are increased into trivalent iron ions and deposited in the metatitanic acid by adding trivalent titanium in the washing and bleaching process of the metatitanic acid, can promote the iron removal effect of rinsing, and can achieve the aim of purifying the metatitanic acid, and secondly, the trivalent titanium is pollution-free, the production cost is low, and the cost is saved.
Description
Technical Field
The invention particularly relates to the technical field of chemical industry, and particularly relates to a preparation method of high-water-dispersibility titanium dioxide.
Background
Titanium white powder is considered to be the best white pigment at present, has excellent optical performance, whiteness and covering power, is widely applied to the fields of coating, plastics, papermaking, printing ink and the like through different surface coating treatments, and in the field of plastics, the color master batch uses more titanium white powder, the amount of the used titanium white powder is more than 70 percent, and the more the amount of the added titanium white powder is, the titanium white powder is required to have better dispersibility so as to ensure the easy processing of the color master batch.
In the existing preparation technology of the dispersed titanium dioxide, aiming at the problems that the glossiness of the titanium dioxide and the dispersibility of the titanium dioxide are not sufficient and cannot meet the requirements of people, the preparation method of the high-water-dispersion titanium dioxide is provided.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of high-water-dispersibility titanium dioxide, which mainly aims at solving the problem that the glossiness and the dispersibility of the titanium dioxide are not sufficient enough and cannot meet the requirements of people.
(II) technical scheme
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-water-dispersion titanium dioxide comprises the following steps:
s1 preparation of raw materials: preparing titanium liquid;
s2 hydrolysis: adding sulfuric acid into the titanium solution for hydrolysis to obtain metatitanic acid;
s3 bleaching: adding the hydrolyzed metatitanic acid into trivalent titanium for bleaching;
s4 salt treatment: adding a phosphorus salt, an anti-caking agent and a salt treating agent into the bleached metatitanic acid solution for salt treatment;
s5 squeezing: air compressing and squeezing the qualified metatitanic acid;
s6 calcination and cooling: adding water into the dehydrated metatitanic acid solution for calcining, and cooling after calcining to obtain a titanium dioxide crude product;
s7 crushing: crushing the crude titanium dioxide product by a Raymond mill to obtain finished titanium dioxide;
s8 dispersing treatment, namely, putting the crushed titanium dioxide into demineralized water, stirring the titanium dioxide to prepare slurry, and adding a dispersing agent and nano titanium dioxide;
s9 drying: and drying the dispersed titanium dioxide slurry, then crushing and grinding, and then packaging to obtain the dispersed titanium dioxide.
Further: in the step S1, the titanium liquid is prepared by selecting fine ilmenite, pulverizing the fine ilmenite by a raymond mill, adding the pulverized ilmenite into a reaction tank, adding 0.5 g of sulfuric acid for acidolysis, wherein the concentration of the sulfuric acid is 93%, performing air-pressure stirring while performing the acidolysis, wherein the stirring time is 0.5 hour, continuing the air-pressure for 5 minutes after the reaction is finished, adding 25 ml of water into the reaction tank after the air-pressure is finished, dissolving the solid phase, adding 15 parts of elemental iron, adding a flocculating agent, precipitating, and filtering after the precipitation, thereby obtaining the titanium liquid.
On the basis of the scheme: in step S2, adding 5 to 10 parts of sulfuric acid to 10 to 15 parts of titanium solution to hydrolyze, wherein the concentration of sulfuric acid is 85%, and the hydrolysis is completed to perform bleaching, specifically, adding trivalent titanium to metatitanic acid to bleach, and the ratio of the solution of trivalent titanium solution to metatitanic acid is 4: 2 by weight ratio.
As a still further scheme of the invention: in step S4, the phosphorous salt, the anti-caking agent and the salt treatment agent are added to the bleached metatitanic acid solution and stirred at a speed of 100 revolutions for 0.5-1 hour, 0.2-1% of ammonium bicarbonate is added in batches while stirring, and then the stirring is continued for 0.5 hour, and then potassium salt is added for use.
Further: and step S5, adding sulfuric acid into the metatitanic acid solution after salt treatment, dehydrating the metatitanic acid solution with the sulfuric acid concentration of 70%, after dehydration, compressing the metatitanic acid slurry qualified by air through a pump, sending the metatitanic acid slurry into a press for oak water pressing, and filtering while pressing.
On the basis of the scheme: and step S6, putting the squeezed metatitanic acid into a rotary kiln for high-temperature calcination, wherein the calcination temperature is 1000 ℃, the calcination time is 0.5-1 hour, and the titanium dioxide crude product is obtained by performing low-temperature cooling after the calcination is finished, wherein the cooling time is 20-30 minutes.
As a still further scheme of the invention: and step S7, adding the crude titanium dioxide into a Raymond mill for crushing, wherein the crushed particles are 150-300 meshes, and obtaining the titanium dioxide.
Further: and step S8, dispersing, namely adding the crushed titanium dioxide particles into a stirrer, and then adding water, wherein the ratio of the water to the titanium dioxide is 4: and 3, stirring at the speed of 360-400 for 15-25 minutes, adding the dispersing agent and the nano titanium dioxide while stirring, and continuously dispersing and stirring for 20-30 minutes, wherein the dispersing agent is 0.4-0.8 part, so as to obtain the dispersed titanium dioxide slurry.
On the basis of the scheme: and in the step S9, drying the stirred dispersed titanium dioxide slurry for 1.5-2 days to obtain a dispersed titanium dioxide cake, and then crushing the dried titanium dioxide cake into 50-100 meshes to obtain the product dispersed titanium dioxide.
The invention has the beneficial effects that:
the invention comprises the following steps: the method has the advantages that the method can better purify and remove iron from the concentrate through sulfuric acid, simultaneously, trivalent titanium is added for washing and bleaching, the metatitanic acid can be effectively prevented from being washed and bleached, so that divalent iron ions in the metatitanic acid are increased into trivalent iron ions and deposited in the metatitanic acid, the iron removal effect of rinsing can be promoted, the purpose of purifying the metatitanic acid can be achieved, secondly, the trivalent titanium is pollution-free and low in production cost, in addition, the water dispersibility of the titanium dioxide product can be stably improved through a salt treatment agent and agglomeration prevention, the dispersing agent and the nano titanium dioxide are added, so that the titanium dioxide has lipophilicity and hydrophilicity, the luster of the titanium dioxide is increased, secondly, the dispersibility of the titanium dioxide is increased, the nano titanium dioxide has good dispersibility and weather resistance, the infringement of ultraviolet rays can be prevented, and the use range of the titanium dioxide is increased, the stirring aims to improve the dispersion effect of the titanium dioxide.
Drawings
FIG. 1 is a schematic flow structure diagram of a preparation method of high water dispersion titanium dioxide powder provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present patent and are not to be construed as limiting the present patent.
In the description of this patent, it is noted that unless otherwise specifically stated or limited, the terms "mounted," "connected," and "disposed" are to be construed broadly and can include, for example, fixedly connected, disposed, detachably connected, disposed, or integrally connected and disposed. The specific meaning of the above terms in this patent may be understood by those of ordinary skill in the art as appropriate.
Example 1
A preparation method of high-water-dispersion titanium dioxide comprises the following steps:
s1 preparation of raw materials: preparing titanium liquid;
s2 hydrolysis: adding sulfuric acid into the titanium solution for hydrolysis to obtain metatitanic acid, wherein the acid is added to better increase the quality of the titanium white acid solution;
s3 bleaching: adding the hydrolyzed metatitanic acid into trivalent titanium for bleaching, and performing the design so as to facilitate the subsequent processing treatment of the titanium dioxide;
s4 salt treatment: the bleached metatitanic acid solution is added with the phosphorus salt, the anti-caking agent and the salt treating agent for salt treatment, so that the cost of the trivalent titanium white is low, and the production cost of the titanium white is reduced;
s5 squeezing: air compressing and squeezing the qualified metatitanic acid, wherein the squeezing is used for better removing water in the metatitanic acid solution;
s6 calcination and cooling: adding water into the dehydrated metatitanic acid solution for calcining, and cooling after calcining to obtain a titanium dioxide crude product;
s7 crushing: crushing the crude titanium dioxide product by a Raymond mill to obtain finished titanium dioxide;
s8, dispersing treatment, namely, putting the crushed titanium dioxide into desalted water, stirring to prepare slurry, and adding a dispersing agent and nano titanium dioxide simultaneously, wherein the dispersing agent and the nano titanium dioxide have low cost and the production cost is reduced;
s9 drying: drying the dispersed titanium dioxide slurry, then crushing and grinding, and then packaging to obtain the dispersed titanium dioxide;
in the invention: in the step S1, the titanium liquid is prepared by selecting fine ilmenite, pulverizing the fine ilmenite by a raymond mill, adding the pulverized ilmenite into a reaction tank, adding sulfuric acid for acidolysis, and particularly, the acidolysis by the sulfuric acid has the advantages that the concentrate can be better purified and deironized, the concentration of the sulfuric acid is 94%, the air pressure stirring is carried out while the acidolysis is carried out, the stirring time is 0.5 hour, after the reaction is finished, the air pressure is continued for 5 minutes, after the air pressure is finished, 25 ml of water is added into the reaction tank, solid phase substances are dissolved, 15 parts of elemental iron are added, a flocculating agent is added, the flocculating agent is modified polyacrylamide, so that impurities and colloidal particles in the titanium liquid can be conveniently removed, the titanium liquid is purified, precipitated, the precipitation is carried out, then the filtration is carried out, the titanium liquid is obtained, and in the step S2, 5-10 parts of sulfuric acid is added into 10-15 parts of the titanium liquid for hydrolysis, the concentration of sulfuric acid is 85%, and the hydrolysis is completed to carry out bleaching, specifically, trivalent titanium is added into metatitanic acid for bleaching, and the ratio of trivalent titanium solution to metatitanic acid solution is 3: 2, adding trivalent titanium for water washing and bleaching, avoiding that the divalent iron ions in the metatitanic acid rise to be trivalent iron ions and are deposited in the metatitanic acid in the water washing and bleaching process of the metatitanic acid, wherein the trivalent titanium is an ideal reducing agent, promoting the iron removal effect of rinsing, achieving the aim of purifying the metatitanic acid, and in addition, the trivalent titanium is pollution-free, adding phosphorus salt, an anti-caking agent and a salt treating agent into the bleached metatitanic acid solution in step S4, stirring at the speed of 100 revolutions for 0.5-1 hour, adding 0.5-1% ammonium bicarbonate in batches while stirring, continuing to stir for 0.5 hour, adding potassium salt for matching use, performing salt treatment for the purpose of reducing the salt content in the metatitanic acid, and influencing the dispersion effect of the titanium pigment due to overhigh salt content, because in the preparation process of the dispersion type titanium pigment, through detecting the range of salt content, the salt content of titanium dioxide is controlled, the dispersibility of the titanium dioxide in a water phase system is improved, the water dispersibility of a titanium dioxide product can be stably improved through a salt treating agent and anti-caking, sulfuric acid is added into a metatitanic acid solution after salt treatment in step S5, the concentration of the sulfuric acid is 70 percent for dehydration treatment, after dehydration treatment, qualified metatitanic acid slurry is subjected to air compression through a pump, the air compression time is 0.5-1 hour, meanwhile, the metatitanic acid slurry is sent into a press machine for oak water pressing, the pressing is used for removing water in the metatitanic acid better, secondly, residues in the metatitanic acid solution are reduced, in addition, filtering work is carried out during pressing, the pressed metatitanic acid is put into a rotary kiln for high-temperature calcination, the calcination temperature is 1000 ℃, the calcination time is 0.5-1 hour, it should be noted that the calcining temperature and the calcining time are controlled to better obtain the titanium dioxide, the titanium dioxide is cooled at low temperature after the calcining is finished, the cooling time is 20-30 minutes, and the design of the low temperature cooling is to improve the viscosity of the titanium dioxide and obtain a crude titanium dioxide product.
In particular: dispersing in step S8, adding the crushed titanium dioxide particles into a stirrer, and then adding water, wherein the ratio of water to titanium dioxide is 3: 2, stirring at the speed of 350-390 f for 15-20 min, adding a dispersing agent and the nano titanium dioxide while stirring, continuously dispersing and stirring for 21-28 min, wherein the dispersing agent is 0.5-0.7 part, so as to obtain dispersed titanium dioxide slurry, the dispersing agent has lipophilicity and hydrophilicity, the luster of the titanium dioxide is increased, the dispersibility of the titanium dioxide is increased, the nano titanium dioxide has good dispersibility and weather resistance, the ultraviolet ray damage can be prevented, the use range of the titanium dioxide is increased, the dispersing and stirring are continuously carried out for 21-28 min, the dispersing effect of the titanium dioxide is improved by stirring and dispersing, the stirred dispersed titanium dioxide slurry is dried in step S9, the drying time is 1-1.5 days, the drying time is controlled within 1-1.5 days, the drying time is short, and the coagulation degree of the titanium dioxide slurry is insufficient, the drying time process causes the titanium dioxide to be too hard, the dispersion effect of the titanium dioxide is influenced, a dispersed titanium dioxide cake is obtained, then the dried titanium dioxide cake is crushed, the crushed particles are 50-100 meshes, and the product of the dispersed titanium dioxide is obtained, the supplementary explanation is needed, in order to improve the grinding effect, the concentration of the dispersed titanium dioxide slurry can be controlled at 45%, and then the grinding time of the particles is not more than 0.5 hour.
The working principle of the embodiment is as follows: firstly selecting concentrate, placing the concentrate into a Raymond mill for crushing, secondly adding the crushed concentrate into a reaction tank, simultaneously adding 0.5 g of sulfuric acid for acidolysis, after the acidolysis is finished, carrying out air compression, after the air compression is finished, adding 50 ml of water, simultaneously adding elementary substance iron for reaction, secondly, adding a flocculating agent for purification again so as to purify impurities and colloid particles in titanium liquid, so that the titanium liquid is purified, secondly, adding 5-10 parts of sulfuric acid into 10-15 parts of titanium liquid for hydrolysis in a hydrolysis pot, after the hydrolysis is finished, adding trivalent titanium for washing and bleaching metatitanic acid, secondly, adding phosphonium salt, an anti-caking agent and a salt treating agent into the bleached metatitanic acid solution for stirring for salt treatment, so that the water dispersibility of a titanium dioxide product can be stably improved, and in addition, adding sulfuric acid into the salted metatitanic acid solution for dehydration treatment, secondly, air compression is carried out on the metatitanic acid slurry qualified through treatment through a pump, meanwhile, the metatitanic acid slurry is sent into a press machine for oak water pressing, the pressing is carried out for better removing water in metatitanic acid, in addition, residues in metatitanic acid solution are reduced, in addition, filtering work is carried out while pressing, then, the pressed metatitanic acid is put into a rotary kiln for high-temperature calcination, low-temperature cooling is carried out after calcination is finished, the low-temperature cooling design is carried out for improving the viscosity of titanium dioxide, then, the crushed titanium dioxide particles are added into a stirrer, then, water is added, stirring is carried out, dispersing agent and nano titanium dioxide are added while stirring, dispersing and stirring is continued, the dispersing agent is 0.6-0.8 part, the dispersing effect of the titanium dioxide is increased, the dispersed titanium dioxide slurry is obtained, the dispersing agent has lipophilicity and hydrophilicity, the luster of the titanium dioxide is increased, and the, the nano titanium dioxide has good dispersibility and weather resistance, can prevent ultraviolet ray from invading, and then the stirred dispersed titanium dioxide slurry is dried to obtain dispersed titanium dioxide cakes, and then the dried titanium dioxide cakes are crushed to obtain the product dispersed titanium dioxide.
Example 2:
s1 preparation of raw materials: preparing titanium liquid;
s2 hydrolysis: adding sulfuric acid into the titanium solution for hydrolysis to obtain metatitanic acid, wherein the acid is added to better increase the quality of the titanium white acid solution;
s3 bleaching: adding the hydrolyzed metatitanic acid into trivalent titanium for bleaching, and performing the design so as to facilitate the subsequent processing treatment of the titanium dioxide;
s4 salt treatment: the bleached metatitanic acid solution is added with the phosphorus salt, the anti-caking agent and the salt treating agent for salt treatment, so that the cost of the trivalent titanium white is low, and the production cost of the titanium white is reduced;
s5 squeezing: air compressing and squeezing the qualified metatitanic acid, wherein the squeezing is used for better removing water in the metatitanic acid solution;
s6 calcination and cooling: adding water into the dehydrated metatitanic acid solution for calcining, and cooling after calcining to obtain a titanium dioxide crude product;
s7 crushing: crushing the crude titanium dioxide product by a Raymond mill to obtain finished titanium dioxide;
s8, dispersing treatment, namely, putting the crushed titanium dioxide into desalted water, stirring to prepare slurry, and adding a dispersing agent and nano titanium dioxide simultaneously, wherein the dispersing agent and the nano titanium dioxide have low cost and the production cost is reduced;
s9 drying: drying the dispersed titanium dioxide slurry, then crushing and grinding, and then packaging to obtain the dispersed titanium dioxide;
in the invention: in the step S1, the titanium liquid is prepared by selecting fine ilmenite, pulverizing the fine ilmenite by a raymond mill, adding the pulverized ilmenite into a reaction tank, adding sulfuric acid for acidolysis, and particularly, the acidolysis by the sulfuric acid has the advantages that the iron in the concentrate can be better purified and removed, the concentration of the sulfuric acid is 95%, the air pressure stirring is carried out while the acidolysis is carried out, the stirring time is 0.5 hour, after the reaction is finished, the air pressure is continued for 5 minutes, after the air pressure is finished, 25 ml of water is added into the reaction tank, the solid phase is dissolved, 15 parts of elemental iron are added, then a flocculating agent is added, the flocculating agent is modified polyacrylamide, so that the impurities and colloidal particles in the titanium liquid can be conveniently removed, the titanium liquid is purified, precipitated, the precipitation is carried out, the filtration is carried out to obtain the titanium liquid, and in the step S2, 5 to 10 parts of sulfuric acid is added into 10 parts of the titanium liquid for hydrolysis, the concentration of sulfuric acid is 85%, and the hydrolysis is completed to carry out bleaching, specifically, trivalent titanium is added into metatitanic acid for bleaching, and the ratio of trivalent titanium solution to metatitanic acid solution is 3: 2, adding trivalent titanium for water washing and bleaching, avoiding that the divalent iron ions in the metatitanic acid rise to be trivalent iron ions and are deposited in the metatitanic acid in the water washing and bleaching process of the metatitanic acid, wherein the trivalent titanium is an ideal reducing agent, promoting the iron removal effect of rinsing, achieving the aim of purifying the metatitanic acid, and in addition, the trivalent titanium is pollution-free, adding phosphorus salt, an anti-caking agent and a salt treating agent into the bleached metatitanic acid solution in step S4, stirring at the speed of 100 revolutions for 0.5-1 hour, adding 0.5-1% ammonium bicarbonate in batches while stirring, continuing to stir for 0.5 hour, adding potassium salt for matching use, performing salt treatment for the purpose of reducing the salt content in the metatitanic acid, and influencing the dispersion effect of the titanium pigment due to overhigh salt content, because in the preparation process of the dispersion type titanium pigment, through detecting the range of salt content, the salt content of titanium dioxide is controlled, the dispersibility of the titanium dioxide in a water phase system is improved, the water dispersibility of a titanium dioxide product can be stably improved through a salt treating agent and anti-caking, sulfuric acid is added into a metatitanic acid solution after salt treatment in step S5, the concentration of the sulfuric acid is 70 percent for dehydration treatment, after dehydration treatment, qualified metatitanic acid slurry is subjected to air compression through a pump, the air compression time is 0.5-1 hour, meanwhile, the metatitanic acid slurry is sent into a press machine for oak water pressing, the pressing is used for removing water in the metatitanic acid better, secondly, residues in the metatitanic acid solution are reduced, in addition, filtering work is carried out during pressing, the pressed metatitanic acid is put into a rotary kiln for high-temperature calcination, the calcination temperature is 1000 ℃, the calcination time is 0.5-1 hour, it should be noted that the calcining temperature and the calcining time are controlled to better obtain the titanium dioxide, the titanium dioxide is cooled at low temperature after the calcining is finished, the cooling time is 20-30 minutes, and the design of the low temperature cooling is to improve the viscosity of the titanium dioxide and obtain a crude titanium dioxide product.
In particular: dispersing in step S8, adding the crushed titanium dioxide particles into a stirrer, and then adding water, wherein the ratio of water to titanium dioxide is 2: 1, stirring at the speed of 350-390 f for 15-25 min, adding a dispersing agent and nano titanium dioxide while stirring, continuously dispersing and stirring for 25-28 min, wherein the dispersing agent is 0.5-0.6 part, so as to obtain dispersed titanium dioxide slurry, the dispersing agent has lipophilicity and hydrophilicity, the luster of the titanium dioxide is increased, the dispersibility of the titanium dioxide is increased, the nano titanium dioxide has good dispersibility and weather resistance, the ultraviolet ray damage can be prevented, the application range of the titanium dioxide is increased, the dispersing and stirring are continuously carried out for 25-28 min, the dispersing effect of the titanium dioxide is improved by stirring and dispersing, the stirred dispersed titanium dioxide slurry is dried in step S9, the drying time is 11-1.5 days, the drying time is controlled within 1.5-2 days, the drying time is short, and the coagulation degree of the titanium dioxide slurry is insufficient, the drying time process causes the titanium dioxide to be too hard, the dispersion effect of the titanium dioxide is influenced, a dispersed titanium dioxide cake is obtained, then the dried titanium dioxide cake is crushed, the crushed particles are 50-100 meshes, and the product of the dispersed titanium dioxide is obtained, the supplementary explanation is needed, in order to improve the grinding effect, the concentration of the dispersed titanium dioxide slurry can be controlled at 45%, and then the grinding time of the particles is not more than 0.5 hour.
The working principle of the embodiment is as follows: firstly selecting concentrate, placing the concentrate into a Raymond mill for crushing, secondly adding the crushed concentrate into a reaction tank, simultaneously adding 0.5 g of sulfuric acid for acidolysis, after the acidolysis is finished, carrying out air compression, after the air compression is finished, adding 50 ml of water, simultaneously adding elementary substance iron for reaction, secondly, adding a flocculating agent for purification again so as to purify impurities and colloid particles in titanium liquid, so that the titanium liquid is purified, secondly, adding 5-10 parts of sulfuric acid into 10-15 parts of titanium liquid for hydrolysis in a hydrolysis pot, after the hydrolysis is finished, adding trivalent titanium for washing and bleaching metatitanic acid, secondly, adding phosphonium salt, an anti-caking agent and a salt treating agent into the bleached metatitanic acid solution for stirring for salt treatment, so that the water dispersibility of a titanium dioxide product can be stably improved, and in addition, adding sulfuric acid into the salted metatitanic acid solution for dehydration treatment, secondly, air compression is carried out on the metatitanic acid slurry qualified through treatment through a pump, meanwhile, the metatitanic acid slurry is sent into a press machine for oak water pressing, the pressing is carried out for better removing water in metatitanic acid, in addition, residues in metatitanic acid solution are reduced, in addition, filtering work is carried out while pressing, then, the pressed metatitanic acid is put into a rotary kiln for high-temperature calcination, low-temperature cooling is carried out after calcination is finished, the low-temperature cooling design is carried out for improving the viscosity of titanium dioxide, then, the crushed titanium dioxide particles are added into a stirrer, then, water is added, stirring is carried out, dispersing agent and nano titanium dioxide are added while stirring, dispersing and stirring is continued, the dispersing effect of the titanium dioxide is improved, so that dispersed titanium dioxide slurry is obtained, the dispersing agent has lipophilicity and hydrophilicity, the luster of the titanium dioxide is improved, the dispersibility of the titanium dioxide is improved, and the nano titanium, secondly, the stirred dispersed titanium dioxide slurry is dried to obtain a dispersed titanium dioxide cake, and then the dried titanium dioxide cake is crushed to obtain the product dispersed titanium dioxide.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A preparation method of high-water-dispersion titanium dioxide is characterized by comprising the following steps:
s1 preparation of raw materials: preparing titanium liquid;
s2 hydrolysis: adding sulfuric acid into the titanium solution for hydrolysis to obtain metatitanic acid;
s3 bleaching: adding the hydrolyzed metatitanic acid into trivalent titanium for bleaching;
s4 salt treatment: adding a phosphorus salt, an anti-caking agent and a salt treating agent into the bleached metatitanic acid solution for salt treatment;
s5 squeezing: air compressing and squeezing the qualified metatitanic acid;
s6 calcination and cooling: adding water into the dehydrated metatitanic acid solution for calcining, and cooling after calcining to obtain a titanium dioxide crude product;
s7 crushing: crushing the crude titanium dioxide product by a Raymond mill to obtain finished titanium dioxide;
s8 dispersing treatment, namely, putting the crushed titanium dioxide into demineralized water, stirring the titanium dioxide to prepare slurry, and adding a dispersing agent and nano titanium dioxide;
s9 drying: and drying the dispersed titanium dioxide slurry, then crushing and grinding, and then packaging to obtain the dispersed titanium dioxide.
2. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: in the step S1, the titanium liquid is prepared by selecting fine ilmenite, pulverizing the fine ilmenite by a raymond mill, adding the pulverized ilmenite into a reaction tank, adding sulfuric acid for acidolysis, wherein the concentration of the sulfuric acid is 93%, performing air-pressure stirring while performing the acidolysis, wherein the stirring time is 0.5 hour, continuing the air-pressure for 5 minutes after the reaction is finished, adding 25 ml of water into the reaction tank after the air-pressure is finished, dissolving the solid phase, adding 15 parts of elemental iron, adding a flocculating agent, precipitating, and filtering after the precipitation, thereby obtaining the titanium liquid.
3. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: in step S2, adding 5 to 10 parts of sulfuric acid to 10 to 15 parts of titanium solution to hydrolyze, wherein the concentration of sulfuric acid is 85%, and the hydrolysis is completed to perform bleaching, specifically, adding trivalent titanium to metatitanic acid to bleach, and the ratio of the solution of trivalent titanium solution to metatitanic acid is 4: 2 by weight ratio.
4. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: in step S4, the phosphorous salt, the anti-caking agent and the salt treatment agent are added to the bleached metatitanic acid solution and stirred at a speed of 100 revolutions for 0.5-1 hour, 0.2-1% of ammonium bicarbonate is added in batches while stirring, and then the stirring is continued for 0.5 hour, and then potassium salt is added for use.
5. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: in step S5, sulfuric acid is added to the salt-treated metatitanic acid solution, and after dehydration treatment, the sulfuric acid solution is dehydrated at a concentration of 70%, and after dehydration treatment, the metatitanic acid slurry qualified for treatment is compressed by air through a pump, and is sent into a press to be pressed by oak water, and in addition, filtration work is performed simultaneously with pressing.
6. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: and step S6, putting the squeezed metatitanic acid into a rotary kiln for high-temperature calcination, wherein the calcination temperature is 1000 ℃, the calcination time is 0.5-1 hour, and the titanium dioxide crude product is obtained by performing low-temperature cooling after the calcination is finished, wherein the cooling time is 20-30 minutes.
7. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: and step S7, adding the crude titanium dioxide into a Raymond mill for crushing, wherein the crushed particles are 150-300 meshes, and obtaining the titanium dioxide.
8. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: and step S8, dispersing, namely adding the crushed titanium dioxide particles into a stirrer, and then adding water, wherein the ratio of the water to the titanium dioxide is 4: and 3, stirring at the speed of 360-400 for 15-25 minutes, adding the dispersing agent and the nano titanium dioxide while stirring, and continuously dispersing and stirring for 20-30 minutes, wherein the dispersing agent is 0.4-0.8 part, so as to obtain the dispersed titanium dioxide slurry.
9. The preparation method of high water-dispersibility titanium dioxide as claimed in claim 1, wherein: and in the step S9, drying the stirred dispersed titanium dioxide slurry for 1.5-2 days to obtain a dispersed titanium dioxide cake, and then crushing the dried titanium dioxide cake into 50-100 meshes to obtain the product dispersed titanium dioxide.
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CN113929132A (en) * | 2021-09-24 | 2022-01-14 | 东华工程科技股份有限公司 | Sulfuric acid method titanium dioxide metatitanic acid bleaching method and system |
CN115924966A (en) * | 2022-12-12 | 2023-04-07 | 龙佰四川钛业有限公司 | Titanium white powder salt treating agent recovery process and titanium white powder production process |
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CN113929132A (en) * | 2021-09-24 | 2022-01-14 | 东华工程科技股份有限公司 | Sulfuric acid method titanium dioxide metatitanic acid bleaching method and system |
CN115924966A (en) * | 2022-12-12 | 2023-04-07 | 龙佰四川钛业有限公司 | Titanium white powder salt treating agent recovery process and titanium white powder production process |
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