CN111849211B - Preparation method of high-light-resistance high-coverage titanium dioxide for papermaking - Google Patents
Preparation method of high-light-resistance high-coverage titanium dioxide for papermaking Download PDFInfo
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- CN111849211B CN111849211B CN201910358828.7A CN201910358828A CN111849211B CN 111849211 B CN111849211 B CN 111849211B CN 201910358828 A CN201910358828 A CN 201910358828A CN 111849211 B CN111849211 B CN 111849211B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of titanium dioxide preparation, and discloses a preparation method of high-light-resistance high-coverage titanium dioxide for papermaking, which comprises the following steps: 1) preparing titanium dioxide slurry; 2) heating the titanium dioxide slurry to 60 ℃, and adding cerium salt solution and TiOCl2Adding phosphate solution into the solution, and homogenizing; 3) adjusting the pH value of the homogenized slurry obtained in the step 2) to 2-4, and then homogenizing, and simultaneously adding FeSO4Solution and dilute alkali solution, and the pH value of the slurry is maintained to be 2-4, and then homogenization is carried out; 4) simultaneously adding an aluminum salt solution and a dilute acid or a dilute alkali solution to coat the aluminum film; 5) and washing the slurry coated with the aluminum film with water, flashing, and performing vapor powdering to obtain a titanium dioxide finished product. The titanium dioxide for papermaking prepared by the method has excellent covering power and light resistance, and does not influence the hue of the final product.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide preparation, and particularly relates to a preparation method of high-light-resistance high-coverage titanium dioxide for papermaking.
Background
Titanium dioxide is a very important white pigment and is widely applied to the industries of paint, plastics, papermaking, printing ink and the like. Paper making is the third largest user of titanium dioxide. Titanium dioxide is used as a paper filler and is mainly used in high-grade paper and thin paper. The titanium dioxide is added into the paper, so that the paper has better whiteness, good gloss, high strength, thinness, smoothness, no penetration during printing and light weight. However, the manufacturing process is the same for any kind of paper, and the main reason for determining which kind of titanium white is selected by the paper mill is the cost of paper making. Because the cost proportion of the titanium white in the paper making is as high as 30% -50%, the selection of the titanium white can be considered as a weight comparison under the condition that a paper mill meets the requirements of users.
For titanium dioxide, the key indexes are the light resistance and the covering power of the titanium dioxide in paper. In the prior art, two methods are generally used for improving the light resistance, namely, a titanium salt or a cerium salt is added respectively, and both can achieve better light resistance; titanium salt (chlorination by-product TiOCl) is added2) The volatility is strong, the coating technology difficulty is high, the light resistance is good when the cerium salt is added, but the cost is high, and the color phase of the final product can be influenced after the cerium salt is yellow.
Disclosure of Invention
Aiming at the situation, the invention aims to provide a preparation method of titanium dioxide for papermaking with high light resistance and high covering power2O3The film layer is helpful for increasing scattering centers, and the ferric oxide has space separation effect and reduces TiO2Agglomeration of the particles to make more TiO2The particles play a role of incident light scattering centers, so that the covering power of the titanium dioxide is improved.
The invention provides a preparation method of high-light-resistance high-coverage titanium dioxide for papermaking, which comprises the following steps:
1) preparing titanium dioxide slurry;
2) heating the titanium dioxide slurry to 60 ℃, and adding cerium salt solution and TiOCl2Adding phosphate solution into the solution, and homogenizing;
3) adjusting the pH value of the homogenized slurry obtained in the step 2) to 2-4, and then homogenizing, and simultaneously adding FeSO4Solution and dilute alkali solution, and the pH value of the slurry is maintained to be 2-4, and then homogenization is carried out;
4) simultaneously adding an aluminum salt solution and a dilute acid or a dilute alkali solution to coat the aluminum film;
5) and washing the slurry coated with the aluminum film with water, flashing, and performing vapor powdering to obtain a titanium dioxide finished product.
Preferably, in step 1), TiO is used2The concentration of the titanium dioxide slurry is 250-800 g/L.
In the present invention, the titanium dioxide slurry is prepared from a sand mill obtained by sand milling a titanium dioxide base material, and the particle size of the sand mill can be selected according to the requirement, for example, the particle size can be 0.30-0.40 μm (obtained by Malvern 3000 test).
Preferably, the cerium salt solution is Ce (NH)4)2(NO3)6Solution or Ce (SO)4)2Solution of CeO2The cerium salt accounts for TiO20.10-0.30wt% of the total amount.
Preferably, in TiO2Meter, TiOCl2The addition amount of the titanium pigment accounts for TiO in the titanium pigment slurry20.15-0.60wt% of the total amount.
In the present invention, the cerium salt solution and TiOCl2The adding time of the solution is 30-60min,
preferably, the phosphate solution is Na2HPO4Solution, NaH2PO4Solution and Na3PO4One or more of the solutions as P2O5The amount of phosphate added is calculated according to the amount of TiO2Adding phosphate solution 2-4wt%, and homogenizing for 60 min.
According to the invention, in step 3), dilute H is used2SO4Adjusting the pH value of the homogenized slurry in the step 2) to 2-4, and homogenizing for 20 min.
Preferably, the FeSO4The concentration of the solution is 80-200g/L, and Fe is used2O3The addition amount of the catalyst is calculated according to the TiO2Adding for 45min, and homogenizing for 30min, wherein the total amount is 1-3 wt%.
Preferably, in the step 4), dilute alkali is used for adjusting the pH value of the slurry to 8.0-9.0, the adjustment is carried out for 30min, and the homogenization is carried out for 30 min; adding NaAlO at the same time2Solution and dilute acid solution or Al2(SO4)3Keeping pH value of the solution and dilute alkali solution at 8.0-9.0, adding for 90min, and homogenizing for 30 min.
Further preferably, Al2O3Meter, the NaAlO2The concentration of the solution is 80-200g/L, and the Al is2(SO4)3Concentration of solution80-200g/L of NaAlO2Or Al2(SO4)3In an amount of TiO21-3wt% (in terms of Al) of the total amount2O3Meter).
The dilute acid in the invention is dilute H2SO4The solution is NaOH solution or KOH solution.
According to the invention, in step 5), before washing with water, dilute H is used2SO4Adjusting pH to 6, adjusting for 30min, and homogenizing for 120 min.
The processes not limited in the present invention are performed by conventional methods in the art, such as water washing, flash evaporation, vapor powder, etc.
Compared with the prior art, the preparation method of the titanium dioxide has the following beneficial effects:
1. according to the invention, the mixed film of titanium phosphate and cerium phosphate is prepared by doping cerium salt and titanium salt, so that the light resistance of the titanium dioxide is improved, and the hue is not influenced; then coating a layer of Fe on the surface of the titanium dioxide2O3The film layer is helpful for increasing scattering centers, and the ferric oxide has space separation effect and reduces TiO2Agglomeration of the particles to make more TiO2The particles play a role of incident light scattering centers, so that the covering power of the titanium dioxide is improved.
2. The method adopts the titanium oxychloride of the partial chlorination process waste byproduct as the titanium source, so that the light resistance of the titanium dioxide can be improved, the waste byproduct can be reused, and the cyclic utilization of resources is promoted.
3. The invention adopts the byproduct FeSO of the sulfuric acid method titanium dioxide process4·7H2And O is used as an iron source, so that the covering power of the product can be improved, the waste and the side products are recycled, and the cyclic continuous development of the sulfuric acid method chlorination method double processes is promoted.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples 1 to 3 are intended to illustrate the preparation of the titanium pigment for papermaking of the present invention having high light resistance and high hiding power.
Example 1
The slurry with qualified sand grinding grain diameter is led into a coating tank, and the concentration of the slurry is controlled to be 300g/L (by TiO)2Meter), and simultaneously heating to 60 ℃; adding 0.2wt% of TiOCl within 30min2(in the form of TiO)2Calculated) and 0.3 wt.% Ce (SO)4)2(with CeO)2Calculated) while adding 2wt% of Na2HPO4Solution and Na3PO4Solution (with P)2O5Metering), homogenizing for 60 min; with dilute H2SO4Adjusting the pH =2 of the slurry, and homogenizing for 20 min; adding 1wt% of FeSO within 45min4Solution (with Fe)2O3Metering) and dilute NaOH solution, maintaining the pH value of the slurry to be 2, and homogenizing for 30 min; adjusting the pH =8.2 of the slurry by using a dilute NaOH solution, adjusting for 30min, and homogenizing for 30 min; adding 1wt% NaAlO within 90min2Solution (with Al)2O3Meter) and dilute H2SO4Solution, maintaining co-current pH =8.2, homogenized for 30 min; with dilute H2SO4Adjusting pH =6.0, adjusting for 30min, and homogenizing for 120 min; washing, flash evaporation and steam powder to obtain the product.
Example 2
The slurry with qualified sand grinding grain diameter is led into a coating tank, and the concentration of the slurry is controlled to be 300g/L (by TiO)2Meter), and simultaneously heating to 60 ℃; adding 0.3wt% of TiOCl within 45min2(in the form of TiO)2Calculated) and 0.2 wt.% Ce (SO)4)2(with CeO)2Calculated) while adding 2wt% of Na2HPO4Solution and Na3PO4Solution (with P)2O5Metering), homogenizing for 60 min; with dilute H2SO4Adjusting the pH =2.5 of the slurry, and homogenizing for 20 min; adding 2wt% of FeSO within 45min4Solution (with Fe)2O3Metering) and dilute NaOH solution, maintaining the pH of the slurry to be 2.5, and homogenizing for 30 min; adjusting the pH =8.2 of the slurry by using a dilute NaOH solution, adjusting for 30min, and homogenizing for 30 min; adding 2wt% NaAlO within 90min2Solution (with Al)2O3Meter) and dilute H2SO4Solution, maintaining co-current pH =8.2, homogenized for 30 min; with dilute H2SO4Adjusting pH =6.0, adjusting for 30min, and homogenizing for 120 min; washing, flash evaporation and steam powder to obtain the product.
Example 3
The slurry with qualified sand grinding grain diameter is led into a coating tank, and the concentration of the slurry is controlled to be 300g/L (by TiO)2Meter), and simultaneously heating to 60 ℃; adding 0.40wt% of TiOCl within 60min2(in the form of TiO)2Calculated) and 0.1 wt.% Ce (SO)4)2(with CeO)2Calculated) while adding 2wt% of Na2HPO4Solution and Na3PO4Solution (with P)2O5Metering), homogenizing for 60 min; with dilute H2SO4Adjusting the pH =3 of the slurry, and homogenizing for 20 min; adding 3wt% of FeSO within 45min4Solution (with Fe)2O3Metering) and dilute NaOH solution, maintaining the pH value of the slurry to be 3, and homogenizing for 30 min; adjusting the pH =8.2 of the slurry by using a dilute NaOH solution, adjusting for 30min, and homogenizing for 30 min; adding 3wt% NaAlO within 90min2Solution (with Al)2O3Meter) and dilute H2SO4Solution, maintaining co-current pH =8.2, homogenized for 30 min; with dilute H2SO4Adjusting pH =6.0, adjusting for 30min, and homogenizing for 120 min; washing, flash evaporation and steam powder to obtain the product.
Comparative example 1
The slurry with qualified sand grinding grain diameter is led into a coating tank, and the concentration of the slurry is controlled to be 300g/L (by TiO)2Meter), and simultaneously heating to 60 ℃; adding 0.5wt% Ce (SO) in 30min4)2(with CeO)2Calculated) while adding 1.2wt% of Na2HPO4Solution and Na3PO4Solution (with P)2O5Metering), homogenizing for 60 min; adjusting the pH =8.2 of the slurry by using a dilute NaOH solution, adjusting for 30min, and homogenizing for 30 min; adding 3wt% NaAlO within 90min2Solution (with Al)2O3Meter) and dilute H2SO4Solution, maintaining co-current pH =8.2, homogenized for 30 min; with dilute H2SO4Adjusting pH =6.0, adjusting for 30min, and homogenizing for 120 min; washing, flash evaporation and steam powder to obtain the product.
Comparative example 2
Slurry with qualified sand grinding particle size is led into a coating tank for controllingThe concentration of the prepared slurry is 300g/L (by TiO)2Meter), and simultaneously heating to 60 ℃; by H2SO4Adjusting pH to 2.0 + -0.2, adding for 20min, and homogenizing for 10 min; adding 3.5wt% of H3PO4Solution (with H)3PO4Metering), adding for 30min, homogenizing for 10 min; adding 5.5wt% NaAlO2(with Al)2O3Calculated) for 60min, adding X% NaAlO2To pH =8.2, homogenized for 20 min; 5.5wt% -X% NaAlO2And H2SO4Keeping pH =8.2 in parallel flow, adding the solution after 60min, and homogenizing for 20 min; with dilute H2SO4Adjusting pH =6.0, adjusting for 30min, and homogenizing for 120 min; washing, flash evaporation and steam powder to obtain the product.
The samples prepared in examples 1-3 and comparative examples 1-2 were tested for hiding power, light fastness, hue and other properties, and the results are shown in table 1.
TABLE 1
As can be seen from the data in Table 1, the covering power and the light resistance of the titanium dioxide prepared by the method of the invention in the paper making of the examples 1 to 3 are superior to those of the common paper making titanium dioxide in the comparative examples 1 to 2, and the color phase of the final product is not influenced.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.
Claims (6)
1. The preparation method of the titanium dioxide for papermaking with high light resistance and high covering power is characterized by comprising the following steps:
1) preparing titanium dioxide slurry;
2) heating the titanium dioxide slurry to 60 ℃, and adding cerium salt solution and TiOCl2Adding phosphate solution into the solution, and homogenizing;
3) adjusting the pH value of the homogenized slurry obtained in the step 2) to 2-4, and then homogenizing, and simultaneously adding FeSO4Solution and dilute alkali solution, and the pH value of the slurry is maintained to be 2-4, and then homogenization is carried out;
4) simultaneously adding an aluminum salt solution and a dilute acid or a dilute alkali solution to coat the aluminum film;
5) washing, flash evaporating and steam pulverizing the slurry coated with the aluminum film to obtain a finished product of titanium dioxide;
in step 1), TiO is used2The concentration of the titanium dioxide slurry is 250-800 g/L;
with CeO2The cerium salt accounts for TiO20.10-0.30wt% of the total amount;
with TiO2Meter, TiOCl2The addition amount of the titanium pigment accounts for TiO in the titanium pigment slurry20.15-0.60wt% of the total amount;
with P2O5The amount of phosphate added is calculated according to the amount of TiO22-4wt% of the total amount;
the FeSO4The concentration of the solution is 80-200g/L, and Fe is used2O3Meter, FeSO4In an amount of TiO21-3wt% of the total amount;
in the step 4), dilute alkali is firstly used for adjusting the pH value of the slurry to 8.0-9.0, and NaAlO is added simultaneously2Solution and dilute acid solution or Al2(SO4)3Solution and dilute alkali solution, keeping pH value of concurrent flow at 8.0-9.0, and adding Al2O3Meter, the NaAlO2The concentration of the solution is 80-200g/L, and the Al is2(SO4)3The concentration of the solution is 80-200g/L, NaAlO2Or Al2(SO4)3In an amount of TiO21-3wt% of the total amount.
2. The method of claim 1, wherein: the cerium salt solution is Ce (NH)4)2(NO3)6Solution or Ce (SO)4)2And (3) solution.
3. The production method according to claim 1 or 2, whichIs characterized in that: the phosphate solution is Na2HPO4Solution, NaH2PO4Solution and Na3PO4One or more of the solutions.
4. The method of claim 1, wherein: in step 3), dilute H is used2SO4Adjusting the pH value of the homogenized slurry in the step 2) to 2-4, and homogenizing for 20 min; the FeSO4The addition time of the solution was 45min, followed by homogenization for 30 min.
5. The method of claim 1, wherein: in the step 4), adjusting the pH value of the slurry by using dilute alkali, adjusting for 30min, and homogenizing for 30 min; NaAlO2Solution and dilute acid solution or Al2(SO4)3The addition time of the solution and the dilute alkali solution was 90min, followed by homogenization for 30 min.
6. The method of claim 1, wherein: in step 5), before washing with water, dilute H is used2SO4Adjusting pH to 6, adjusting for 30min, and homogenizing for 120 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0649886A2 (en) * | 1993-10-21 | 1995-04-26 | The Mearl Corporation | Improved weather resistant pearlescent pigments |
| CN102040869A (en) * | 2010-11-26 | 2011-05-04 | 攀钢集团钢铁钒钛股份有限公司 | Preparation method of colorful titanium dioxide |
| CN105199434A (en) * | 2015-07-30 | 2015-12-30 | 四川大学 | Surface treatment method of papermaking dedicated titanium dioxide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0649886A2 (en) * | 1993-10-21 | 1995-04-26 | The Mearl Corporation | Improved weather resistant pearlescent pigments |
| CN102040869A (en) * | 2010-11-26 | 2011-05-04 | 攀钢集团钢铁钒钛股份有限公司 | Preparation method of colorful titanium dioxide |
| CN105199434A (en) * | 2015-07-30 | 2015-12-30 | 四川大学 | Surface treatment method of papermaking dedicated titanium dioxide |
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