CN111471323A - Preparation method of special titanium dioxide for papermaking - Google Patents

Preparation method of special titanium dioxide for papermaking Download PDF

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CN111471323A
CN111471323A CN202010385058.8A CN202010385058A CN111471323A CN 111471323 A CN111471323 A CN 111471323A CN 202010385058 A CN202010385058 A CN 202010385058A CN 111471323 A CN111471323 A CN 111471323A
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titanium dioxide
preparation
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CN111471323B (en
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赵波
王丽萍
王永珊
周文静
冯亚阳
曹青喜
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Henan Billions Advanced Material Co Ltd
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    • 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
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    • C09C1/3607—Titanium dioxide
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C1/3661—Coating
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • 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
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • 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
    • D21H17/675—Oxides, hydroxides or carbonates
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

The invention discloses a preparation method of special titanium dioxide for papermaking, which comprises the steps of slurry preparation, coating, three-washing, flash evaporation and steam powder preparation to obtain a finished product; the polybasic acid containing hydroxyl is particularly selected as the coating agent. The invention uses polybasic acid containing hydroxyl as a special coating agent, so that the film layer can be more compact, thereby achieving higher light resistance and covering power; the hydroxyl-containing polyacid is attached to the surface of the titanium dioxide in a bonding manner, so that the hydroxyl-containing polyacid cannot remain in the filtrate, cannot influence VOC (volatile organic compounds) and further cannot influence the environment.

Description

Preparation method of special titanium dioxide for papermaking
Technical Field
The invention relates to the technical field of titanium dioxide preparation, in particular to a preparation method of special titanium dioxide for papermaking.
Background
Titanium dioxide(TiO2) Titanium white, which is a white pigment with no substitution and optimal performance, has the excellent properties of no toxicity, optimal whiteness and brightness, optimal opacity, high-refractive-index covering performance, light resistance, chemical-medium resistance and the like, so that the titanium white is used as an important inorganic functional material and is widely applied to the industries of coatings, printing ink, plastics, papermaking, rubber, chemical fibers, cosmetics and the like. At present, the consumption of titanium dioxide in the world is nearly 60% for coating, 16% for plastic, 14% for paper making, 3% for printing ink and 7% for others (including rubber, cosmetics, medicines, enamels and chemical fibers).
Publication No. CN108929574A discloses a preparation method of titanium dioxide special for papermaking, a titanium dioxide coating layer formed on the surface of the titanium dioxide is of a three-layer structure, the innermost layer is a cerium compound, the middle layer is zirconia, and the outer layer is an alumina layer, although the titanium dioxide pigment obtained by the method has higher sun resistance and covering power, the zirconium compound is used in the coating process, so the cost is higher; the publication No. CN102585559A discloses a preparation method of titanium dioxide for decorative paper, the coating layer of the method is composed of silicon oxide, aluminum phosphate, aluminum oxide and an organic treatment layer, and the obtained titanium dioxide has high covering power but poor light resistance.
Therefore, a new preparation method of the titanium dioxide special for papermaking is needed to produce the titanium dioxide which has high light resistance, high covering power, environmental friendliness and low cost.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of special titanium dioxide for papermaking.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a preparation method of titanium dioxide special for papermaking comprises the following steps,
step 1, guiding the sanded slurry into a coating tank; with TiO2Controlling the concentration of the slurry to be 250-800 g/L, and heating to 60-90 ℃;
step 2, adding the material obtained in the step 1Carrying out first layer of coating on the pulp; the film layer of the first coating film is Fe (OH)3A film layer;
step 3, adding a coating agent into the slurry coated with the first layer in the step 2; the coating agent is polybasic acid containing hydroxyl;
step 4, adding a first aluminum salt solution and a phosphate radical-containing solution into the slurry obtained in the step 3 in a parallel flow manner; with P2O5The addition amount of the solution containing phosphate radical accounts for TiO21.0-3.0 wt% of the total amount; with Al2O3The adding amount of the first aluminum salt solution accounts for TiO20.3-1.0 wt% of the total amount;
step 5, adding an alkali solution into the slurry obtained in the step 4, and adjusting the pH value to 8.0-9.5;
step 6, adding a second aluminum salt solution and an acid-base regulator into the slurry obtained in the step 5, regulating and keeping the pH value of the slurry to be 8.0-9.5, and then homogenizing;
step 7, adding a dilute acid solution into the slurry obtained in the step 6, adjusting the pH value to 7.0, and then homogenizing;
and 8, carrying out three-washing, flash evaporation and steam powder treatment on the slurry obtained in the step 7 to obtain a finished product.
Preferably, in step 3, the polybasic acid is added in an amount based on TiO20.3-0.9 wt% of the total amount; the polybasic acid is one of citric acid and malic acid.
Preferably, in step 4, the adding time of the first aluminum salt solution and the phosphate radical-containing solution is 30-60 min.
Preferably, in the step 4, the phosphate radical-containing solution is one or more of a phosphoric acid solution, a dihydrogen phosphate solution, a hydrogen phosphate solution, a phosphate solution and a pyrophosphate solution; the first aluminum salt solution is a sodium metaaluminate solution; with Al2O3The concentration of the sodium metaaluminate solution is 80-200 g/L.
Preferably, in step 6, Al is used2O3The adding amount of the second aluminum salt solution accounts for TiO22.0-3.0 wt% of the total amount.
Preferably, in step 6, Al is used2O3Of the second aluminum salt solutionThe concentration is 80-200 g/L, and the second aluminum salt solution is sodium metaaluminate solution or aluminum sulfate solution.
Preferably, in step 6, the adding time of the second aluminum salt solution is 90-120 min; the homogenization time was 30 min.
Preferably, in the step 7, the adjusting time of the pH value is 30 min; the homogenization time was 120 min.
Preferably, the dilute acid solution is a sulfuric acid solution; the acid-base regulator is sodium hydroxide solution or sulfuric acid solution.
The invention has the following function principle:
the invention adopts polybasic acid solution containing hydroxyl (such as citric acid, malic acid and the like) as the coating agent. The polybasic acid containing hydroxyl can form double salt with metal ions to delay the reactivity of the metal ions, so that the inorganic coating agent can be deposited on the titanium dioxide more uniformly and compactly, thereby improving the light resistance of the titanium dioxide; and citric acid is attached to the titanium dioxide in a bonding mode, so that the citric acid cannot remain in the filtrate, cannot influence VOC (volatile organic compounds), and further cannot influence the environment.
The invention adopts hydroxyl-containing polybasic acid (citric acid, malic acid and the like) as a special coating agent, so that the coating layer can be more compact, thereby achieving higher light resistance and covering power, and the citric acid is attached to the titanium dioxide in a bonding way, thereby not influencing the environment
Compared with the prior art, the invention has the beneficial effects that:
1. the invention uses polybasic acid containing hydroxyl as a special coating agent, so that the film layer can be more compact, thereby achieving higher light resistance and covering power;
2. the hydroxyl-containing polyacid is attached to the surface of the titanium dioxide in a bonding manner, so that the hydroxyl-containing polyacid cannot remain in the filtrate, cannot influence VOC (volatile organic compounds) and further cannot influence the environment.
Detailed Description
The present invention will be further described with reference to specific examples, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
A preparation method of titanium dioxide special for papermaking comprises the following steps,
step 1, slurry with qualified sand grinding grain diameter is led into a coating tank; with TiO2Measuring, controlling the concentration of the slurry to be 300 g/L, and simultaneously heating to 80 ℃;
step 2, FeSO is added within 60min4Solution and dilute NaOH solution, maintaining the pH of the slurry at 2, and homogenizing for 30 min; with Fe2O3Meter, FeSO4The solution is added in an amount of TiO20.5 wt% of the total;
step 3, adding a citric acid solution within 20min, and homogenizing for 30 min; adding NaOH solution to adjust the pH value of the slurry to 5.0, adjusting for 20min, and homogenizing for 10 min; the citric acid solution accounts for TiO calculated by citric acid20.60 wt% of the total;
step 4, adding H in parallel flow within 60min3PO4Solution with NaAlO2Homogenizing the solution for 30min while keeping the pH at 5.0; with P2O5Meter, H3PO4The solution is added in an amount of TiO22.5 wt% of the total; with Al2O3Meter, NaAlO2The solution is added in an amount of TiO20.76 wt% of the total, NaAlO2The concentration of the solution is 80 g/L;
step 5, adjusting the pH value of the slurry to 9.0 by using NaOH solution, adjusting the pH value for 30min, and homogenizing for 30 min;
step 6, adding NaAlO within 120min2Solution and H2SO4The solution is cocurrent, the pH is kept at 9.0, and the solution is homogenized for 30 min; with Al2O3Meter, NaAlO2The solution is added in an amount of TiO23.0 wt% of the total amount of NaAlO2The concentration of the solution is 80 g/L;
step 7, dilute H is used2SO4Adjusting pH to 7.0, adjusting for 30min, and homogenizing for 120 min;
and 8, carrying out three-washing, flash evaporation and steam powder treatment to obtain a finished product.
Example 2
A preparation method of titanium dioxide special for papermaking comprises the following steps,
in the step 1, the method comprises the following steps of,slurry with qualified sand grinding particle size is led into a coating tank and is treated with TiO2Measuring, controlling the concentration of the slurry to be 300 g/L, and simultaneously heating to 80 ℃;
step 2, FeSO is added within 60min4Solution and dilute NaOH solution, maintaining the pH of the slurry at 2, and homogenizing for 30 min; with Fe2O3Meter, FeSO4The solution is added in an amount of TiO20.5 wt% of the total;
step 3, adding malic acid solution within 20min, and homogenizing for 30 min; adjusting the pH value of the slurry to 5.0 by NaOH, adjusting the pH value after 20min, and homogenizing for 10 min; the addition amount of the malic acid solution is calculated by malic acid and accounts for TiO20.60 wt% of the total;
step 4, adding H in parallel flow within 60min3PO4Solution with NaAlO2Homogenizing the solution for 30min while keeping the pH at 5.0; with P2O5Meter, H3PO4The solution is added in an amount of TiO22.5 wt% of the total; with Al2O3Meter, NaAlO2The solution is added in an amount of TiO20.73 wt% of the total amount of NaAlO2The concentration of the solution is 140 g/L;
step 5, adjusting the pH value of the slurry to 9.0 by using NaOH solution, adjusting the pH value for 30min, and homogenizing for 30 min;
step 6, adding NaAlO within 120min2Solution and H2SO4The solution is cocurrent, the pH is kept at 8.5, and homogenization is carried out for 30 min; with Al2O3Meter, NaAlO2The solution is added in an amount of TiO23.0 wt% of the total amount of NaAlO2The concentration of the solution is 140 g/L;
step 7, dilute H is used2SO4Adjusting pH to 7.0, adjusting for 30min, and homogenizing for 120 min;
and 8, carrying out three-washing, flash evaporation and steam powder treatment to obtain a finished product.
Example 3
A preparation method of titanium dioxide special for papermaking comprises the following steps,
step 1, guiding the slurry with qualified sand grinding grain diameter into a coating tank by TiO2Measuring, controlling the concentration of the slurry to be 300 g/L, and simultaneously heating to 80 ℃;
step 2, FeSO is added within 60min4Solution and dilute NaOH solution, maintaining the pH of the slurry at 2, and homogenizing for 30 min; FeSO4The amount of the solution added is Fe2O3Calculated on TiO20.5 wt% of the total;
step 3, adding a citric acid solution within 20min, and homogenizing for 30 min; adjusting the pH value of the slurry to 5.0 by NaOH, adjusting the pH value after 20min, and homogenizing for 10 min; the citric acid solution is added in an amount accounting for TiO according to citric acid20.60 wt% of the total;
step 4, adding H in parallel flow within 60min3PO4Solution with NaAlO2Homogenizing the solution for 30min while keeping the pH at 5.0; with P2O5Meter, H3PO4The solution is added in an amount of TiO22.5 wt% of the total; with Al2O3Meter, NaAlO2The solution is added in an amount of TiO20.74 wt% of the total, NaAlO2The concentration of the solution is 200 g/L;
step 5, adjusting the pH value of the slurry to 9.0 by using NaOH solution, adjusting the pH value for 30min, and homogenizing for 30 min;
step 6, adding NaAlO within 120min2Solution and H2SO4Parallel flow, keeping pH at 9.0, homogenizing for 30 min; with Al2O3Meter, NaAlO2The solution is added in an amount of TiO23.0 wt% of the total amount of NaAlO2The concentration of the solution is 200 g/L;
step 7, dilute H is used2SO4Adjusting pH to 7.0, adjusting for 30min, and homogenizing for 120 min;
and 8, carrying out three-washing, flash evaporation and steam powder treatment to obtain a finished product.
Comparative example
The slurry with qualified sand grinding grain diameter is led into a coating tank, and the concentration of the slurry is controlled to be 300 g/L (by TiO)2Metering), and simultaneously heating to 80 ℃; adding 0.2 wt% Ce (NH) within 30min4)2(NO3)6(with CeO)2Calculated) while adding 0.8 wt% Na3PO4(with P)2O5Metering) the solution, and homogenizing for 30 min; adjusting the pH value of the slurry to 5.0 by NaOH, adjusting the pH value after 20min, and homogenizing for 10 min; 2.5 wt% H is added within 60min3PO4(with P)2O5Calculated) solution with 0.78 wt% NaAlO2(in the form of TiO)2Meter) solution was co-flowed and homogenized for 30min maintaining pH 5.0; with 0.44 wt% NaAlO2(in the form of TiO)2Metering) the pH value of the solution adjusting slurry is 8.0-9.0, adjusting for 30min, and homogenizing for 30 min; adding 3.78 wt% NaAlO within 120min2(in the form of TiO)2Meter) solution with H2SO4Parallel flow, keeping pH 8.2, homogenizing for 30 min; with dilute H2SO4Adjusting pH to 7.0, adjusting for 30min, and homogenizing for 120 min; and obtaining a finished product after three-washing, flash evaporation and steam powder.
The light resistance of the products obtained in example 1, example 2, example 3 and comparative example and the COD of the washing water during the production thereof were tested and the results are shown in table 1.
TABLE 1 comparison of examples and comparative example data
Sample (I) Light resistance (delta E) L a b Wg COD(mg/L)
Comparative example 0.30 99.32 0.22 1.40 95.44 8.8
Example 1 0.23 99.38 0.18 1.38 95.42 8.9
Example 2 0.21 99.40 0.15 1.36 95.40 9.2
Example 3 021 99.41 0.16 1.37 95.35 9.4
The data show that the titanium dioxide prepared by the invention has good light resistance in papermaking, citric acid is used, and the COD (chemical oxygen demand) of the washing water coated by malic acid is equivalent to that of a comparative example, so that the use of downstream customers is not influenced. It is much lower in cost than the comparative example.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.

Claims (9)

1. A preparation method of titanium dioxide special for papermaking is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
step 1, guiding the sanded slurry into a coating tank; with TiO2Controlling the concentration of the slurry to be 250-800 g/L, and heating to 60-90 ℃;
step 2, performing a first layer of coating on the slurry obtained in the step 1; the film layer of the first coating film is Fe (OH)3A film layer;
step 3, adding a coating agent into the slurry coated with the first layer in the step 2; the coating agent is polybasic acid containing hydroxyl;
step 4, adding a first aluminum salt solution and a phosphate radical-containing solution into the slurry obtained in the step 3 in a parallel flow manner; with P2O5The addition amount of the solution containing phosphate radical accounts for TiO21.0-3.0 wt% of the total amount; with Al2O3The adding amount of the first aluminum salt solution accounts for TiO20.3-1.0 wt% of the total amount;
step 5, adding an alkali solution into the slurry obtained in the step 4, and adjusting the pH value to 8.0-9.5;
step 6, adding a second aluminum salt solution and an acid-base regulator into the slurry obtained in the step 5, regulating and keeping the pH value of the slurry to be 8.0-9.5, and then homogenizing;
step 7, adding a dilute acid solution into the slurry obtained in the step 6, adjusting the pH value to 7.0, and then homogenizing;
and 8, carrying out three-washing, flash evaporation and steam powder treatment on the slurry obtained in the step 7 to obtain a finished product.
2. The preparation method of the special titanium dioxide for papermaking according to claim 1, characterized by comprising the following steps: in step 3, the addition of the polybasic acid accounts for TiO20.3-0.9 wt% of the total amount; the polybasic acid is one of citric acid and malic acid.
3. The preparation method of the special titanium dioxide for papermaking according to claim 1, characterized by comprising the following steps: in step 4, the adding time of the first aluminum salt solution and the phosphate radical-containing solution is 30-60 min.
4. The preparation method of the special titanium dioxide for papermaking according to claim 3, characterized by comprising the following steps: in the step 4, the phosphate radical-containing solution is one or more of a phosphoric acid solution, a dihydrogen phosphate solution, a hydrogen phosphate solution, a phosphate solution and a pyrophosphate solution; the first aluminum salt solution is a sodium metaaluminate solution; with Al2O3The concentration of the sodium metaaluminate solution is 80-200 g/L.
5. The preparation method of the special titanium dioxide for papermaking according to claim 1, characterized by comprising the following steps: in step 6, Al is added2O3The adding amount of the second aluminum salt solution accounts for TiO22.0-3.0 wt% of the total amount.
6. The preparation method of the special titanium dioxide for papermaking according to claim 5, characterized in that: in step 6, Al is added2O3The concentration of the second aluminum salt solution is 80-200 g/L, and the second aluminum salt solution is sodium metaaluminate solution or aluminum sulfate solution.
7. The preparation method of the special titanium dioxide for papermaking according to claim 6, characterized by comprising the following steps: in the step 6, the adding time of the second aluminum salt solution is 90-120 min; the homogenization time was 30 min.
8. The preparation method of the special titanium dioxide for papermaking according to claim 1, characterized by comprising the following steps: in the step 7, the adjusting time of the pH value is 30 min; the homogenization time was 120 min.
9. The preparation method of the special titanium dioxide for papermaking according to claim 1, characterized by comprising the following steps: the dilute acid solution is a sulfuric acid solution; the acid-base regulator is sodium hydroxide solution or sulfuric acid solution.
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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
CN109705630A (en) * 2018-12-21 2019-05-03 中信钛业股份有限公司 A kind of preparation method of high fast light laminated paper titanium dioxide pigment

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