CN109160537A - A kind of production technology improving anatase thpe white powder performance - Google Patents

A kind of production technology improving anatase thpe white powder performance Download PDF

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Publication number
CN109160537A
CN109160537A CN201811239377.7A CN201811239377A CN109160537A CN 109160537 A CN109160537 A CN 109160537A CN 201811239377 A CN201811239377 A CN 201811239377A CN 109160537 A CN109160537 A CN 109160537A
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CN
China
Prior art keywords
production technology
white powder
content
improving
thpe white
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Pending
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CN201811239377.7A
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Chinese (zh)
Inventor
陈建立
肖莎莎
冯娜
孙亮
刘晓洁
张曼
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Longmang Group Ltd By Share Ltd Billions
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Longmang Group Ltd By Share Ltd Billions
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Priority to CN201811239377.7A priority Critical patent/CN109160537A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/62L* (lightness axis)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/64Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)

Abstract

The present invention relates to a kind of production technology for improving anatase thpe white powder performance, including ammonium hydroxide neutralizes, washing, slurrying and salt treatment, calcining.Calcination temperature highest, which is effectively reduced, in the present invention reduces about 40 DEG C, calcination temperature reduces, time shortens, and tail gas low-sulfur can achieve discharge standard, saves vent gas treatment cost, it reduces environmental pollution, the sintering situation of material is largely improved, material is softer, is easy to grind, finished product whiteness and reynolds value improve, and the raising of reynolds value is conducive to improve the covering power of material;Filtrate after neutralizing simultaneously can recycle ammonium sulfate by our company's special film processing mode, and water further be recycled, avoid because ammonia-nitrogen content it is unqualified caused by environmental pollution.

Description

A kind of production technology improving anatase thpe white powder performance
Technical field
The present invention relates to a kind of production technologies for improving anatase thpe white powder performance, belong to chemical industry metallurgical field.
Background technique
Titanium dioxide is widely used in applying because having the features such as excellent whiteness, covering power, weatherability and chemical stability Material, plastics, the fields such as papermaking and ink.In nature, titanium dioxide is broadly divided into three kinds of plate titanium-type, rutile titania and rutile crystalline substances Type.Brockite all has stable lattice and becomes due to crystal form is unstable without industrial utility value, anatase titanium dioxide and rutile-type Important white pigment is widely used.
The production technology of anatase titanium dioxide generally includes:
(1) acidolysis: acidolysis reaction is carried out with ilmenite concentrate or acid-soluble waste residue and sulfuric acid, obtains titanyl sulfate;
(2) it hydrolyzes, hydrolysing titanyl sulfate obtains metatitanic acid slurry;
(3) one wash: washing to the metatitanic acid slurry after hydrolysis;
(4) bleaching, two wash: the metatitanic acid after washing to one is bleached, is washed, and obtains the qualified metatitanic acid slurry of washing;
(5) salt treatment: the qualified metatitanic acid of washing is subjected to salt treatment, filters pressing obtains filter cake before kiln;
(6) it calcines: filter cake before kiln being sent into rotary kiln and is calcined, obtains falling kiln product.
Calcination process is divided into dehydration, desulfurization, crystal transfer and grain growth four-stage, production practices in step (6) Middle discovery, the still chemisorption sulfuric acid containing 7% or so is (including one in the qualified metatitanic acid of the middle bleaching washing of step (5) Part combines acid), which not can be removed in water-washing process, can only could remove under calcining kiln high temperature, in this way It will result in the increased costs of vent gas treatment and the increase of calcinating consumption, while easily causing material to be sintered under high temperature, influence to produce The pigment performance of product.
The performance for usually improving anatase thpe white powder, mainly starts in terms of salt treatment.At the salt of anatase thpe white powder Reason agent is generally sylvite and phosphoric acid.Patent No. CN102745740B joined outside traditional salt treatment agent phosphoric acid and sylvite Ammonium salt, pink salt, strontium salt and trace rare-earth element;Patent No. CN106853991A by the way of being added at one time salt treatment agent into Row salt treatment, while adding aluminium chloride again on the basis of traditional salt treatment agent, patent No. CN106853988A is added using disposable The mode for entering salt treatment agent carries out salt treatment, while adding aluminium chloride and magnesium sulfate again on the basis of traditional salt treatment agent.But Salt treatment, than relatively limited, while may bring the raising of Calcine Strength to the improvement of properties of product.
Being there is no at present through the sulfur content before reduction kiln in filter cake reduces Calcine Strength to improve anatase thpe white powder Aspect of performance technology.
Summary of the invention
The object of the invention, which is that, overcomes above-mentioned deficiency, provides a kind of production technology for improving anatase thpe white powder performance. Used technical solution is the present invention to solve above-mentioned technical problem:
To achieve the above object, the present invention is to be achieved through the following technical solutions:
A kind of production technology improving anatase thpe white powder performance, comprising the following steps:
A, the metatitanic acid slurry for taking bleaching washing qualified, is warming up to 60~80 DEG C, is neutralized with ammonium hydroxide, endpoint pH 6.0 ~7.0, it stirs evenly, cures 0.5~2h;
B, slurry after curing in step A is filtered, then washing 15-40min is carried out with deionized water, obtains filter cake;
C, it is beaten with the filter cake that deionized water obtains step B, keeps TiO in slurry2Content is 250~270/L;
D, salt treatment agent is added in the slurry of step C to stir evenly, is filtered, obtains filter cake;
E, filter cake in step D is calcined, using reducing power 100 as material calcining criterion of acceptability;
F, it crushes, detects the whiteness and Reynolds number of finished product.
In order to be better achieved the present invention, in the step A, TiO in metatitanic acid slurry2Content is 210~250g/L.
Further, it in the step A, is neutralized with ammonium hydroxide, endpoint pH is 6.0~7.0;
Further, in the step C, TiO in metatitanic acid slurry2Content is 250~270g/L.
Further, in the step D, salt treatment agent is potassium hydroxide and phosphoric acid, guarantees K in finished product2O content is 0.20%, P2O5Content is 0.30%;
The present invention compared with the prior art, have the following advantages that and the utility model has the advantages that
A, metatitanic acid is by ammonium hydroxide and after sulphur removal, when reaching identical reducing power 100, required calcination temperature highest is reduced about 40 DEG C, the sintering situation of material is largely improved, material is softer, is easy to grind, and finished product whiteness and reynolds value mention Height, the raising of reynolds value are conducive to improve the covering power of material;
B, the filtrate after neutralization can recycle ammonium sulfate by our company's special film processing mode, and water further obtains circulation benefit With, avoid because ammonia-nitrogen content it is unqualified caused by environmental pollution;
C, calcination temperature reduces, and the time shortens, and tail gas low-sulfur can achieve discharge standard, saves vent gas treatment cost, reduces ring Border pollution.
Figure of description
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention is described in further detail below with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1
(1) the metatitanic acid slurry for taking bleaching washing qualified, adjusts TiO2Content is 245g/L, is warming up to 60 DEG C, with ammonium hydroxide tune pH It is 7.0, cures 2h;
(2) it filters slurry after neutralizing and obtains filter cake, then carry out washing 40min with deionized water, filter cake mashing is made into TiO2Contain Amount is 253g/L;
(3) potassium hydroxide, phosphoric acid progress salt treatment are added, is then filtered, K in base-material after guarantee calcining2O content is 0.20%, P2O5Content is 0.30%;
(4) filter cake is calcined in rotary kiln, using reducing power 100 as material calcining criterion of acceptability, and is tested with exhaust analyzer Tail gas sulfur content.
(5) it crushes, detect the whiteness of finished product and disappears black (reynolds value), testing result is shown in Table 1.
Embodiment 2
(1) the metatitanic acid slurry for taking bleaching washing qualified, adjusts TiO2Content is 228g/L, is warming up to 70 DEG C, with ammonium hydroxide condiment Starching pH is 6.7, cures 1.5h;
(2) it filters slurry after neutralizing and obtains filter cake, then carry out washing 25min with deionized water, filter cake mashing is made into TiO2Contain Amount is 263g/L;
(3) potassium hydroxide, phosphoric acid and zinc chloride are added and carries out salt treatment, then filtered, K in base-material after guarantee calcining2O content is 0.20%, P2O5Content is 0.30%;
(4) filter cake is calcined in rotary kiln, using reducing power 100 as material calcining criterion of acceptability, and is tested with exhaust analyzer Tail gas sulfur content.
(5) it crushes, detect the whiteness of finished product and disappears black (reynolds value), testing result is shown in Table 1.
Embodiment 3
(1) the metatitanic acid slurry of bleaching washing qualification is taken, wherein TiO2Content is 219g/L, is warming up to 80 DEG C, with ammonium hydroxide condiment Starching pH is 6.0, cures 0.5h;
(2) it filters slurry after neutralizing and obtains filter cake, then carry out washing 15min with deionized water, filter cake mashing is made into TiO2Contain Amount is 268g/L;
(3) potassium hydroxide, phosphoric acid and zinc chloride are added and carries out salt treatment, then filtered, K in base-material after guarantee calcining2O content is 0.20%, P2O5Content is 0.30%;
(4) filter cake is calcined in rotary kiln, using reducing power 100 as material calcining criterion of acceptability, and is tested with exhaust analyzer Tail gas sulfur content.
(5) it crushes, detect the whiteness of finished product and disappears black (reynolds value), testing result is shown in Table 1.
Comparative example
(1) the metatitanic acid slurry for taking bleaching washing qualified, TiO2Content is 309g/L, and addition potassium hydroxide, phosphoric acid carry out at salt Reason, then filters, K in base-material after guarantee calcining2O content is 0.20%, P2O5Content is 0.30%;
(2) filter cake is calcined in rotary kiln, using reducing power 100 as material calcining criterion of acceptability, and is tested with exhaust analyzer Tail gas sulfur content.
(3) it crushes, detect the whiteness of finished product and disappears black (reynolds value), testing result is shown in Table 1.
Each embodiment index of correlation testing result contrast table of table 1
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technical staff of the industry It should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe the present invention Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent Object defines.
The present invention relates to it is a kind of improve anatase thpe white powder performance production technology, including ammonium hydroxide neutralize, washing, slurrying and Salt treatment, calcining and etc..Calcination temperature highest, which is effectively reduced, in the present invention reduces about 40 DEG C, and calcination temperature reduces, and the time shortens, Tail gas low-sulfur can achieve discharge standard, saves vent gas treatment cost, reduces environmental pollution, largely improve material It is sintered situation, material is softer, is easy to grind, and finished product whiteness and reynolds value improve, and the raising of reynolds value is conducive to improve object The covering power of material;Filtrate after neutralizing simultaneously can recycle ammonium sulfate by our company's special film processing mode, and water further obtains To recycling, avoid because ammonia-nitrogen content it is unqualified caused by environmental pollution.

Claims (5)

1. a kind of production technology for improving anatase thpe white powder performance, it is characterised in that: the raising anatase titanium dioxide mealiness Can production technology the following steps are included:
A, the metatitanic acid slurry for taking bleaching washing qualified, is warming up to 60~80 DEG C, is neutralized with ammonium hydroxide, endpoint pH 6.0 ~7.0, it stirs evenly, cures 0.5~2h;
B, slurry after curing in step A is filtered, then 15~40min of washing is carried out with deionized water, obtains filter cake;
C, it is beaten with the filter cake that deionized water obtains step B, keeps TiO in slurry2Content is 250~270/L;
D, salt treatment agent is added in the slurry of step C to stir evenly, is filtered, obtains filter cake;
E, filter cake in step D is calcined, using reducing power 100 as material calcining criterion of acceptability;
F, it crushes, detects the whiteness and Reynolds number of finished product.
2. a kind of production technology for improving anatase thpe white powder performance according to claim 1, which is characterized in that the step In rapid A, TiO in metatitanic acid slurry2Content is 210~250g/L.
3. a kind of production technology for improving anatase thpe white powder performance according to claim 1, which is characterized in that the step It in rapid A, is neutralized with ammonium hydroxide, endpoint pH is 6.0~7.0.
4. a kind of production technology for improving anatase thpe white powder performance according to claim 1, which is characterized in that the step In rapid C, TiO in metatitanic acid slurry2Content is 250~270g/L.
5. a kind of production technology for improving anatase thpe white powder performance according to claim 1, which is characterized in that the step In rapid D, salt treatment agent is potassium hydroxide and phosphoric acid, guarantees K in finished product2O content is 0.20%, P2O5Content is 0.30%.
CN201811239377.7A 2018-10-23 2018-10-23 A kind of production technology improving anatase thpe white powder performance Pending CN109160537A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113044879A (en) * 2021-03-22 2021-06-29 龙蟒佰利联集团股份有限公司 Method for improving quality of sulfuric acid process titanium dioxide
CN115367795A (en) * 2022-09-01 2022-11-22 山东东佳集团股份有限公司 Novel process for preparing ammonium sulfate by recycling catalyst titanium dioxide water washing liquid in acid making tail gas system

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1766137A (en) * 2005-11-11 2006-05-03 陈泽安 Hydrochloric acid-extraction method for preparing rutile titanium white
CN106853991A (en) * 2015-12-09 2017-06-16 攀枝花大互通钛业有限公司 The method for producing anatase thpe white powder
CN108408770A (en) * 2018-06-08 2018-08-17 龙蟒佰利联集团股份有限公司 A kind of metatitanic acid sulphur removal production technology

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1766137A (en) * 2005-11-11 2006-05-03 陈泽安 Hydrochloric acid-extraction method for preparing rutile titanium white
CN106853991A (en) * 2015-12-09 2017-06-16 攀枝花大互通钛业有限公司 The method for producing anatase thpe white powder
CN108408770A (en) * 2018-06-08 2018-08-17 龙蟒佰利联集团股份有限公司 A kind of metatitanic acid sulphur removal production technology

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113044879A (en) * 2021-03-22 2021-06-29 龙蟒佰利联集团股份有限公司 Method for improving quality of sulfuric acid process titanium dioxide
CN113044879B (en) * 2021-03-22 2023-11-03 龙蟒佰利联集团股份有限公司 Method for improving quality of titanium dioxide by sulfuric acid method
CN115367795A (en) * 2022-09-01 2022-11-22 山东东佳集团股份有限公司 Novel process for preparing ammonium sulfate by recycling catalyst titanium dioxide water washing liquid in acid making tail gas system
CN115367795B (en) * 2022-09-01 2024-02-20 山东东佳集团股份有限公司 Novel process for preparing ammonium sulfate by recycling catalyst titanium dioxide washing liquid in acid-making tail gas system

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