CN105347390A - Method for reducing iron content of metatitanic acid prepared by sulfuric acid method - Google Patents

Method for reducing iron content of metatitanic acid prepared by sulfuric acid method Download PDF

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Publication number
CN105347390A
CN105347390A CN201510833520.5A CN201510833520A CN105347390A CN 105347390 A CN105347390 A CN 105347390A CN 201510833520 A CN201510833520 A CN 201510833520A CN 105347390 A CN105347390 A CN 105347390A
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China
Prior art keywords
metatitanic acid
sulfuric acid
slurry
acid
iron level
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Chinese (zh)
Inventor
袁立军
朱玉杰
刘琦
柳令
景建林
廖荣华
周俊
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Titanium Industry Co Ltd of Pangang Group
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Titanium Industry Co Ltd of Pangang Group
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Priority to CN201510833520.5A priority Critical patent/CN105347390A/en
Publication of CN105347390A publication Critical patent/CN105347390A/en
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Abstract

The invention belongs to the field of titanium dioxide preparation, and particularly relates to a method for reducing iron content of metatitanic acid prepared by a sulfuric acid method. The method provided by the invention aims to solve the technical problem that the whiteness is affected as the iron content in titanium dioxide prepared by the existing method is relatively high. The scheme for solving the technical problem is to provide the method for reducing iron content of metatitanic acid prepared by the sulfuric acid method. The method comprises the following steps: a, adding desalinated water into metatitanic acid to obtain slurry, and adjusting the pH value of the slurry to 3-7; b, maintaining the temperature of the slurry at 30-60 DEG C, and adding EDTA to react for 1-2 hours; and c, filtering and washing the reacted slurry to obtain low-iron metatitanic acid. The method provided by the invention is simple and feasible, and provides a new option for reducing the iron content in titanium dioxide prepared by the sulfuric acid method.

Description

Reduce the method for iron level in sulfuric acid process metatitanic acid
Technical field
The invention belongs to titanium dioxide preparation field, be specifically related to the method reducing iron level in sulfuric acid process metatitanic acid.
Background technology
Titanium dioxide is a kind of white pigment of performance brilliance, can be widely used in the fields such as coating, plastics, papermaking, ink, catalyzer and the cosmetics of super quality.In sulfuric acid method titanium pigment production technique, after washing, the prolongation of Trace Iron impurity along with washing time in metatitanic acid, the reduction of acidity, oxidized gradually, exists, cannot be removed, be converted into Fe by washing with the form of solid hydrogen oxidation high ferro 2o 3massfraction at about 30PPM, the whiteness of its dry powder is between 92.5-94.0, if reduce the iron level of 5 PPM, the whiteness of dry powder will between 94.5-96.5.For production high-end coating, high-end titanium dioxide used for decorative paper, it will seriously have influence on the whiteness of titanium dioxide.
Summary of the invention
The technical problem to be solved in the present invention is that in the titanium dioxide prepared of existing method, iron-holder is higher, affects whiteness.
The scheme that the present invention solves the problems of the technologies described above is to provide a kind of method reducing iron level in sulfuric acid process metatitanic acid, comprises the following steps:
A, in metatitanic acid, add de-salted water, obtain slurry; The pH value regulating slurry is 3 ~ 7;
B, the temperature of slurry is remained on 30 ~ 60 DEG C, add EDTA (ethylenediamine tetraacetic acid (EDTA)), react 1 ~ 2 hour;
C, reacted slurry after filtration, washing, obtain the metatitanic acid of low iron.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, the metatitanic acid described in step a be in sulfuric acid method titanium pigment production technique washing after metatitanic acid.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, described in step a, the iron level of metatitanic acid is converted into Fe 2o 3massfraction count 30 ~ 100PPM.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, adding de-salted water described in step a is to make the concentration of slurry be that 200 ~ 260 grams per liters are (with TiO 2meter).
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, described in step a, pH value sulfuric acid regulates.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, the add-on of EDTA described in step b is that metatitanic acid is (with TiO 2meter) quality 0.1 ~ 1%.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, the solid content of metatitanic acid described in step c is 50 ~ 60%.
Method provided by the invention is simple, by the metatitanic acid after washing, adds certain proportion EDTA, uses certain density acidic solution to carry out washing metatitanic acid, significantly can reduce the iron level in metatitanic acid, meanwhile, improve the whiteness of titanium dioxide.
Embodiment
Reduce the method for iron level in sulfuric acid process metatitanic acid, comprise the following steps:
A, in metatitanic acid, add de-salted water, obtain slurry; The pH value regulating slurry is 3 ~ 7;
B, the temperature of slurry is remained on 30 ~ 60 DEG C, add EDTA, react 1 ~ 2 hour;
C, reacted slurry after filtration, washing, obtain the metatitanic acid of low iron.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, the metatitanic acid described in step a be in sulfuric acid method titanium pigment production technique washing after metatitanic acid.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, described in step a, the iron level of metatitanic acid is converted into Fe 2o 3massfraction count 30 ~ 100PPM.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, adding de-salted water described in step a is to make the concentration of slurry be that 200 ~ 260 grams per liters are (with TiO 2meter).
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, described in step a, pH value sulfuric acid regulates.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, the add-on of EDTA described in step b is that metatitanic acid is (with TiO 2meter) quality 0.1 ~ 1%.
If EDTA add-on is very few do not reach the effect reducing iron level, EDTA add-on is too much, and Financial cost can increase, and extends the washing time of washing procedure simultaneously.
In above-mentioned reduction sulfuric acid process metatitanic acid iron level method in, the solid content of metatitanic acid described in step c is 50 ~ 60%.
Embodiment 1
Metatitanic acid 500g in sulfuric acid method titanium pigment production technique after washing, iron level (is converted into Fe 2o 3massfraction meter) be 35PPM, add de-salted water 500g, obtain the slurry that concentration is 260 grams per liters (titanium dioxide meter), sulfuric acid is used to control slurry pH about 5, temperature keeps 30 ~ 60 degree, adds EDTA0.2g, abundant stirring reaction 1 hour.
The slurry of sufficient reacting is carrying out press filtration with diaphragm pressing machine, and washing, obtain product, its metatitanic acid solid content is 55%.
Embodiment 2
Metatitanic acid 500g in sulfuric acid method titanium pigment production technique after washing, iron level (is converted into Fe 2o 3massfraction meter) be 35PPM, add de-salted water 500g, obtain the slurry that concentration is 260 grams per liters (titanium dioxide meter), sulfuric acid is used to control slurry pH about 5.5, temperature keeps 30 ~ 60 degree, adds EDTA1g, abundant stirring reaction 1 hour.
The slurry of sufficient reacting is carrying out press filtration with diaphragm pressing machine, and washing, obtain product, its metatitanic acid solid content is 55%.
Embodiment 3
Metatitanic acid 500g in sulfuric acid method titanium pigment production technique after washing, iron level (is converted into Fe 2o 3massfraction meter) be 35PPM, add de-salted water 500g, obtain the slurry that concentration is 260 grams per liters (titanium dioxide meter), use sulfuric acid to control slurry pH about 6, temperature keeps 30 ~ 60 degree, interpolation EDTA2g, abundant stirring reaction 1 hour.
The slurry of sufficient reacting is carrying out press filtration with diaphragm pressing machine, and washing, obtain product, its metatitanic acid solid content is 55%.
Above 3 samples are made the transition into rutile titanium white powder sample for 2 hours 890 degree of high-temperature calcinations under similarity condition, compares in the detection carrying out dry powder whiteness and trace element.
Conclusion:
The product sample that embodiment 1 ~ 3 prepares is made standard jig, adopts the method for GB/T1706-2006 to detect whiteness with whiteness instrument.
Detect trace elements iron with XRF instrument, the method is all better to the analytical results preci-sion and accuracy of titanium white medium trace element, can meet the quality monitoring of titanium powder plant production process.The results are shown in Table 1.
Table 1
Fe content in table 1 is converted into Fe 2o 3massfraction calculate.
From table 1, the titanium dioxide adopting the inventive method to prepare, significantly can reduce iron level in titanium dioxide and improve the whiteness of titanium dioxide simultaneously.

Claims (7)

1. reduce the method for iron level in sulfuric acid process metatitanic acid, comprise the following steps:
A, in metatitanic acid, add de-salted water, obtain slurry; The pH value regulating slurry is 3 ~ 7;
B, the temperature of slurry is remained on 30 ~ 60 DEG C, add ethylenediamine tetraacetic acid (EDTA), react 1 ~ 2 hour;
C, reacted slurry after filtration, washing, obtain the metatitanic acid of low iron.
2. the method for iron level in reduction sulfuric acid process metatitanic acid according to claim 1, is characterized in that: the metatitanic acid described in step a is the metatitanic acid in sulfuric acid method titanium pigment production technique after washing.
3. the method for iron level in reduction sulfuric acid process metatitanic acid according to claim 1, is characterized in that: described in step a, the iron level of metatitanic acid is converted into Fe 2o 3massfraction count 30 ~ 100PPM.
4. the method for iron level in reduction sulfuric acid process metatitanic acid according to claim 1, is characterized in that: adding de-salted water described in step a is to make the concentration of slurry be that 200 ~ 260 grams per liters are (with TiO 2meter).
5. the method for iron level in reduction sulfuric acid process metatitanic acid according to claim 1, is characterized in that: described in step a, pH value sulfuric acid regulates.
6. the method for iron level in reduction sulfuric acid process metatitanic acid according to claim 1, is characterized in that: the add-on of ethylenediamine tetraacetic acid (EDTA) described in step b is that metatitanic acid is (with TiO 2meter) quality 0.1 ~ 1%.
7. the method for iron level in reduction sulfuric acid process metatitanic acid according to claim 1, is characterized in that: the solid content of the metatitanic acid described in step c is 50 ~ 60%.
CN201510833520.5A 2015-11-25 2015-11-25 Method for reducing iron content of metatitanic acid prepared by sulfuric acid method Pending CN105347390A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111470532A (en) * 2020-06-15 2020-07-31 云南中烟工业有限责任公司 Method for preparing nano anatase titanium dioxide from cold rolling titanic acid washing waste liquid
CN114014355A (en) * 2021-09-16 2022-02-08 攀枝花学院 Method for purifying and deironing industrial metatitanic acid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
历明涛: "含钛高炉渣中钛的浸出及提取工艺的实验研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111470532A (en) * 2020-06-15 2020-07-31 云南中烟工业有限责任公司 Method for preparing nano anatase titanium dioxide from cold rolling titanic acid washing waste liquid
CN114014355A (en) * 2021-09-16 2022-02-08 攀枝花学院 Method for purifying and deironing industrial metatitanic acid
CN114014355B (en) * 2021-09-16 2023-07-25 攀枝花学院 Industrial meta-titanic acid purifying and deironing method

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Application publication date: 20160224