CN107935029B - A kind of purification method of decorating base paper titanium white production raw material - Google Patents
A kind of purification method of decorating base paper titanium white production raw material Download PDFInfo
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- CN107935029B CN107935029B CN201711183959.3A CN201711183959A CN107935029B CN 107935029 B CN107935029 B CN 107935029B CN 201711183959 A CN201711183959 A CN 201711183959A CN 107935029 B CN107935029 B CN 107935029B
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- C01G23/00—Compounds of titanium
- C01G23/008—Titanium- and titanyl sulfate
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Abstract
A kind of purification method of decorating base paper titanium white production raw material, belongs to sulfuric acid method titanium pigment production technical field, is handled in the crystallizing tank with blender, comprising the following steps: titanium sulfate liquid, turn on agitator A, are added into crystallizing tank；B, the pressure inside the tank for controlling crystallizing tank is cooling by material；C, be passed through auxiliary steam into crystallizing tank, while being passed through auxiliary circulation water into crystallizing tank, control auxiliary circulation water into temperature of charge in tank temperature degree and opening temperature, pressure inside the tank, tank；D, be passed through main steam into crystallizing tank, while being passed through major cycle water into crystallizing tank, control major cycle water into temperature of charge in tank temperature degree and opening temperature, pressure inside the tank, tank；E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure, blowing, filtering to pressure inside the tank.The method of the present invention realizes the purification to titanium sulfate liquid, improves the efficiency of ferrous sulfate crystallization in titanium sulfate liquid.
Description
Technical field
The invention belongs to sulfuric acid method titanium pigment production technical field, it is related to a kind of the net of decorating base paper titanium white production raw material
Change method specifically separates the method for ferrous sulfate.Purification method of the present invention can greatly improve ferrous sulfate in titanium sulfate liquid
The efficiency of crystallization realizes the separation to ferrous sulfate, while ensure that iron titanium ratio in titanium sulfate liquid.
Background technique
Sulfuric acid process decorating base paper titanium white production raw material sulphuric acid titanium liquid decomposes titanium ore by the concentrated sulfuric acid and forms, in titanium sulfate liquid
Fe2+Content is higher, influences the granularity and particle diameter distribution, strainability, washing effect that hydrolyze metatitanic acid, and titanium sulfate liquid needs to control
Certain Fe2+/TiO2Value, needs a large amount of Fe before titanium sulfate liquid acidolysis2+With FeSO4·7H2The form of O is separated off, stringent to control
Titanium liquid iron titanium ratio processed is in a suitable range.Ferrous sulfate solubility is influenced by temperature very big.Current each manufacturer
Ferrous sulfate supersaturation crystallization in titanium sulfate liquid all is precipitated using reduction titanium sulfate liquid temperature, then removing is isolated by filtration
FeSO4·7H2The method of O crystal controls iron titanium ratio in titanium sulfate liquid.
There are two types of key industry methods for the temperature of reduction titanium sulfate liquid, and one is the cooling frozen coolings of cryogenic media, usually
It is freezing and crystallizing；One is heat is absorbed by the water in negative pressure evaporation titanium sulfate liquid, titanium sulfate liquid temperature is reduced, is usually cried true
Sky crystallization.The freezing and crystallizing thermal efficiency is low；The vacuum crystallization thermal efficiency is relatively high, and capacity of equipment is relatively large.Vacuum crystallization is gradually
Main method as sulfuric acid method titanium pigment production ferrous sulfate crystallization.Vacuum crystallization belongs to ratio in sulfuric acid method titanium pigment production
A kind of newer method for crystallising, although belonging to physical process, simple process, it is operated and equipment influences clean-up effect, existing
There are poor vacuum crystallization purification method clean-up effect, ferrous sulfate crystallization low efficiency, separation difficult.
Summary of the invention
The problem of present invention aim to address ferrous sulfate separation and above-mentioned described existing ferrous sulfate separation are deposited
The problem of, the present invention realizes the purification to titanium sulfate liquid by starting in terms of crystalline texture and technology controlling and process two, improves
The efficiency of ferrous sulfate crystallization in titanium sulfate liquid.
The present invention be realize its purpose the technical solution adopted is that:
A kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
The following steps are included:
A, titanium sulfate liquid, turn on agitator are added into crystallizing tank；
B, the pressure inside the tank of crystallizing tank is controlled as 6.0-13KPa absolute pressure, material is cooled to 35-38 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 15-20kg/min, while with 1-2m3/ min flow is to crystallization
Auxiliary circulation water is passed through in tank, control auxiliary circulation water is 30-32 DEG C into tank temperature degree, and opening temperature is 35-37 DEG C, crystallizing tank
Pressure inside the tank be 3.0-4.0kPa absolute pressure, temperature of charge is 26-29 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 60-80kg/min, while with 5-6m3/ min flow is to crystallizing tank
In be passed through major cycle water, control major cycle water is 30-32 DEG C into tank temperature degree, and opening temperature is 35-37 DEG C, in the tank of crystallizing tank
Pressure is 1.5-1.8kPa absolute pressure, and temperature of charge is 14-16 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank,
Blowing, filtering.
For the blender in the tilted setting of crystallizing tank, blender and horizontal direction angle are 15-20 °.Present invention stirring
The purpose that device is obliquely installed is to increase Radial Flow, and for angle less than 15 °, Radial Flow gain effect is unobvious；Angle is big
In 20 °, the uniformity of crystal structure is influenced, therefore, it is necessary to 15-20 ° of strict control blenders and horizontal direction angle.
The cylinder of crystallizing tank is increased into 500mm.Equipment increased value is lower than 500mm, and secondary steam folder liquid measure is more, titanium liquid damage
It loses more；Equipment increased value is higher than 500mm, and cylinder is excessively high to will cause vacuum crystallization tank unstability.
The additional amount of titanium sulfate liquid is the 44.6-50% for crystallizing tank volume.
In step A, the revolving speed of blender is 150-200r/min.
The beneficial effects of the present invention are:
1, crystallization technique of the present invention has been saved crystallisation by cooling time, steam consumption, titaniferous in isolated errous sulfate crystal
Amount reduces, and improves Crystallization Separation process yield.
2, the crystal amount of precipitation of ferrous sulfate is indicated in the present invention with iron titanium ratio in purified product, iron titanium ratio is by embodiment
It determines.
3, errous sulfate crystal is byproduct, and the titaniferous amount in errous sulfate crystal is below the titaniferous of reference 0.31%
Amount.
4, the steam of small flow is first passed through in the present invention and water is that crystal generation needs first to generate nucleus, improve the pure of crystal
Degree；It is passed through the steam and water of big flow again, is the thermodynamic cycle in order to guarantee the good boiling and titanium liquid of crystallizing system or more, makes
Ferrous sulfate crystallization is uniformly pure.
5, the pressure in tank is controlled in 6.0-16kPa in step B, makes to reach in crystallizing tank certain vacuum degree, reduced
Titanium liquid boiling point is conducive to ferrous sulfate precipitation, improves titanium liquid purity.
6, material is cooled to 35-40 DEG C, when titanium liquid is extracted by titanium ore in step B, concentrated sulfuric acid heat production, temperature mistake is added
Crystallization in height crystallizing tank not easy to control is precipitated, and ferrous sulfate solubility can be reduced by being cooled to room temperature, and it is brilliant to be conducive to ferrous sulfate
Body is precipitated, and improves titanium liquid purity.
7, the design of step C process is the thermodynamic cycle for being passed through auxiliary steam and promoting titanium liquid, controls the good boiling of titanium liquid
Thermodynamic cycle up and down in improvement material system, is first passed through auxiliary steam, with the flow control of 15-20kg/min, makes nucleus
It generates more and uniform, improves the purity of crystal.
8, the design of step D process is the thermodynamic cycle that logical main steam further promotes titanium liquid, controls the good boiling of titanium liquid
It rises and improves the thermodynamic cycle up and down in material system, main steam is passed through with the flow of 60-80kg/min, it is therefore an objective to promote crystal
Rate of crystalline growth is accelerated in growth.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that blender of the present invention is arranged in crystallizing tank.
Wherein, 01 crystallizing tank is represented, 02 represents blender, and 03 represents secondary steam outlet, and 04 represents discharge port, and 05 represents
Feed inlet, 06 represents outlet of sewer, and 07 represents evacuated tube.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
One, specific embodiment
Embodiment 1
A kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
The volume of crystallizing tank used is 56m3, cylinder has been increased into 500mm on the crystallizing tank of purchase, which increases secondary steam
With titanium sulfate liquid separated space, reduces secondary steam folder liquid measure, reduce the loss of titanium sulfate liquid；Blender and horizontal direction
Angle be 15 °, which increase material by Radial Flow, and material mixes more evenly, and crystalline rate improves, ferrous sulfate
Crystal more evenly, glue wall and reduce by errous sulfate crystal, comprising the following steps:
A, 25m is added into crystallizing tank3Titanium sulfate liquid (concentration TiO2121g/L), turn on agitator controls revolving speed 150r/
min；
B, the pressure inside the tank of crystallizing tank is controlled as 6.9kPa absolute pressure, material is cooled to 38 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 15kg/min, pressure 1.0MPa (table), while with 1m3/min
Flow is passed through auxiliary circulation water into crystallizing tank, and control auxiliary circulation water is 30 DEG C into tank temperature degree, and opening temperature is 35 DEG C, knot
The pressure inside the tank of brilliant tank is 3.5kPa absolute pressure, and temperature of charge is 27 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 60kg/min, while with 5m3/ min flow leads into crystallizing tank
Recirculated water is become owner of, control major cycle water is 31 DEG C into tank temperature degree, and opening temperature is 35 DEG C, and the pressure inside the tank of crystallizing tank is
1.7kPa absolute pressure, temperature of charge is 16 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank,
Blowing, filtering.
Embodiment 2
A kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
The volume of crystallizing tank used is 56m3, cylinder has been increased into 500mm on the crystallizing tank of purchase, which increases secondary steam
With titanium sulfate liquid separated space, reduces secondary steam folder liquid measure, reduce the loss of titanium sulfate liquid；Blender and horizontal direction
Angle be 15 °, which increase material by Radial Flow, and material mixes more evenly, and crystalline rate improves, ferrous sulfate
Crystal more evenly, glue wall and reduce by errous sulfate crystal, comprising the following steps:
A, 26m is added into crystallizing tank3Titanium sulfate liquid (concentration TiO2121g/L), turn on agitator controls revolving speed 170r/
min；
B, the pressure inside the tank of crystallizing tank is controlled as 6.6kPa absolute pressure, material is cooled to 38 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 18kg/min, pressure 1.2MPa (table), while with 1.2m3/
Min flow is passed through auxiliary circulation water into crystallizing tank, control auxiliary circulation water into tank temperature degree be 30 DEG C, opening temperature 35
DEG C, the pressure inside the tank of crystallizing tank is 3.7KPa absolute pressure, and temperature of charge is 29 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 70kg/min, while with 5m3/ min flow leads into crystallizing tank
Recirculated water is become owner of, control major cycle water is 30 DEG C into tank temperature degree, and opening temperature is 35 DEG C, and the pressure inside the tank of crystallizing tank is
1.5kPa absolute pressure, temperature of charge is 14 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank,
Blowing, filtering.
Embodiment 3
A kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
The volume of crystallizing tank used is 56m3, cylinder has been increased into 500mm on the crystallizing tank of purchase, which increases secondary steam
With titanium sulfate liquid separated space, reduces secondary steam folder liquid measure, reduce the loss of titanium sulfate liquid；Blender and horizontal direction
Angle be 20 °, which increase material by Radial Flow, and material mixes more evenly, and crystalline rate improves, ferrous sulfate
Crystal more evenly, glue wall and reduce by errous sulfate crystal, comprising the following steps:
A, 25m is added into crystallizing tank3Titanium sulfate liquid (concentration TiO2121g/L), turn on agitator controls revolving speed 200r/
min；
B, the pressure inside the tank of crystallizing tank is controlled as 7.0kPa absolute pressure, material is cooled to 35 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 20kg/min, pressure 1.2MPa (table), while with 1.8m3/
Min flow is passed through auxiliary circulation water into crystallizing tank, control auxiliary circulation water into tank temperature degree be 32 DEG C, opening temperature 37
DEG C, the pressure inside the tank of crystallizing tank is 4.0kPa absolute pressure, and temperature of charge is 29 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 80kg/min, while with 6m3/ min flow leads into crystallizing tank
Recirculated water is become owner of, control major cycle water is 32 DEG C into tank temperature degree, and opening temperature is 37 DEG C, and the pressure inside the tank of crystallizing tank is
1.5kPa absolute pressure, temperature of charge is 16 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank,
Blowing, filtering.
Embodiment 4
A kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
The volume of crystallizing tank used is 56m3, cylinder has been increased into 500mm on the crystallizing tank of purchase, which increases secondary steam
With titanium sulfate liquid separated space, reduces secondary steam folder liquid measure, reduce the loss of titanium sulfate liquid；Blender and horizontal direction
Angle be 15 °, which increase material by Radial Flow, and material mixes more evenly, and crystalline rate improves, ferrous sulfate
Crystal more evenly, glue wall and reduce by errous sulfate crystal, comprising the following steps:
A, 27m is added into crystallizing tank3Titanium sulfate liquid, turn on agitator control revolving speed 180r/min；
B, the pressure inside the tank of crystallizing tank is controlled as 10kPa absolute pressure, material is cooled to 36 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 17kg/min, while with 1.5m3/ min flow is to crystallizing tank
In be passed through auxiliary circulation water, control auxiliary circulation water is 31 DEG C into tank temperature degree, and opening temperature is 36 DEG C, the tank internal pressure of crystallizing tank
Power is 3.0kPa absolute pressure, and temperature of charge is 26 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 65kg/min, while with 6m3/ min flow leads into crystallizing tank
Recirculated water is become owner of, control major cycle water is 31 DEG C into tank temperature degree, and opening temperature is 36 DEG C, and the pressure inside the tank of crystallizing tank is
1.6kPa absolute pressure, temperature of charge is 15 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank,
Blowing, filtering.
Embodiment 5
A kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
The volume of crystallizing tank used is 56m3, cylinder has been increased into 500mm on the crystallizing tank of purchase, which increases secondary steam
With titanium sulfate liquid separated space, reduces secondary steam folder liquid measure, reduce the loss of titanium sulfate liquid；Blender and horizontal direction
Angle be 20 °, which increase material by Radial Flow, and material mixes more evenly, and crystalline rate improves, ferrous sulfate
Crystal more evenly, glue wall and reduce by errous sulfate crystal, comprising the following steps:
A, 26m is added into crystallizing tank3Titanium sulfate liquid, turn on agitator control revolving speed 160r/min；
B, the pressure inside the tank of crystallizing tank is controlled as 13kPa absolute pressure, material is cooled to 36 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 19kg/min, while with 2m3/ min flow is into crystallizing tank
It is passed through auxiliary circulation water, control auxiliary circulation water is 32 DEG C into tank temperature degree, and opening temperature is 37 DEG C, the pressure inside the tank of crystallizing tank
For 3.3kPa absolute pressure, temperature of charge is 28 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 75kg/min, while with 5m3/ min flow leads into crystallizing tank
Recirculated water is become owner of, control major cycle water is 32 DEG C into tank temperature degree, and opening temperature is 37 DEG C, and the pressure inside the tank of crystallizing tank is
1.8kPa absolute pressure, temperature of charge is 16 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank,
Blowing, filtering.
Embodiment 6
A kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
The volume of crystallizing tank used is 56m3, cylinder has been increased into 500mm on the crystallizing tank of purchase, which increases secondary steam
With titanium sulfate liquid separated space, reduces secondary steam folder liquid measure, reduce the loss of titanium sulfate liquid；Blender and horizontal direction
Angle be 15 °, which increase material by Radial Flow, and material mixes more evenly, and crystalline rate improves, ferrous sulfate
Crystal more evenly, glue wall and reduce by errous sulfate crystal, comprising the following steps:
A, 27m is added into crystallizing tank3Titanium sulfate liquid, turn on agitator control revolving speed 190r/min；
B, the pressure inside the tank of crystallizing tank is controlled as 12kPa absolute pressure, material is cooled to 37 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 16kg/min, while with 1.6m3/ min flow is to crystallizing tank
In be passed through auxiliary circulation water, control auxiliary circulation water is 30 DEG C into tank temperature degree, and opening temperature is 35 DEG C, the tank internal pressure of crystallizing tank
Power is 3.8KPa absolute pressure, and temperature of charge is 29 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 80kg/min, while with 5m3/ min flow leads into crystallizing tank
Recirculated water is become owner of, control major cycle water is 30 DEG C into tank temperature degree, and opening temperature is 37 DEG C, and the pressure inside the tank of crystallizing tank is
1.7kPa absolute pressure, temperature of charge is 15 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank,
Blowing, filtering.
Two, test effect
Compare the embodiment of the present invention and existing crystallization technique makees reference, with crystallization time, steam consumption, ferrous sulfate
Three indexs of crystal titaniferous amount carry out measurement technology effect.As a result it see the table below 1.
Table 1
As shown in Table 1, crystallization technique of the present invention has been saved crystallisation by cooling time, steam consumption, and isolated ferrous sulfate is brilliant
Body titaniferous amount reduces, and improves Crystallization Separation process yield.
Claims (5)
1. a kind of purification method of decorating base paper titanium white production raw material is handled in the crystallizing tank with blender,
It is characterized in that, comprising the following steps:
A, titanium sulfate liquid, turn on agitator are added into crystallizing tank；
B, the pressure inside the tank of crystallizing tank is controlled as 6.0-13KPa absolute pressure, material is cooled to 35-38 DEG C；
C, auxiliary steam is passed through into crystallizing tank with the flow of 15-20kg/min, while with 1-2m3/ min flow is into crystallizing tank
It is passed through auxiliary circulation water, control auxiliary circulation water is 30-32 DEG C into tank temperature degree, and opening temperature is 35-37 DEG C, the tank of crystallizing tank
Interior pressure is 3.0-4.0kPa absolute pressure, and temperature of charge is 26-29 DEG C in tank；
D, main steam is passed through into crystallizing tank with the flow of 60-80kg/min, while with 5-6m3/ min flow leads into crystallizing tank
Recirculated water is become owner of, control major cycle water is 30-32 DEG C into tank temperature degree, and opening temperature is 35-37 DEG C, the pressure inside the tank of crystallizing tank
For 1.5-1.8kPa absolute pressure, temperature of charge is 14-16 DEG C in tank；
E, stop being passed through auxiliary steam, main steam, auxiliary circulation water, major cycle water, be equal to environmental pressure to pressure inside the tank, put
Material, filtering.
2. a kind of purification method of decorating base paper titanium white production raw material according to claim 1, which is characterized in that described
For blender in the tilted setting of crystallizing tank, blender and horizontal direction angle are 15-20 °.
3. a kind of purification method of decorating base paper titanium white production raw material according to claim 1, which is characterized in that will tie
The cylinder of brilliant tank increases 500mm.
4. a kind of purification method of decorating base paper titanium white production raw material according to claim 1, which is characterized in that sulfuric acid
The additional amount of titanium liquid is the 44.6-50% for crystallizing tank volume.
5. a kind of purification method of decorating base paper titanium white production raw material according to claim 1, which is characterized in that step
In A, the revolving speed of blender is 150-200r/min.
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| CN201711183959.3A CN107935029B (en) | 2017-11-23 | 2017-11-23 | A kind of purification method of decorating base paper titanium white production raw material |
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| CN203469527U (en) * | 2013-08-30 | 2014-03-12 | 漯河兴茂钛业股份有限公司 | Multistage high-efficiency titanium liquid vacuum crystallization device |
| CN204865055U (en) * | 2015-06-11 | 2015-12-16 | 江阴市江中设备制造有限公司 | Titanium liquid vacuum crystallization equipment |
| CN105289036A (en) * | 2015-10-27 | 2016-02-03 | 南京白云化工环境监测有限公司 | Novel method for performing vacuum crystallization on ferrous sulfate from titanium liquid in titanium dioxide production process |
| CN106390507B (en) * | 2016-11-23 | 2018-04-10 | 重庆鹏越科技发展有限公司 | A kind of the continuous vacuum crystallization system and its application method of black titanium liquid |
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