CN105949823B - A kind of method that chlorination by-product hydrochloric acid is used for titanium dioxide coating - Google Patents
A kind of method that chlorination by-product hydrochloric acid is used for titanium dioxide coating Download PDFInfo
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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
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/3669—Treatment with low-molecular organic compounds
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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
Abstract
The invention discloses a kind of methods that chlorination by-product hydrochloric acid is used for titanium dioxide coating, this method passes through spare after the crude salt acid progress impurity elimination to chlorinated exhaust washing recycling, and using zirconates, silicon salt, aluminium salt and inorganic coating is carried out to titanium dioxide, it is coated again using organic coated dose, obtains superior in quality titanium dioxide coated product.The acid that the method for the titanium dioxide coating of the present invention uses is the crude salt acid that chlorinated exhaust washing recycling obtains, and by using inorganic and organic composite coating process, hydrophily, resistance to chalking, reducing power and the colour retention of titanium dioxide are greatly improved, while improves titanium dioxide wetability, dispersiveness and covering power in a dispersion medium.
Description
Technical field
The present invention relates to a kind of preparation methods of coating titanium dioxide, and in particular to a kind of chlorination by-product hydrochloric acid is used for titanium dioxide
The method of coating.
Background technology
Titanium dioxide scientific name is titanium dioxide, it is considered to be the best a kind of white pigment of performance in the world has higher
Covering power, weatherability, reducing power etc. are widely used in coating, plastics, papermaking, printing ink, chemical fibre, rubber, ceramics, makeup
The Fine Chemicals such as product, food and medicine.The method of production titanium dioxide mainly has two kinds of techniques of sulfuric acid process and chloridising at present.
Sulfuric acid process is that titanium-iron powder and the concentrated sulfuric acid are carried out acidolysis reaction production titanium sesquisulfate, and metatitanic acid is generated through hydrolysis, then
Titanium dioxide product is obtained through being calcined, crushing.The advantage of this process is that can be using the low ilmenite being easy to get of valency and sulfuric acid as raw material, skill
Art is more ripe, and equipment is simple, and anticorrosion material easily solves.The drawback is that long flow path, it can only be based on intermittently operated, wet method behaviour
Make, sulfuric acid, water consumption are high, and waste and by-product are more, cause serious pollution to the environment.
Chloridising is that high-temp chlorination production essence four is carried out after mixing rutile, ilmenite concentrate or high-titanium slag powder with coke
Titanium chloride, rectifying, except vanadium after, carry out high-temperature oxydation, classification, surface treatment, using filter, washing, it is dry, crush and obtain titanium white
Powder product.Its advantage is that flow is short, and production capacity easily expands, and continuous and automatic degree is high, and energy consumption is relatively low, and it is excellent that " three wastes " are few etc.
Point, due to its advantage in environmental protection and product quality, chloridising becomes the direction of domestic titanium dioxide industry industrial upgrading.In chlorine
In change method titanium white production, often with the generation of chlorinated exhaust, condensation afterchlorinate tail gas contains TiCl4、SiCl4It is acid with HCl etc.
Gas, in order to recycle the HCl gas in chlorinated exhaust, according to TiCl4、SiCl4Facile hydrolysis generates TiOCl respectively2、
H4SiO4Chlorinated exhaust is removed TiCl by colloidal sol and hydrochloric acid by two level pickling tower and one-stage water wash tower respectively4、SiCl4Etc. acidity
Subsequently into Chlorine Scrubber, one-stage water wash tower and two level pickling tower and tail gas adverse current are passed through using process water respectively for gas,
Level-one pickling tower generates 20% crude salt acid.
Not surface treated TiO2Pigment has photochemical activity, and surrounding organic matter can be made to degrade, and generates
Powder phenomenon-tion.The TiO of practical application2Pigment must be surface-treated, i.e., in TiO2Particle surface forms the film continuously coated,
Make TiO2Particle formed between surrounding organic matter together with barrier.High-quality titanium dioxide is mainly by import, due to external core
Technology blockage, the rutile conversion ratio for causing the titanium dioxide of domestic titanium dioxide enterprise production is relatively low, and titanium white comprehensive performance is poor,
The titanium dioxide that can not be produced in quality and in price with transnational enterprises such as the U.S. competes,
The content of the invention
The purpose of the present invention is in view of the above-mentioned problems of the prior art, providing a kind of chlorination by-product hydrochloric acid for titanium white
The method of powder coating.
A kind of method that chlorination by-product hydrochloric acid is used for titanium dioxide coating, comprises the following steps：
Chlorination by-product hydrochloric acid refers to the crude salt acid obtained using chlorinated exhaust after washing, purifying, and chlorinated exhaust is passed through
After washing obtains the hydrochloric acid solution that mass concentration is 20%, the crude salt acid solution is subjected to preliminary sedimentation into first deep gouge, on
Clear liquid enters hydrochloric acid storage tank；Bottom underflow in first deep gouge filters TiOCl therein into a membrane filtration system2, filtrate salt
Acid enters hydrochloric acid storage tank；As the TiOCl of membrane filtration system filtering2When reaching the limitation, backwash operation is carried out, with water by TiOCl2Punching
Under, filter membrane enters next filter cycle；When being rinsed with water TiOCl2When, TiOCl2It reacts with water, generates TiO2With
HCl, HCl are dissolved in water and form hydrochloric acid solution；Contain TiO2The hydrochloric acid solution of solid enters secondary membrane filtration system, and filtering is therein
TiO2, filtrate hydrochloric acid enters hydrochloric acid storage tank；Then by the hydrochloric acid that hydrochloric acid storage tank is collected with pure water be diluted to mass concentration for 5%~
10%, it is spare；
(1), it is 5%~10% crude salt acid to be diluted to mass concentration with pure water, spare；
(2), to the tio_2 suspension that concentration is 10-30wt%, the 0.02- of addition titanium dioxide powder weight
0.3% calgon adjusts pH to 8-12 with sodium hydroxide, is stirred for 2-4h, obtains Titanium dioxide slurry；
(3), in the Titanium dioxide slurry obtained by step (2), it is 60-90 DEG C to adjust temperature, and it is 7- to add in salt acid for adjusting pH
9, it then adds in plus zirconates, the addition of zirconates accounts for the 0.5-2% of titanium dioxide powder weight, 30-100min followed by aging, then
It is secondary with salt acid for adjusting pH to 7-9, then cure 50-90min；
(4), slurry obtained by above-mentioned steps (3) is adjusted into temperature to 60-80 DEG C, adds in water soluble silicon compound, use hydrochloric acid
Adjusting pH value is 7.5-8.6, and inactive slurry 30-120min makes silicon be deposited in titanium dioxide powder particle in the form of silica
Surface, wherein, with SiO2The addition for counting water soluble silicon compound is the 0.5-8% of titanium dioxide powder weight, is mixed
Slurry；
(5), in the mixed slurry obtained by above-mentioned steps (4), water-soluble aluminum salt is added in, is configured to the molten of 20-100g/L
Liquid adjusts temperature to 60-90 DEG C, and adding in sodium hydroxide makes the pH of mixed slurry be maintained at 8-10, can stir evenly,
Then add in hydrochloric acid be adjusted to neutrality, and be kept stirring 1-3 it is small when, make aluminium salt complete hydrolysis；Wherein, with A12O3Count water-soluble aluminum
The addition of salt is the 1-6% of titanium dioxide powder weight, obtains slurry；
(6), slurries obtained by step (5) filtered, washed, gained filter cake drying, grinding obtain surface modification
Titanium white powder particles；
(7), the organic matter of titanium dioxide granular mass 0.2-1.5wt% is added in into titanium white powder particles obtained by step (6),
30-100min is stirred at 40-70 DEG C, obtains Titanium dioxide slurry；
(8), Titanium dioxide slurry obtained by step (7) is filtered, washes, dried at 100-130 DEG C, through crushing, i.e.,
Obtain inorganic and organic coated titanium dioxide.
Wherein, the effect of calgon mainly improves dispersiveness of the titanium dioxide in slurry in step (2), improves grinding
Efficiency；
One or more of the zirconates in zirconium sulfate, zirconium oxychloride, zirconium chloride described in step (3)；
Water soluble silicon compound described in step (4) is selected from one or both of sodium metasilicate, sodium metasilicate；
One or more of the water-soluble aluminum salt in aluminum sulfate, aluminium chloride, sodium metaaluminate described in step (5)；
Organic matter described in step (7) is selected from trimethylolpropane, trimethylolethane, triethanolamine, neopentyl glycol, silicon
The one or more such as oil.
Advantageous effect
The present invention carries out the preparation of titanium dioxide coating by the crude salt acid obtained to chlorinated exhaust washing recycling, with conventional profit
Chlorinated exhaust technique is directly washed with NaOH lye to compare, and has not only been saved production cost, but also has been created new value for enterprise.
The titanium dioxide haveing excellent performance is made using inorganic and organic composite coating process simultaneously in the present invention, covering power, resistance to
Hou Xing, dispersiveness and resistance to chalking etc. are greatly improved.Wherein, aluminium coating main function is to improve titanium dioxide anti-powdering
Performance improves glossiness and whiteness, reduces titanium dioxide photochemical activity, improves weatherability；Silicon coating is with silica modified
Titanium dioxide, after showing to be formed fine and close film at it, the weatherability of titanium dioxide is especially good, strong covering power；Zirconium coating can improve
Weatherability, glossiness and the durability of titanium dioxide；Organic coated main function is to improve the scattered energy of titanium dioxide in media as well
Power, different disposal agent improve pigment lipophile or hydrophily, improve coating bin stability, improve gloss of film and titanium dioxide disappears
Color power and covering power.Therefore the hydrophily of titanium dioxide, resistance to chalking greatly improved using inorganic and organic composite coating agent, disappeared
Color power and colour retention, while improve titanium dioxide wetability, dispersiveness and covering power in a dispersion medium, with individually it is organic,
Inorganic coating agent is compared, and comprehensive performance is more excellent.
Specific embodiment
With reference to the embodiment of the present invention, the invention will be further elaborated
Embodiment 1
(1), it is 5%~10% crude salt acid to be diluted to mass concentration with pure water, spare；
(2), to concentration be 10wt% tio_2 suspension, add in titanium dioxide powder weight 0.02% six partially
Sodium phosphate adjusts pH to 8 with sodium hydroxide, is stirred for 2h, obtains Titanium dioxide slurry；
(3), it is 9 salt acid for adjusting pH to be added in Titanium dioxide slurry obtained by step (2), is warming up to 60 DEG C, is then slowly added
Zirconium sulfate, the addition of zirconium sulfate account for the 0.5% of titanium dioxide powder weight, 30min followed by aging, again with salt acid for adjusting pH
To 7, then cure 50min；
(4), in the mixed powder slurry obtained by step (3), 70 DEG C are warming up to, adds in sodium metasilicate (with SiO2Meter) it is dioxy
Change the 0.5% of titanium valve weight, obtain mixed slurry, be 7.5, inactive slurry 30min with salt acid for adjusting pH value, make silicon to aoxidize
The form of silicon is deposited in titanium dioxide powder particle surface；
(5), in the mixed slurry obtained by above-mentioned steps (4), aluminium chloride is added in, addition is titanium dioxide powder weight
1%, be configured to 20g/L (with A12O3Meter) solution, be warming up to 80 DEG C, and adding in sodium hydroxide keeps the pH of mixed slurry
8, can stir evenly, when then adding in inorganic acid and be adjusted to neutrality, and being kept stirring 1, make aluminium salt complete hydrolysis, obtain
To slurry；
(6), slurries obtained by step (5) filtered, washed, gained filter cake drying, grinding obtain surface modification
Titanium white powder particles；
(7), the trimethylolpropane of titanium dioxide granular mass 0.2wt% is added in into titanium white powder particles obtained by step (6),
30min is stirred at 40 DEG C, obtains Titanium dioxide slurry；
(8), Titanium dioxide slurry obtained by step (7) is filtered, washes, dried at 50 DEG C, through crushing to get to nothing
Machine and organic coated titanium dioxide, the titanium dioxide performance indicator after coating are shown in Table 1.
Embodiment 2
(1), it is 5%~10% crude salt acid to be diluted to mass concentration with pure water, spare；
(2), to concentration be 20wt% tio_2 suspension, add in titanium dioxide powder weight 0.2% six partially
Sodium phosphate adjusts pH to 10 with sodium hydroxide, is stirred for 3h, obtains Titanium dioxide slurry；
(3), in the Titanium dioxide slurry obtained by step (2), 80 DEG C are warming up to, it is 8 to add in salt acid for adjusting pH, then slowly
Oxygenation zirconium chloride, the addition of zirconium oxychloride account for the 1% of titanium dioxide powder weight, 60min followed by aging, again with hydrochloric acid tune
PH is saved to 8, then cures 60min；
(4), by above-mentioned steps (3) obtained by mixed slurry, cool to 70 DEG C, add in sodium metasilicate (with SiO2Meter) it is two
The 3% of titanium oxide powder weight is 8.2 with salt acid for adjusting pH value, and inactive slurry 60min makes silicon be precipitated in the form of silica
In titanium dioxide powder particle surface, mixed slurry is obtained；
(5), aluminum sulfate is added in the slurry after step (4) complete hydrolysis, addition is titanium dioxide powder weight
5%, 80g/L is configured to (with A12O3Meter) solution, be warming up to 80 DEG C, and adding in sodium hydroxide is maintained at the pH of mixed slurry
9, can stir evenly, then add in hydrochloric acid be adjusted to neutrality, and be kept stirring 2 it is small when, make aluminium salt complete hydrolysis, obtain
Slurry；
(6), slurries obtained by step (5) filtered, washed, gained filter cake drying, grinding obtain surface modification
Titanium white powder particles；
(7), added in titanium white powder particles obtained by the step (6) titanium dioxide granular mass 1wt% trimethylolethane and
Neopentyl glycol mixed liquor stirs 90min at 65 DEG C, obtains Titanium dioxide slurry；
(8), Titanium dioxide slurry obtained by step (7) is filtered, washes, dried at 85 DEG C, through crushing to get to nothing
Machine and organic coated titanium dioxide, the titanium dioxide performance indicator after coating are shown in Table 1.
Embodiment 3
(1), it is 5%~10% crude salt acid to be diluted to mass concentration with pure water, spare；
(2), to concentration be 30wt% tio_2 suspension, add in titanium dioxide powder weight 0.3% six partially
Sodium phosphate adjusts pH to 12 with sodium hydroxide, is stirred for 4h, obtains Titanium dioxide slurry；
(3), into the Titanium dioxide slurry obtained by step (2), 85 DEG C are warming up to, it is 9 to add in salt acid for adjusting pH, then slowly
Add zirconium chloride, the addition of zirconium chloride accounts for the 2% of titanium dioxide powder weight, 30-100min followed by aging, again with hydrochloric acid tune
PH is saved to 9, then cures 90min；
(4), by the mixed slurry obtained by above-mentioned steps (3), 70 DEG C are cooled to, the addition of sodium metasilicate is (with SiO2Meter)
It is 8.6 with salt acid for adjusting pH value, inactive slurry 120min makes silicon in the form of silica for the 2% of titanium dioxide powder weight
Titanium dioxide powder particle surface is deposited in, obtains mixed slurry；
(5), sodium metaaluminate is added in the slurry after step (4) complete hydrolysis, addition is titanium dioxide powder weight
6%, be configured to 100g/L (with A12O3Meter) solution, be warming up to 80 DEG C, and adding in sodium hydroxide protects the pH of mixed slurry
Hold 10, can stir evenly, then add in hydrochloric acid be adjusted to neutrality, and be kept stirring 1.5 it is small when, make the complete water of aluminium salt
Solution obtains slurry；
(6), slurries obtained by step (5) filtered, washed, gained filter cake drying, grinding obtain surface modification
Titanium white powder particles；
(7), the trimethylolethane of titanium dioxide granular mass 1.5wt% is added in into titanium white powder particles obtained by step (6)
And silicone oil, 100min is stirred at 70 DEG C, obtains Titanium dioxide slurry；
(8), Titanium dioxide slurry obtained by step (7) is filtered, washes, dried at 50-100 DEG C, through crush to get
To inorganic and organic coated titanium dioxide, the titanium dioxide performance indicator after coating is shown in Table 1.
Titanium dioxide performance detection index obtained by table 1, embodiment
Claims (5)
1. a kind of method that chlorination by-product hydrochloric acid is used for titanium dioxide coating, it is characterised in that：Comprise the following steps：
(1), it is 5%~10% crude salt acid to be diluted to mass concentration with pure water, spare；
(2), to the tio_2 suspension that concentration is 10-30wt%, add in the 0.02-0.3%'s of titanium dioxide powder weight
Calgon adjusts pH to 8-12 with sodium hydroxide, is stirred for 2-4h, obtains Titanium dioxide slurry；
(3), in the Titanium dioxide slurry obtained by step (2), it is 60-90 DEG C to adjust temperature, adds in hydrochloric acid spare in step (1)
Adjusting pH is 7-9, then adds in zirconates, the addition of zirconates accounts for the 0.5-2% of titanium dioxide powder weight, followed by aging
30-100min again with salt acid for adjusting pH spare in step (1) to 7-9, then cures 50-90min；
(4), slurry obtained by above-mentioned steps (3) is adjusted into temperature to 60-80 DEG C, water soluble silicon compound is added in, in step (1)
Spare salt acid for adjusting pH value is 7.5-8.6, and inactive slurry 30-120min makes silicon be deposited in titanium dioxide in the form of silica
Titanium valve body particle surface, wherein, with SiO2The addition for counting water soluble silicon compound is the 0.5- of titanium dioxide powder weight
8%, obtain mixed slurry；
(5), in the mixed slurry obtained by above-mentioned steps (4), water-soluble aluminum salt is added in, is configured to the solution of 20-100g/L, is adjusted
Temperature is saved to 60-90 DEG C, and adding in sodium hydroxide makes the pH of mixed slurry be maintained at 8-10, can stir evenly, then
Hydrochloric acid spare in step (1) is added in be adjusted to neutrality, and be kept stirring 1-3 it is small when, make aluminium salt complete hydrolysis；Wherein, with
A12O3The addition for counting water-soluble aluminum salt is the 1-6% of titanium dioxide powder weight, obtains slurry；
(6), slurries obtained by step (5) filtered, washed, gained filter cake drying, grinding obtain the titanium white of surface modification
Powder particles；
(7), the organic matter of titanium dioxide granular mass 0.2-1.5wt% is added in into titanium white powder particles obtained by step (6), in 40-
30-100min is stirred at 70 DEG C, obtains Titanium dioxide slurry；
(8), Titanium dioxide slurry obtained by step (7) is filtered, washes, dried at 100-130 DEG C, through crush to get to
Inorganic and organic coated titanium dioxide；
It, will be described thick after chlorinated exhaust specifically is obtained the hydrochloric acid solution that mass concentration is 20% by washing in step (1)
Hydrochloric acid solution carries out preliminary sedimentation into first deep gouge, and supernatant enters hydrochloric acid storage tank；Bottom underflow in first deep gouge is into once
Membrane filtration system filters TiOCl therein2, filtrate hydrochloric acid enters hydrochloric acid storage tank；As the TiOCl of membrane filtration system filtering2Reach
During limit, backwash operation is carried out, with water by TiOCl2It sweeps away, filter membrane enters next filter cycle；When being rinsed with water TiOCl2
When, TiOCl2It reacts with water, generates TiO2And HCl, HCl are dissolved in water and form hydrochloric acid solution；Contain TiO2The hydrochloric acid of solid is molten
Liquid enters secondary membrane filtration system, filters TiO therein2, filtrate hydrochloric acid enters hydrochloric acid storage tank；Then hydrochloric acid storage tank is collected
It is 5%~10% that hydrochloric acid is diluted to mass concentration with pure water, spare.
2. the method that a kind of chlorination by-product hydrochloric acid according to claim 1 is used for titanium dioxide coating, it is characterised in that：Step
(3) one or more of the zirconates in zirconium sulfate, zirconium oxychloride, zirconium chloride described in.
3. the method that a kind of chlorination by-product hydrochloric acid according to claim 1 is used for titanium dioxide coating, it is characterised in that：Step
(4) water soluble silicon compound described in is selected from one or both of sodium metasilicate, sodium metasilicate.
4. the method that a kind of chlorination by-product hydrochloric acid according to claim 1 is used for titanium dioxide coating, it is characterised in that：Step
(5) one or more of the water-soluble aluminum salt in aluminum sulfate, aluminium chloride, sodium metaaluminate described in.
5. the method that a kind of chlorination by-product hydrochloric acid according to claim 1 is used for titanium dioxide coating, it is characterised in that：Step
(7) organic matter described in be selected from trimethylolpropane, trimethylolethane, triethanolamine, neopentyl glycol, silicone oil etc. it is a kind of or
It is a variety of.
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| CN105419403A (en) * | 2015-11-23 | 2016-03-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Method of applying chloridized waste acid to titanium dioxide film coating |
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| US4623396A (en) * | 1983-09-14 | 1986-11-18 | Shiseido Company Ltd. | Titanium-mica composite material |
| CN101255288A (en) * | 2007-11-29 | 2008-09-03 | 江苏河海纳米科技股份有限公司 | Nano titanium oxide inorganic surface treatment method |
| CN101880479A (en) * | 2010-06-25 | 2010-11-10 | 宁波新福钛白粉有限公司 | Method for producing special rutile type titanium white powder for power coating |
| CN103555001A (en) * | 2013-10-31 | 2014-02-05 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for coating titanium dioxide |
| CN105419403A (en) * | 2015-11-23 | 2016-03-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Method of applying chloridized waste acid to titanium dioxide film coating |
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