CN110256874A - The process of zirconium silicon compound adhesive cyst membrane coated red schorl type titanium dioxide - Google Patents
The process of zirconium silicon compound adhesive cyst membrane coated red schorl type titanium dioxide Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 25
- 206010011732 Cyst Diseases 0.000 title claims abstract description 10
- 208000031513 cyst Diseases 0.000 title claims abstract description 10
- 239000012528 membrane Substances 0.000 title claims abstract description 10
- IDIJOAIHTRIPRC-UHFFFAOYSA-J hexaaluminum;sodium;2,2,4,4,6,6,8,8,10,10,12,12-dodecaoxido-1,3,5,7,9,11-hexaoxa-2,4,6,8,10,12-hexasilacyclododecane;iron(2+);triborate;tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Fe+2].[Fe+2].[Fe+2].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-][Si]1([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O1 IDIJOAIHTRIPRC-UHFFFAOYSA-J 0.000 title claims abstract description 5
- 229910000246 schorl Inorganic materials 0.000 title claims abstract description 5
- UVGLBOPDEUYYCS-UHFFFAOYSA-N silicon zirconium Chemical compound [Si].[Zr] UVGLBOPDEUYYCS-UHFFFAOYSA-N 0.000 title claims description 7
- 239000000853 adhesive Substances 0.000 title claims description 5
- 230000001070 adhesive effect Effects 0.000 title claims description 5
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 58
- 239000002002 slurry Substances 0.000 claims abstract description 21
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 18
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims abstract 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims abstract 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims abstract 2
- 230000032683 aging Effects 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000011248 coating agent Substances 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 9
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- XIFFNSGJZPAYQJ-UHFFFAOYSA-N sulfuric acid;zirconium Chemical compound [Zr].OS(O)(=O)=O XIFFNSGJZPAYQJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 32
- 239000000377 silicon dioxide Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 8
- 239000002775 capsule Substances 0.000 abstract description 7
- 239000002270 dispersing agent Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000011241 protective layer Substances 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 abstract 1
- 230000002572 peristaltic effect Effects 0.000 description 17
- 238000013019 agitation Methods 0.000 description 10
- 239000011268 mixed slurry Substances 0.000 description 10
- 238000005253 cladding Methods 0.000 description 7
- 239000002131 composite material Substances 0.000 description 7
- 235000019832 sodium triphosphate Nutrition 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
- 238000000227 grinding Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- 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
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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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
- 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
- C09C3/063—Coating
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/40—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention belongs to coat titanium white production technical field, disclose the process of a clock zirconium silicate gel cyst membrane coated red schorl type titanium dioxide, the process conditions slurry concentration is 300g/L, sodium hexametaphosphate dispersant content is 0.1-0.5%, the wherein process conditions that zirconium oxide coats rutile type titanium white are as follows: bath temperature is 40-60 DEG C, zirconium oxide covering amount is 1-3wt%, reaction pH is 3-6, the process conditions that silica coats rutile type titanium white are as follows: bath temperature is 70-90 DEG C, silica covering amount is 1-2wt%, reaction pH is 8-10, zirconium oxide and silica form dense uniform complex capsule nanometer film in titanium dioxide surface.The present invention can make titanium dioxide particle surface coat compact zirconia/silica complex capsule nanometer film protective layer, to reduce titanium dioxide surface-active, increase titanium dioxide dispersibility, weatherability.
Description
Technical field
The invention belongs to coat titanium white production technical field, coated more particularly, to a kind of zirconium silicon compound adhesive cyst membrane
The process of rutile type titanium white.
Background technique
The features such as titanium dioxide is because of its chemical property stabilization and good whiteness, tinting strength, tinting power, covering power and heat resistance is wide
General is applied to the industries such as pigment such as coating, rubber, plastics, papermaking, while being also used as photochemical catalyst, photoelectric cell, ultraviolet light
Screener etc. is widely used.Not surface treated titanium dioxide surface is generally by polar group as (- OH) is coated, so titanium
White powder is easy to generate reunion because of polarity absorption or the moisture absorption, is difficult to disperse in other systems.Therefore titanium dioxide is coated
It is very important.With the high speed development of national economy, titanium dioxide demand also constantly rises.Though China's titanium dioxide production capacity is big
But product quality is not high, has a long way to go with the product of foreign well-known enterprise.So developing one kind is able to produce high quality titanium white powder
Method be very necessary.
There are many influence factor for being modified processing to titanium dioxide surface, such as the selection of covering, additional amount, addition are suitable
Sequence, addition speed, pH value, temperature, reaction time etc. all have a great impact to the property of powder.
At present in technology, in TiO2Surface easily forms island particles coat, cannot form continuous dense film, TiO2It is weather-proof
Property is poor, limits TiO2Application range, it is impossible to be used in the preparation of high-end product.
Summary of the invention
The purpose of the present invention is to provide a kind of titanium dioxide powders of surface cladding Zirconium oxide and Si oxide protective layer
Body, the titanium dioxide powder after making cladding have preferably dispersibility and weatherability.
The present invention is completed by following technical proposal:
A kind of process of zirconium silicon compound adhesive cyst membrane coated red schorl type titanium dioxide, comprising the following steps:
1) rutile type titanium white is taken, deionized water is added, constant volume forms slurries；
2) appropriate sodium tripolyphosphate solution is added into slurries, ultrasonic disperse obtains dispersion liquid；
3) under certain bath temperature, sulfuric acid zirconium solution and sodium hydroxide solution is added simultaneously to dispersion liquid, adjusts charging
Rate control pH value, is stirred to react；
4) after the completion of feeding, first time aging is carried out；
5) after aging, bath temperature and pH value are adjusted；Under the bath temperature, sodium metasilicate is added simultaneously to dispersion liquid
Solution and sulfuric acid solution adjust feed rate and keep pH value, be stirred to react；
6) after the completion of feeding, second of aging is carried out；Obtain the slurries that coating is completed；
7) slurries after gained coating are filtered, and wash filter cake；
8) gained filter cake is dried, and is ground, is obtained the rutile type titanium white of zirconium silicon compound coating；
In step 1), the concentration of the slurries is 300g/L；
In step 2), the additional amount of the sodium tripolyphosphate is the 0.1- of the mass ratio relative to rutile type titanium white
0.5%；
In step 2), the ultrasonic disperse time is 30min；
In step 3), the bath temperature is 40-60 DEG C；
In step 3), the pH value is 3-6；
In step 3), the zirconium sulfate additional amount is the 1-3% of titanium dioxide powder quality, charging according to the content of zirconium oxide
Time is 1h；
In step 4), the first time ageing time is 2h, is kept stirring rate, bath temperature, pH value in ageing process
It is constant；
In step 5), the bath temperature is 70-90 DEG C；The pH value is 8-10；
In step 5), the sodium metasilicate additional amount is the 1-2% of titanium dioxide powder quality, charging according to the content of silica
Time is 1h；
In step 6), second of ageing time is 2h, is kept stirring rate, bath temperature, pH value in ageing process
It is constant；
In step 7), the Washing of Filter Cake to neutrality；
In step 8), the drying carries out at 105 DEG C, and the time is for 24 hours.
The present invention has following advantages and effect:
Using the above scheme, dense uniform capsule shape Zirconium oxide/Si oxide can be coated in titanium dioxide particle surface to protect
Sheath increases titanium dioxide dispersibility and weatherability, surface functionalization improves TiO to reduce titanium dioxide surface-active2Using
Field.The method of the present invention is simple and easy, at low cost, pollution-free.
Detailed description of the invention
When attached drawing 1 is that projection Electronic Speculum amplifies 800,000 times, the TEM picture of uncoated sample.
Attached drawing 2 is projection Electronic Speculum when amplifying 800,000 times, and packet zirconium oxide pH is 3, covering amount 1%；Packet silica pH be 8,
The TEM picture that covering amount is 1%.
Attached drawing 3 is projection Electronic Speculum when amplifying 800,000 times, and packet zirconium oxide pH is 4, covering amount 2%；Packet silica pH be 9,
The TEM picture that covering amount is 1%.
Attached drawing 4 is projection Electronic Speculum when amplifying 800,000 times, and packet zirconium oxide pH is 6, covering amount 3%；Packet silica pH be 10,
The TEM picture that covering amount is 2%.
Attached drawing 5 is projection Electronic Speculum when amplifying 800,000 times, and packet zirconium oxide pH is 4, covering amount 2%；Packet silica pH is
9.5, the TEM picture that covering amount is 1%.
Attached drawing 6 is projection Electronic Speculum when amplifying 800,000 times, and packet zirconium oxide pH is 9, covering amount 2%；Packet silica pH is
9.5, the TEM picture that covering amount is 1%.
Attached drawing 7 is ultraviolet light 2 hours, and uncoated sample, different embodiment and comparative examples are to methylene blue solution
Photocatalytic activity comparison diagram.
Specific embodiment
Below with reference to example and Figure of description, the present invention is further described.
Embodiment 1
150g rutile type titanium white is taken, 500mL deionized water is added, is made into the slurries of 300g/L, 15mL concentration, which is added, is
The sodium tripolyphosphate solution of 10g/L makees dispersing agent, and suspension is made；Ultrasonic disperse 30min, obtains dispersion liquid；Move to 40 DEG C of perseverance
In warm water bath, pH to 3 is adjusted, under agitation, the zirconium sulfate coating agent that mass fraction is 10% is added with peristaltic pump, directly
ZrO into mixed slurry2Content is the 1% of titanium dioxide powder quality, and mass fraction is added with another peristaltic pump and is
10% NaOH solution, maintaining pH value is 3, and feed time controls after 1h or so, charging, keeps bath temperature and stirring
Rate aging 2h；80 DEG C are adjusted the temperature to again, and pH is adjusted to 8；Under agitation, mass fraction is added with peristaltic pump is 10%
Sodium metasilicate coating agent, until mixed slurry in SiO2Content is the 1% of titanium dioxide powder quality, and with another peristaltic pump
The H that mass fraction is 10% is added2SO4Solution, maintaining pH value is 8, and feed time controls after 1h or so, charging, is kept
Bath temperature and stirring rate aging 2h；Gained slurries are filtered, washing, drying, grinding, obtains sample.
Made sample analyzes its surface cladding situation through TEM, and the results are shown in attached figure 2.From Fig. 2 it can be found that at this
Under the conditions of embodiment, even compact zirconium oxide/silica composite nanometer film of capsule structure is formed in titanium dioxide particle surface, it is multiple
Close the thickness 3.0nm of nanometre glue cyst membrane, clad ratio 100%.
Embodiment 2
150g rutile type titanium white is taken, 500mL deionized water is added, is made into the slurries of 300g/L, 30mL concentration, which is added, is
The sodium tripolyphosphate solution of 10g/L makees dispersing agent, and suspension is made；Ultrasonic disperse 30min, obtains dispersion liquid；Move to 50 DEG C of perseverance
In warm water bath, pH to 4 is adjusted, under agitation, the zirconium sulfate coating agent of mass fraction 10% is added with peristaltic pump, until
ZrO in mixed slurry2Content is the 2% of titanium dioxide powder quality, and it is 10% that mass fraction, which is added, with another peristaltic pump
NaOH solution, maintaining pH value is 4, and feed time controls after 1h or so, charging, keeps bath temperature and stirring rate
Aging 2h；90 DEG C are adjusted the temperature to again, and pH is adjusted to 9；Under agitation, the silicon that mass fraction is 10% is added with peristaltic pump
Sour sodium coating agent, until the SiO in mixed slurry2Content is the 1% of titanium dioxide powder quality, and is added with another peristaltic pump
The H that mass fraction is 10%2SO4Solution, maintaining pH value is 9, and feed time controls after 1h or so, charging, keeps water-bath
Temperature and stirring rate aging 2h；Gained slurries are filtered, washing, drying, grinding, obtains sample.
Made sample analyzes its surface cladding situation through TEM, and the results are shown in attached figure 3.From Fig. 3 it can be found that at this
Under the conditions of embodiment, even compact zirconium oxide/silica composite nanometer film of capsule structure is formed in titanium dioxide particle surface, it is multiple
Close the thickness 3.6nm of nanometre glue cyst membrane, clad ratio 100%.
Embodiment 3
150g rutile type titanium white is taken, 500mL deionized water is added, is made into the slurries of 300g/L, 75mL concentration, which is added, is
The sodium tripolyphosphate solution of 10g/L makees dispersing agent, and suspension is made；Ultrasonic disperse 30min, obtains dispersion liquid；Move to 60 DEG C of perseverance
In warm water bath, pH to 6 is adjusted, under agitation, the zirconium sulfate coating agent that mass fraction is 10% is added with peristaltic pump, directly
ZrO into mixed slurry2Content is the 3% of titanium dioxide powder quality, and mass fraction is added with another peristaltic pump and is
10% NaOH solution, maintaining pH value is 6, and feed time controls after 1h or so, charging, keeps bath temperature and stirring
Rate aging 2h；70 DEG C are adjusted the temperature to again, and pH is adjusted to 10；Under agitation, mass fraction is added with peristaltic pump is
10% sodium metasilicate coating agent, until the SiO in mixed slurry2Content is the 2% of titanium dioxide powder quality, and compacted with another
The H that mass fraction is 10% is added in dynamic pump2SO4Solution, maintaining pH value is 10, and feed time is controlled in 1h or so, and charging finishes
Afterwards, bath temperature and stirring rate aging 2h are kept；Gained slurries are filtered, washing, drying, grinding, obtains sample.
Made sample analyzes its surface cladding situation through TEM, and the results are shown in attached figure 4.From Fig. 4 it can be found that at this
Under the conditions of embodiment, even compact zirconium oxide/silica composite nanometer film of capsule structure is formed in titanium dioxide particle surface, it is multiple
Close the thickness 4.7nm of nanometre glue cyst membrane, clad ratio 100%.
Embodiment 4
150g rutile type titanium white is taken, 500mL deionized water is added, is made into the slurries of 300g/L, 15mL concentration, which is added, is
The sodium tripolyphosphate solution of 10g/L makees dispersing agent, and suspension is made；Ultrasonic disperse 30min, obtains dispersion liquid；Move to 50 DEG C of perseverance
In warm water bath, pH to 4 is adjusted, under agitation, the zirconium sulfate coating agent that mass fraction is 10% is added with peristaltic pump, directly
ZrO into mixed slurry2Content is the 2% of titanium dioxide powder quality, and mass fraction is added with another peristaltic pump and is
10% NaOH solution, maintaining pH value is 4, and feed time controls after 1h or so, charging, keeps bath temperature and stirring
Rate aging 2h；80 DEG C are adjusted the temperature to again, and pH is adjusted to 9.5；Under agitation, mass fraction is added with peristaltic pump is
10% sodium metasilicate coating agent, until the SiO in mixed slurry2Content is the 1% of titanium dioxide powder quality, and compacted with another
The H that mass fraction is 10% is added in dynamic pump2SO4Solution, maintaining pH value is 9.5, and feed time is controlled in 1h or so, and charging finishes
Afterwards, bath temperature and stirring rate aging 2h are kept；Gained slurries are filtered, washing, drying, grinding, obtains sample.
Made sample analyzes its surface cladding situation through TEM, and the results are shown in attached figure 5.From Fig. 5 it can be found that at this
Under the conditions of embodiment, even compact zirconium oxide/silica composite nanometer film of capsule structure is formed in titanium dioxide particle surface, it is multiple
Close the thickness 3.7nm of nanometre glue cyst membrane, clad ratio 100%.
Comparative example 1
150g rutile type titanium white is taken, 500mL deionized water is added, is made into the slurries of 300g/L, 15mL concentration, which is added, is
The sodium tripolyphosphate solution of 10g/L makees dispersing agent, and suspension is made；Ultrasonic disperse 30min, obtains dispersion liquid；Move to 50 DEG C of perseverance
In warm water bath, pH to 9 is adjusted, under agitation, the zirconium sulfate coating agent that mass fraction is 10% is added with peristaltic pump, directly
ZrO into mixed slurry2Content is the 2% of titanium dioxide powder quality, and mass fraction is added with another peristaltic pump and is
10% NaOH solution, maintaining pH value is 9, and feed time controls after 1h or so, charging, keeps bath temperature and stirring
Rate aging 2h；80 DEG C are adjusted the temperature to again, and pH is adjusted to 9.5；Under agitation, mass fraction is added with peristaltic pump is
10% sodium metasilicate coating agent, until the SiO in mixed slurry2Content is the 1% of titanium dioxide powder quality, and compacted with another
The H that mass fraction is 10% is added in dynamic pump2SO4Solution, maintaining pH value is 9.5, and feed time is controlled in 1h or so, and charging finishes
Afterwards, bath temperature and stirring rate aging 2h are kept；Gained slurries are filtered, washing, drying, grinding, obtains sample.
Made sample analyzes its surface cladding situation through TEM, and the results are shown in attached figure 6.From Fig. 6 it can be found that at this
Under the conditions of embodiment, zirconium oxide/silica composite nanometer film of island structure, composite nanometer film are formed in titanium dioxide particle surface
Thickness 3.9nm, clad ratio 75%.
Embodiment 5
Photocatalytic activity experiment
Experimental method: the methylene blue solution for preparing 10mg/L is placed in glass beaker, is added a certain amount of by surface
The rutile type titanium white of coating forms the suspension of 50mg/L.It is placed under the xenon lamp of some strength and irradiates, and continue electromagnetism and stir
It mixes, 10mL is sampled after 2h, after being centrifuged, suspension supernatant liquor is taken to carry out ultraviolet specrophotometer measurement.Experimental result
See attached drawing 7.
From Fig. 7 it can be found that the degradation rate of Methylene Blue in Solution can be effectively reduced in the sample after coating, illustrate titanium dioxide
After surface coats zirconium oxide/silica composite nanometer film, photocatalytic activity is inhibited, to be conducive to improve its weather-proof
Property.
Claims (10)
1. the process of zirconium silicon compound adhesive cyst membrane coated red schorl type titanium dioxide, which comprises the following steps:
1) rutile type titanium white is taken, deionized water is added, constant volume forms slurries；
2) appropriate sodium hexametaphosphate solution is added into slurries, ultrasonic disperse obtains dispersion liquid；
3) under certain bath temperature, sulfuric acid zirconium solution and sodium hydroxide solution is added simultaneously to dispersion liquid, adjusts feed rate
PH value is controlled, is stirred to react；
4) after the completion of feeding, first time aging is carried out；
5) after aging, bath temperature and pH value are adjusted；Under the bath temperature, sodium silicate solution is added simultaneously to dispersion liquid
And sulfuric acid solution, it adjusts feed rate and keeps pH value, be stirred to react；
6) after the completion of feeding, second of aging is carried out；Obtain the slurries that coating is completed；
7) slurries after gained coating are filtered, and wash filter cake；
8) gained filter cake is dried, and is ground, is obtained the rutile type titanium white of zirconium silicon compound coating.
2. process according to claim 1, which is characterized in that in step 1), the concentration of the slurries is 300g/L.
3. process according to claim 1, which is characterized in that in step 2), the additional amount of the calgon
For the 0.1-0.5% of the mass ratio relative to rutile type titanium white；The ultrasonic disperse time is 30min.
4. process according to claim 1, which is characterized in that in step 3), the bath temperature is 40-60 DEG C；
PH value is 3-6；The zirconium sulfate additional amount is the 1-3% of titanium dioxide powder quality according to the content of zirconium oxide, and feed time is
1h。
5. process according to claim 1, which is characterized in that in step 4), the first time ageing time is 2h,
It is kept stirring rate in ageing process, bath temperature, pH value is constant.
6. process according to claim 1, which is characterized in that in step 5), the bath temperature is 70-90 DEG C；
The pH value is 8-10.
7. process according to claim 1, which is characterized in that in step 5), the sodium metasilicate additional amount is according to oxygen
The content of SiClx is the 1-2%, feed time 1h of titanium dioxide powder quality.
8. process according to claim 1, which is characterized in that in step 6), second of ageing time is 2h,
It is kept stirring rate in ageing process, bath temperature, pH value is constant.
9. process according to claim 1, which is characterized in that in step 7), the Washing of Filter Cake to neutrality.
10. process according to claim 1, which is characterized in that in step 8), the drying carries out at 105 DEG C,
Time is for 24 hours.
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