CN1839098A - Purification of finely divided, pyrogenically prepared metal oxide particles - Google Patents
Purification of finely divided, pyrogenically prepared metal oxide particles Download PDFInfo
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- CN1839098A CN1839098A CNA2004800238118A CN200480023811A CN1839098A CN 1839098 A CN1839098 A CN 1839098A CN A2004800238118 A CNA2004800238118 A CN A2004800238118A CN 200480023811 A CN200480023811 A CN 200480023811A CN 1839098 A CN1839098 A CN 1839098A
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- 239000002245 particle Substances 0.000 title claims abstract description 57
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 53
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 53
- 238000000746 purification Methods 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 37
- 230000005484 gravity Effects 0.000 claims abstract description 3
- 125000005843 halogen group Chemical group 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 230000002411 adverse Effects 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 2
- -1 halide compounds Chemical class 0.000 abstract description 3
- 150000004820 halides Chemical group 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 21
- 229910004298 SiO 2 Inorganic materials 0.000 description 18
- 230000008719 thickening Effects 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229960001866 silicon dioxide Drugs 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000001464 adherent effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910000039 hydrogen halide Inorganic materials 0.000 description 2
- 239000012433 hydrogen halide Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
- C01G23/075—Evacuation and cooling of the gaseous suspension containing the oxide; Desacidification and elimination of gases occluded in the separated oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Silicon Compounds (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Process for removing halide compounds adhering to finely divided metal oxide particles by means of steam, wherein the metal oxide particles are applied to the upper part of an upright column and migrate downwards by means of gravity, the steam is applied at the bottom end of the column, the metal oxide particles and the steam are fed counter-currently, the metal oxide particles freed of halide residues are removed at the base of the column, steam and halide residues are removed at the head of the column, wherein the column is heated in such a manner that the temperature difference Tbottom - Ttop between the lower part and the upper part of the column is at least 20 DEG C and a maximum temperature of 500 DEG C prevails in the column, and the metal oxide particles have a residence time in the column of from 1 second to 30 minutes.
Description
Technical field
The invention provides the halid method of removing on the metal oxide particle that adheres to pyrolysis preparation in small, broken bits.
Background technology
Knownly prepare metal oxide particle by flame hydrolysis or by flame oxidation.Be commonly called the metal oxide particle of pyrolysis preparation by the metal oxide particle of these method preparations.Usually, metal halide, especially muriate are used as raw material wherein.They are converted to metal oxide and haloid acid, normally spirit of salt under reaction conditions.When most of haloid acid left reaction process with the form of waste gas, remaining meeting adhered to metal oxide particle or direct and its bonding.In the deacidification step, may remove adherent haloid acid or pass through OH or OH from metal oxide particle by steam
2Replace the halogen atom of Direct Bonding to metal oxide.
DE 1150955 claimed a kind of methods, wherein deacidification is in thermopnore, temperature is to carry out under 450 ℃ to 800 ℃ in the presence of steam.In the method, metal oxide particle and steam can and stream or adverse current feeding, preferably with and flow to material.The high temperature that deacidification requires is a unfavorable factor to this method.
The purifying method of the claimed a kind of metal oxide particle in small, broken bits of GB-A-1197271, wherein metal oxide particle and steam or steam and air pass through post upstream in the mode that does not form fluidized-bed.Therefore the deacidification temperature that can lower the requirement is 400 ℃ to 600 ℃.Yet, found that these temperature remain a unfavorable factor to metal oxide particle.
The purifying method of the claimed a kind of pyrogenic silicon dioxide powder of EP-B-709340.In the method, the temperature of deacidification requirement only is 250 ℃ to 350 ℃.In the method, metal oxide particle and steam and stream ground from the bottom of right cylinder to its top feed.Speed is 1 to 10cm/s so that form fluidized-bed.Shift out the SiO 2 powder of purification at capital.Disadvantageously this method must be carried out with the form that fluidized-bed exists, and this has increased expense aspect control.In addition, the risk that always exists in the co-current process is that the SiO 2 powder and the spirit of salt that purify are moved out of at capital, and the silicon-dioxide of Jing Huaing may be polluted by spirit of salt like this.
Summary of the invention
The purpose of this invention is to provide the method for removing the halogenide residue from metal oxide particle, this method has been avoided the shortcoming of prior art.Especially this method condition is moderate and economical.
The invention provides by steam and remove the halid method that adheres on the metal oxide particle in small, broken bits, described metal oxide particle forms by containing the reaction of halid raw material by hydrolysis or oxidizing gas, wherein
-described the metal oxide particle in small, broken bits that contains the halogenide residue applies from the top of right cylinder and relies on gravity to move down with reactant gases,
-described steam randomly with air mixed, applies in the bottom of described post,
-described metal oxide particle in small, broken bits and the described steam counter-flow charging that contains the halogenide residue,
-the metal oxide particle of halide residue is not moved out of in the bottom of described post,
-steam and halogenide residue are moved out of at the top of described post,
Wherein, described method is characterised in that:
-described post is heated as follows, the bottom of described post and the temperature difference T on top
The bottom-T
The topAt least be 20 ℃, and the top temperature in the described post be to the maximum 500 ℃ and
The residence time of-described metal oxide particle in described post is 1 second to 30 minutes.
Embodiment
Halogenide within the scope of the present invention is hydrogen halide normally, especially spirit of salt.Halogenide comprises that also those covalently or ion ground or the halide atoms or the halide ions that link to each other with metal oxide particle by physical adsorption.
Contain normally corresponding metal muriate of halid raw material, as titanium tetrachloride, silicon tetrachloride or aluminum chloride.Yet, also can be organometallic compound, as the chlorine alkyl silane.
Within the scope of the present invention, metal oxide particle be understood that to obtain by flame hydrolysis or flame oxidation by the raw material of halide those.Metal oxide particle also can be understood that the nonmetal oxide particle.They are mixed oxides of silicon-dioxide, aluminum oxide, titanium dioxide, cerium oxide, zinc oxide, zirconium white, stannic oxide, bismuth oxide and above-claimed cpd.Metal oxide particle also comprises adulterated oxide particle, those as describing in DE-A-19650500.Metal oxide particle also can be understood that by flame hydrolysis and be encapsulated in the metal oxide particle that obtains in the housing, for example be encapsulated in the titanium dioxide granule in the silicon-dioxide, as described at DE 10260718.4 (December 23 2002 date of application).In above-mentioned oxide compound, silicon-dioxide, aluminum oxide and titanium dioxide are extremely important.
These particles are with form in small, broken bits.This is understood that they are 5 to 600m with the form of the aggregate of primary particle and the BET surface-area that has usually
2/ g.
Reactant gases is the reaction product of used gas and steam, forms preparing in the metal oxide particle by flame oxidation or flame hydrolysis.They can be hydrogen halide, steam, carbonic acid gas and unreacted gas.
The method according to this invention can preferably be carried out temperature difference T under following mode
The bottom-T
The topBe 20 ℃ to 150 ℃, especially preferably 50 ℃ to 100 ℃.
Temperature T
The bottomMeasurement be based on the whole height of reactor, carry out from the measurement point that is positioned at 10-15% more than the bottom of reactor.
Temperature T
The topMeasurement be based on the whole height of reactor, carry out from the measurement point that is positioned at 10-15% below the top of reactor.
The method according to this invention can preferably be carried out under following mode, and top temperature is 150 ℃ to 500 ℃.Usually preferred especially 350 ℃ to 450 ℃.
The residence time is preferably 5 seconds to 5 minutes, and the temperature that particulate matter flows in the post preferably can be from about 100 ℃ to 250 ℃.
The introducing amount of steam is preferably per hour every kilogram of metal oxide particle 0.0025 to 0.25kg steam, is preferably per hour every kilogram of metal oxide particle 0.025 to 0.1kg steam especially.Vapor temperature preferably is chosen as 100 ℃ to 500 ℃, wherein preferred especially 120 ℃ to 200 ℃.
If air is introduced in the post, proved that per hour every kilogram of metal oxide particle 0.005 is to 0.2m with steam
3The amount of air be favourable, particularly advantageous per hour is that every kilogram of metal oxide particle 0.01 is to 0.1m
3Air.
Present method can be carried out under following mode, and SiO 2 powder to be clean and steam randomly with air, form fluidized-bed.More advantageously, present method can be carried out with the form that does not form fluidized-bed.In this case, can reduce the expense of control, though the degree of purification that also can realize ideal at low temperatures, and the residence time is short relatively.Present method has also been avoided the emission problem of SiO 2 powder and steam and air, and this need relate in fluid process.When metal oxide particle after the column bottom is moved out of, if desired, they can be again by another post at least, top temperature wherein is no more than 500 ℃.This makes adherent halid content further be reduced.
Metal oxide particle and steam, and optional air can and flow or adverse current feeding.
Advantageously, described second and the post bottom that has of ensuing post and the temperature difference T between the top
The bottom-T
The topAt least it is 5 ℃.
Description of drawings
Fig. 1 is a synoptic diagram of describing present method.In Fig. 1: 1=metal oxide particle inlet; 2=steam and optional gas inlet; The outlet of 3=metal oxide particle; The 4=pneumatic outlet.
Embodiment
Embodiment 1 (according to the present invention)
Introduce the SiO 2 powder of 100kg/h (the BET surface-area is 200m on the top of right cylinder
2/ g) particle logistics, it has pH is 1.6, cl content is that 0.1 weight % and initial temperature are 190 ℃.Introduce the 5kg/h temperature in the bottom of post and be 120 ℃ steam and 4.5Nm
3The air of/h.Heat this post by internal heat, make the temperature T of the upper area of post
The topBe 350 ℃, the temperature T of the lower region of post
The bottomIt is 425 ℃.After leaving post (residence time: 10 seconds), the pH of SiO 2 powder is 4.2, and cl content is 0.0018 weight %, and thickening (thickening) is 3110mPas.
Embodiment 2 (Comparative Examples)
Similar to Example 1, be temperature T
The bottomBe 680 ℃ and T
The topIt is 670 ℃.
Embodiment 3 (Comparative Examples)
(the BET surface-area is 200m also to flow the SiO 2 powder of introducing 100kg/h in the right cylinder bottom
2/ g, pH are 1.6, and cl content is 0.1 weight %, and initial temperature is 190 ℃) the particle logistics, 5kg/h steam and 4.5Nm
3The air of/h.Heat this post by internal heat, make the temperature T of post upper area
The topBe 350 ℃, the temperature T of post lower region
The bottomIt is 425 ℃.After leaving post (residence time: 10 seconds), the pH of SiO 2 powder is 4.0, and cl content is 0.09 weight %, and thickening is 2850mPas.
Embodiment 4 (the present invention)
Similar to Example 1, (the BET surface-area is 99m to use alumina powder
2/ g, pH are 1.7, and cl content is 0.6 weight %, and initial temperature is 185 ℃) replace SiO 2 powder, and use 6kg/h temperature is 160 ℃ steam and 5Nm
3The air of/h (residence time: 150 seconds).
Embodiment 5 (the present invention)
Similar to Example 1, (the BET surface-area is 46m to use the titania powder of 200kg/h
2/ g, pH are 1.7, and cl content is 0.6 weight %, and initial temperature is 172 ℃) replace the SiO 2 powder of 100kg/h, and to use the 12kg/h temperature be 180 ℃ steam and 10Nm
3The air of/h (residence time: 85 seconds), T
The bottomIt is 400 ℃.
Embodiment 6 (the present invention)
In the bottom of right cylinder one controllable baffle plate is installed and is used to assemble SiO 2 powder.Introduce the SiO 2 powder of 100kg/h (the BET surface-area is 200m on post top
2/ g) particle logistics, its pH that has is 1.6, cl content is 0.1 weight %, and initial temperature is 190 ℃.Introduce the 5kg/h temperature in the bottom of post and be 120 ℃ steam and 4.5Nm
3The air of/h.Heat this post by internal heat, make the temperature T of post upper area
The topBe 350 ℃, the temperature T of post lower region
The bottomIt is 425 ℃.After leaving post (residence time: 10 minutes), the pH of SiO 2 powder is 4.3, and cl content is 0.0010 weight %, and thickening is 3070mPas.
Table: purify front/rear powder data analysis
| Embodiment | Powder | pH | Cl content [weight %] | Thickening [mPas] | ||
| Before | After | Before | After | After | ||
| 1 | SiO 2 | 1.6 | 4.2 | 0.1 | 0.0016 | 3110 |
| 2 | SiO 2 | 1.6 | 4.2 | 0.1 | 0.0018 | 2750 |
| 3 | SiO 2 | 1.6 | 4.0 | 0.1 | 0.04 | 2850 |
| 4 | Al 2O 3 | 1.7 | 4.1 | 0.6 | 0.08 | - |
| 5 | TiO 2 | 1.7 | 4.0 | 0.6 | 0.004 | - |
| 6 | SiO 2 | 1.6 | 4.3 | 0.1 | 0.001 | 3070 |
Embodiment 1,4 and 5 shows can remove adherent halogenide effectively by method of the present invention.
Although the contrast of embodiment 1 and 2 shows that higher temperature has adverse influence to thickening effect (thickeningeffect) owing to can purify the halogenide residue equally effectively among the higher temperature embodiment 2.Therefore, the thickening effect that the powder that obtains among the embodiment 1 shows is 3110mPas, and the powder of embodiment 2 only is 2750mPas.Embodiment 3 compares the removal that shows relatively poor halogenide residue with embodiment 1, and described powder shows relatively poor thickening effect.
Measure thickening effect according to following method: under 22 ℃ to the solution of the unsaturated vibrin of 142.5g in vinylbenzene (viscosity be 1300+/-100mPas) in adding 7.5g SiO 2 powder, by dissolver at 3000min
-1Under disperse.The example of suitable unsaturated polyester resin is Ludopal P6, BASF.In the dispersion of 60g, add the solution of the unsaturated vibrin of 90g in vinylbenzene again, the repeating dispersion operation.Thickening effect is 25 ℃ and uses rotational viscosimeter with 2.7s down
-1The viscosity number of representing with mPas of the dispersion measured of shearing rate.
Claims (10)
1. remove the halid method that adheres on the metal oxide particle in small, broken bits by steam, described metal oxide particle forms by containing the reaction of halid raw material by hydrolysis or oxidizing gas, wherein,
-described the metal oxide particle in small, broken bits that contains the halogenide residue applies from the top of right cylinder and relies on gravity to move down with reactant gases,
-described steam randomly with air mixed, applies in the bottom of described post,
-described metal oxide particle in small, broken bits that contains the halogenide residue and described steam counter-flow charging and
-the metal oxide particle of halide residue is not moved out of in the bottom of described post,
-steam and halogenide residue are moved out of at the top of described post,
Wherein, described method is characterised in that:
-described post is heated as follows, the bottom of described post and the temperature difference T on top
The bottom-T
The topAt least be 20 ℃, and the top temperature in the described post be to the maximum 500 ℃ and
The residence time of-described metal oxide particle in described post is 1 second to 30 minutes.
2. the method for claim 1 is characterized in that described temperature difference T
The bottom-T
The topIt is 20 ℃ to 150 ℃.
3. method as claimed in claim 1 or 2 is characterized in that the top temperature in the described post is 150 ℃ to 500 ℃.
4. as the described method of claim 1 to 3, it is characterized in that the described residence time is 5 seconds to 5 minutes.
5. as the described method of claim 1 to 4, it is characterized in that the temperature that the metal oxide particle in the logistics that enters described post has is about 100 ℃ to 500 ℃.
6. as the described method of claim 1 to 5, the introducing amount that it is characterized in that described steam is every kilogram of metal oxide particle 0.0025 to 0.25kg steam per hour.
7. as the described method of claim 1 to 6, it is characterized in that with the amount of the air of described vapor mixing for every kilogram of metal oxide particle 0.005 per hour to 0.2m
3Air.
8. as the described method of claim 1 to 7, it is characterized in that when described metal oxide particle after described column bottom is moved out of, they again by at least another wherein top temperature be no more than 500 ℃ post.
9. method as claimed in claim 8 is characterized in that described metal oxide particle and described steam also flow or adverse current feeding in described another post.
10. method as claimed in claim 8 or 9 is characterized in that described second and the post bottom that has of ensuing post and the temperature difference T between the top
The bottom-T
The topAt least it is 5 ℃.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10338219.4 | 2003-08-20 | ||
| DE10338219 | 2003-08-20 | ||
| DE10342827.5 | 2003-09-17 |
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| Publication Number | Publication Date |
|---|---|
| CN1839098A true CN1839098A (en) | 2006-09-27 |
| CN100447083C CN100447083C (en) | 2008-12-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004800238118A Expired - Lifetime CN100447083C (en) | 2003-08-20 | 2004-06-22 | Purification of finely divided, pyrogenically prepared metal oxide particles |
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| Country | Link |
|---|---|
| JP (1) | JP4778427B2 (en) |
| CN (1) | CN100447083C (en) |
| DE (1) | DE10342827A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109999734A (en) * | 2019-04-18 | 2019-07-12 | 山东大学 | A kind of apparatus and method reverse flow heat exchange and reacted |
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| JP5231195B2 (en) * | 2008-12-18 | 2013-07-10 | 東邦チタニウム株式会社 | Method for producing low halogen titanium oxide powder |
| WO2021121557A1 (en) | 2019-12-17 | 2021-06-24 | Wacker Chemie Ag | Fluidized-bed reactor for the control of the dwell time distribution in continuously operated fluidized beds |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1150955B (en) * | 1961-04-20 | 1963-07-04 | Degussa | Method and device for cleaning highly dispersed oxides |
| DE1642994A1 (en) * | 1967-01-21 | 1971-06-03 | Degussa | Process for cleaning finely divided oxides |
| JP3546494B2 (en) * | 1994-10-27 | 2004-07-28 | 信越化学工業株式会社 | Purification method of fine silica |
| DE19921059A1 (en) * | 1999-05-07 | 2000-11-16 | Heraeus Quarzglas | Process for cleaning Si0¶2¶ particles, device for carrying out the process, and grain produced by the process |
-
2003
- 2003-09-17 DE DE10342827A patent/DE10342827A1/en not_active Withdrawn
-
2004
- 2004-06-22 JP JP2006523536A patent/JP4778427B2/en not_active Expired - Lifetime
- 2004-06-22 CN CNB2004800238118A patent/CN100447083C/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109999734A (en) * | 2019-04-18 | 2019-07-12 | 山东大学 | A kind of apparatus and method reverse flow heat exchange and reacted |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4778427B2 (en) | 2011-09-21 |
| JP2007502766A (en) | 2007-02-15 |
| DE10342827A1 (en) | 2005-03-17 |
| CN100447083C (en) | 2008-12-31 |
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