CN109205669A - The combined preparation process of zirconium chloride and ocratation - Google Patents
The combined preparation process of zirconium chloride and ocratation Download PDFInfo
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- CN109205669A CN109205669A CN201811375200.XA CN201811375200A CN109205669A CN 109205669 A CN109205669 A CN 109205669A CN 201811375200 A CN201811375200 A CN 201811375200A CN 109205669 A CN109205669 A CN 109205669A
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- zircon sand
- desiccant
- gas
- ocratation
- zirconium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/04—Halides
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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
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10705—Tetrafluoride
Abstract
The invention discloses a kind of zirconium chloride and the combined preparation process of ocratation, method includes the following steps: zircon sand is mixed with desiccant, to being passed through hydrogen fluoride in the mixture of zircon sand and desiccant, heating, silica and hydrogen fluoride reaction in zircon sand generate silicon tetrafluoride gas, the mixture and gas gas-phase objects of the zircon sand and desiccant that are purified, gas gas-phase objects include ocratation；The mixture of the zircon sand of purification and desiccant is subjected to separating-purifying, the zircon sand purified；The zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, generates zirconium chloride.Above-mentioned preparation method realizes the purification of zircon sand using the silica component in zircon sand with hydrogen fluoride gas, zirconium chloride is prepared, by-product ocratation simultaneously, realize that zirconium, element silicon make full use of, zirconium oxide purity greatly promotes in zircon sand after purification, impurity content reduces, and improves subsequent chlorination reaction efficiency, reduces the separating difficulty of zirconium chloride.
Description
Technical field
The invention belongs to zirconium oxide production technical fields, and in particular to a kind of preparation of the joint of zirconium chloride and ocratation
Method.
Background technique
Zirconium dioxide (ZrO2) it is a kind of important ceramic material, there is the superior function such as high temperature resistant, wear-resistant, corrosion-resistant
Can, other than being applied to refractory material and ceramic paint, have become the main of electronic ceramics, function ceramics and synthetic cut stone
Raw material, in high-tech area using increasingly extensive.
The production method of zirconium oxide industrially applied at present mainly has electric smelting method, alkali fusion and three kinds of chloridising.Electric smelting
Method process flow is simple, but the zirconium oxide product quality prepared is lower；The product quality of alkali fusion preparation is higher, still
Production technology is complicated, and " three wastes " problem is serious；Fluidizing chlorination method is the current production ideal technique of zirconium oxide, has product quality
The advantages that height, production cost is low, and raw material availability is high.The key technology of chlorination process is the synthesis of zirconium chloride, existing
Reaction four chlorinations of preparation are carried out in fluidized-bed reactor using the mixture of zircon sand, reducing agent and chemical concurrent heating agent in technology
Zirconium, wherein reducing agent includes charcoal, petroleum coke, coal dust etc., and chemical concurrent heating agent includes silicon powder, ferrosilicon, silicon carbide etc..But it is existing
The yield for having the chloridising in technology to prepare silicon tetrachloride is lower.
Summary of the invention
The technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide zirconium chloride and
The combined preparation process of ocratation, this method have prepared zirconium chloride, while by-product ocratation.
Solve the joint that technical solution used by present invention problem is to provide a kind of zirconium chloride and ocratation
Preparation method, comprising the following steps:
Zircon sand is mixed with desiccant, to hydrogen fluoride is passed through in the mixture of zircon sand and desiccant, is heated, zircon sand
In silica and hydrogen fluoride reaction generate silicon tetrafluoride gas, the mixture of the zircon sand and desiccant that are purified and
Gas gas-phase objects, gas gas-phase objects include ocratation；
The mixture of the zircon sand of purification and desiccant is subjected to separating-purifying, the zircon sand purified；
The zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, generates zirconium chloride.
Preferably, zircon sand includes: 92-96mas%ZrSiO4, 1-2mas%HfSiO4, 1-2mas%SiO2, 1-
2mas%Al2O3, 0-1mas%Fe2O3, 0-1mas%TiO2, 0-0.1mas%UO2, 0-0.1mas%ThO2, 0-0.1mas%
CaO, 0-0.5mas%Y2O3, remainder is other impurity.
Preferably, zircon sand includes: 92-96mas%ZrSiO4, 1-2mas%HfSiO4, 1-2mas%SiO2, 1-
2mas%Al2O3, 0.5-1mas%Fe2O3, 0.5-1mas%TiO2, 0.001-0.1mas%UO2, 0.001-0.1mas%
ThO2, 0.001-0.1mas%CaO, 0.001-0.5mas%Y2O3, remainder is other impurity.
Preferably, desiccant is solid or liquid.
Preferably, solid drier is active carbon；Liquid drier is the concentrated sulfuric acid, the concentration of the concentrated sulfuric acid is 70~
98wt%.
Preferably, desiccant is solid, and desiccant is different from the partial size of zircon sand, by the method for screening by purification
Zircon sand is separated with desiccant；
Desiccant is liquid, is separated the zircon sand of purification with desiccant by method either in filtering, being centrifuged.
Preferably, desiccant is solid, and the partial size of zircon sand is 100~200 mesh, and the partial size of desiccant is 1~3mm.
Preferably, the combined preparation process of the zirconium chloride and ocratation, the desiccant of zircon sand and solid
Weight ratio be 1:(0.2~1), alternatively, the weight ratio of the desiccant of zircon sand and liquid be 1:(1~3).
Preferably, gas gas-phase objects further include hydrogen fluoride, and the preparation method is further comprising the steps of: gas gas-phase objects being passed through dry
Dry, compression, condensation, remove hydrogen fluoride, obtain tetrafluoride silicon liquid.
Preferably, by gas gas-phase objects by the way that in dry, compression, condensing steps, the pressure of compression is 2.0~3.0MPa, cold
Solidifying temperature is -30~-40 DEG C.
Preferably, the heating temperature of the silica in zircon sand and hydrogen fluoride reaction is 30~70 DEG C.
Preferably, the molar ratio of the zircon sand of purification and reaction raw materials active carbon is 1:(4~5).
Preferably, the zircon sand of purification and chlorine reaction temperature are 1100~1200 DEG C.
The combined preparation process of zirconium chloride and ocratation in the present invention has following remarkable result:
Using the purification of silica component and hydrogen fluoride gas realization zircon sand in zircon sand, four chlorinations have been prepared
Zirconium, while by-product ocratation, realize zirconium, element silicon makes full use of, and zirconium oxide purity is significantly in the zircon sand after purification
It is promoted, impurity content reduces, and improves subsequent chlorination reaction efficiency, reduces the separating difficulty of zirconium chloride.
Detailed description of the invention
Fig. 1 is the flow chart of the combined preparation process of the zirconium chloride and ocratation in the embodiment of the present invention 2；
Fig. 2 is the flow chart of the combined preparation process of the zirconium chloride and ocratation in the embodiment of the present invention 5.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing and specific embodiment party
Present invention is further described in detail for formula.
The embodiment of this patent is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, and is only used for explaining this patent, and cannot be understood as a limitation of this patent.
Embodiment 1
The present embodiment provides a kind of zirconium chloride and the combined preparation process of ocratation, comprising the following steps:
Zircon sand is mixed with desiccant, to hydrogen fluoride is passed through in the mixture of zircon sand and desiccant, is heated, zircon sand
In silica and hydrogen fluoride reaction generate silicon tetrafluoride gas, the mixture of the zircon sand and desiccant that are purified and
Gas gas-phase objects, gas gas-phase objects include ocratation；
The mixture of the zircon sand of purification and desiccant is subjected to separating-purifying, the zircon sand purified；
The zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, generates zirconium chloride.
The combined preparation process of zirconium chloride and ocratation in the present embodiment has following remarkable result: utilizing zirconium
Silica component and hydrogen fluoride gas in sand realize the purification of zircon sand, have prepared zirconium chloride, while by-product four
Silicon fluoride, realizes zirconium, element silicon makes full use of, and zirconium oxide purity greatly promotes in the zircon sand after purification, impurity content
It reduces, improves subsequent chlorination reaction efficiency, reduce the separating difficulty of zirconium chloride.
Embodiment 2
As shown in Figure 1, the present embodiment provides a kind of zirconium chloride and the combined preparation process of ocratation, including following step
It is rapid:
It 1) is that 1mm active carbon desiccant mixes with partial size by the zircon sand for the 183kg that partial size is 100 mesh, zircon sand and work
Property charcoal desiccant weight ratio be 1:1, be passed through hydrogen fluoride into the mixture of zircon sand and active carbon desiccant, heating temperature is
50 DEG C, under normal pressure, silica and hydrogen fluoride in zircon sand occur fluorination reaction and generate silicon tetrafluoride gas and water, and water generates
It is absorbed afterwards by active carbon desiccant rapidly, the solid-phase mixture and gas phase of the zircon sand and active carbon desiccant that are purified
Object, gas gas-phase objects include ocratation, and gas gas-phase objects further include hydrogen fluoride.
Specifically, zircon sand includes: 92-96mas%ZrSiO in the present embodiment4, 1-2mas%HfSiO4, 1-2mas%
SiO2, 1-2mas%Al2O3, 0-1mas%Fe2O3, 0-1mas%TiO2, 0-0.1mas%UO2, 0-0.1mas%ThO2, 0-
0.1mas%CaO, 0-0.5mas%Y2O3, remainder is other impurity.
2) by gas gas-phase objects by the way that a small amount of moisture for removing and carrying in gas gas-phase objects is dried in anhydrous calcium chloride drier,
Gas gas-phase objects after drying enter compressor compresses to 2.5MPa, and compressed gas enters freon cooler and is cooled to -40 DEG C,
Hydrogen fluoride is removed, tetrafluoride silicon liquid is obtained, wherein the ocratation being collected into is 103kg；
3) by the mixture of the zircon sand of purification and active carbon desiccant, separating-purifying is carried out by the method for screening, is obtained
To the zircon sand of purification, and the active carbon desiccant for being adsorbed with moisture separated；Active carbon desiccant is heated to 120
DEG C, while it being passed through nitrogen purging, realize the regeneration of active carbon desiccant.
4) chlorination reaction being occurred into for the zircon sand of purification and chlorine, reaction raw materials active carbon, reaction temperature is 1100 DEG C,
In, the zircon sand of purification and the molar ratio of reaction raw materials active carbon are 1:5, generate zirconium chloride, wherein four chlorinations being collected into
Zirconium is 218kg.
The combined preparation process of zirconium chloride and ocratation in the present embodiment has following remarkable result: utilizing zirconium
Silica component and hydrogen fluoride gas in sand realize the purification of zircon sand, have prepared zirconium chloride, while by-product four
Silicon fluoride, realizes zirconium, element silicon makes full use of, and zirconium oxide purity greatly promotes in the zircon sand after purification, impurity content
It reduces, improves subsequent chlorination reaction efficiency, reduce the separating difficulty of zirconium chloride.
Embodiment 3
The present embodiment provides a kind of zirconium chloride and the combined preparation process of ocratation, comprising the following steps:
It 1) is that 2mm active carbon desiccant mixes with partial size by the zircon sand for the 183kg that partial size is 200 mesh, zircon sand and work
Property charcoal desiccant weight ratio be 1:0.2, be passed through hydrogen fluoride into the mixture of zircon sand and active carbon desiccant, heating temperature
It is 30 DEG C, under normal pressure, the silica in zircon sand and hydrogen fluoride reaction generate silicon tetrafluoride gas and water, and water is rapid after generating
It is absorbed by active carbon desiccant, the mixture and gas gas-phase objects of the zircon sand and active carbon desiccant that are purified, gas gas-phase objects packet
Ocratation is included, gas gas-phase objects further include hydrogen fluoride；
Specifically, zircon sand includes: 92-96mas%ZrSiO in the present embodiment4, 1-2mas%HfSiO4, 1-2mas%
SiO2, 1-2mas%Al2O3, 0.5-1mas%Fe2O3, 0.5-1mas%TiO2, 0.001-0.1mas%UO2, 0.001-
0.1mas%ThO2, 0.001-0.1mas%CaO, 0.001-0.5mas%Y2O3, remainder is other impurity.
2) by gas gas-phase objects by the way that a small amount of moisture for removing and carrying in gas gas-phase objects is dried in anhydrous calcium chloride drier,
Gas gas-phase objects after drying enter compressor compresses to 2.0MPa, and compressed gas enters freon cooler and is cooled to -35 DEG C,
Hydrogen fluoride is removed, tetrafluoride silicon liquid is obtained, wherein the ocratation being collected into is 79kg；
3) by the mixture of the zircon sand of purification and active carbon desiccant, separating-purifying is carried out by the method for screening, is obtained
To the zircon sand of purification, and the active carbon desiccant for being adsorbed with moisture separated；Active carbon desiccant is heated to 120
DEG C, while it being passed through nitrogen purging, realize the regeneration of active carbon desiccant.
4) zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, reaction temperature is 1200 DEG C, wherein purification
Zircon sand and the molar ratio of reaction raw materials active carbon be 1:4, generate zirconium chloride, wherein the zirconium chloride being collected into is
200kg。
The combined preparation process of zirconium chloride and ocratation in the present embodiment has following remarkable result: utilizing zirconium
Silica component and hydrogen fluoride gas in sand realize the purification of zircon sand, have prepared zirconium chloride, while by-product four
The yield of silicon fluoride, silicon tetrachloride is high, and the utilization rate of zircon sand improves.
Embodiment 4
The present embodiment provides a kind of zirconium chloride and the combined preparation process of ocratation, comprising the following steps:
It 1) is that 3mm active carbon desiccant mixes with partial size by the zircon sand for the 183kg that partial size is 150 mesh, zircon sand and work
Property charcoal desiccant weight ratio be 1:0.6, be passed through hydrogen fluoride into the mixture of zircon sand and active carbon desiccant, heating temperature
It is 70 DEG C, under normal pressure, the silica in zircon sand and hydrogen fluoride reaction generate silicon tetrafluoride gas and water, and water is rapid after generating
It is absorbed by active carbon desiccant, the mixture and gas gas-phase objects of the zircon sand and active carbon desiccant that are purified, gas gas-phase objects packet
Ocratation is included, gas gas-phase objects further include hydrogen fluoride.
Specifically, zircon sand includes: 92-96mas%ZrSiO in the present embodiment4, 1-2mas%HfSiO4, 1-2mas%
SiO2, 1-2mas%Al2O3, 0-1mas%Fe2O3, 0-1mas%TiO2, 0-0.1mas%UO2, 0-0.1mas%ThO2, 0-
0.1mas%CaO, 0-0.5mas%Y2O3, remainder is other impurity.
2) by gas gas-phase objects by the way that a small amount of moisture for removing and carrying in gas gas-phase objects is dried in anhydrous calcium chloride drier,
Gas gas-phase objects after drying enter compressor compresses to 3.0MPa, and compressed gas enters freon cooler and is cooled to -30 DEG C,
Hydrogen fluoride is removed, tetrafluoride silicon liquid is obtained, wherein the ocratation being collected into is 92kg；
3) by the mixture of the zircon sand of purification and active carbon desiccant, separating-purifying is carried out by the method for screening, is obtained
To the zircon sand of purification, and the active carbon desiccant for being adsorbed with moisture separated；Active carbon desiccant is heated to 120
DEG C, while it being passed through nitrogen purging, realize the regeneration of active carbon desiccant.
4) zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, reaction temperature is 1150 DEG C, wherein purification
Zircon sand and the molar ratio of reaction raw materials active carbon be 1:4.5, generate zirconium chloride, wherein the zirconium chloride being collected into is
192kg。
The combined preparation process of zirconium chloride and ocratation in the present embodiment has following remarkable result: utilizing zirconium
Silica component and hydrogen fluoride gas in sand realize the purification of zircon sand, have prepared zirconium chloride, while by-product four
Silicon fluoride, realizes zirconium, element silicon makes full use of, and zirconium oxide purity greatly promotes in the zircon sand after purification, impurity content
It reduces, improves subsequent chlorination reaction efficiency, reduce the separating difficulty of zirconium chloride.
Embodiment 5
As shown in Fig. 2, the present embodiment provides a kind of zirconium chloride and the combined preparation process of ocratation, including following step
It is rapid:
1) by partial size be 200 mesh the zircon sand of 183kg mixed with the concentrated sulfuric acid desiccant of 98wt% concentration, zircon sand and
The weight ratio of concentrated sulfuric acid desiccant is 1:3, is passed through hydrogen fluoride, heating temperature into zircon sand and the mixture of concentrated sulfuric acid desiccant
It is 40 DEG C, under normal pressure, the silica in zircon sand and hydrogen fluoride occur fluorination reaction and generates silicon tetrafluoride gas and water, aquatic
It is absorbed by concentrated sulfuric acid desiccant rapidly at rear, the liquid-solid mixture and gas phase of the zircon sand and concentrated sulfuric acid desiccant that are purified
Object, gas gas-phase objects include ocratation, and gas gas-phase objects further include hydrogen fluoride.
Specifically, zircon sand includes: 92-96mas%ZrSiO in the present embodiment4, 1-2mas%HfSiO4, 1-2mas%
SiO2, 1-2mas%Al2O3, 0.5-1mas%Fe2O3, 0.5-1mas%TiO2, 0.001-0.1mas%UO2, 0.001-
0.1mas%ThO2, 0.001-0.1mas%CaO, 0.001-0.5mas%Y2O3, remainder is other impurity.
2) by gas gas-phase objects by the way that a small amount of moisture for removing and carrying in gas gas-phase objects is dried in anhydrous calcium chloride drier,
Gas gas-phase objects after drying enter compressor compresses to 3.0MPa, and compressed gas enters freon cooler and is cooled to -35 DEG C,
Hydrogen fluoride is removed, tetrafluoride silicon liquid is obtained, wherein the ocratation being collected into is 85kg；
3) by the liquid-solid mixture of the zircon sand of purification and concentrated sulfuric acid desiccant, separation is carried out by the method for filtering and is mentioned
Filter cake is washed to by zircon sand that is pure, being purified, the concentrated sulfuric acid waste liquid for being adsorbed with moisture for obtaining filter cake and separating
Property, it is dried to obtain the zircon sand of purification；Concentrated sulfuric acid waste liquid is improved concentration at least 90wt% by heating distillation；
4) chlorination reaction being occurred into for the zircon sand of purification and chlorine, reaction raw materials active carbon, reaction temperature is 1120 DEG C,
In, the zircon sand of purification and the molar ratio of reaction raw materials active carbon are 1:4.2, generate zirconium chloride, wherein the tetrachloro being collected into
Change zirconium is 199kg.
The combined preparation process of zirconium chloride and ocratation in the present embodiment has following remarkable result: utilizing zirconium
Silica component and hydrogen fluoride gas in sand realize the purification of zircon sand, have prepared zirconium chloride, while by-product four
The yield of silicon fluoride, silicon tetrachloride is high, and the utilization rate of zircon sand improves.
Embodiment 6
The present embodiment provides a kind of zirconium chloride and the combined preparation process of ocratation, comprising the following steps:
1) by partial size be 160 mesh the zircon sand of 183kg mixed with the concentrated sulfuric acid desiccant of 85wt% concentration, zircon sand and
The weight ratio of concentrated sulfuric acid desiccant is 1:1, is passed through hydrogen fluoride, heating temperature into zircon sand and the mixture of concentrated sulfuric acid desiccant
It is 60 DEG C, under normal pressure, the silica in zircon sand and hydrogen fluoride reaction generate silicon tetrafluoride gas and water, and water is rapid after generating
It is absorbed by concentrated sulfuric acid desiccant, the mixture and gas gas-phase objects of the zircon sand and concentrated sulfuric acid desiccant that are purified, gas gas-phase objects packet
Ocratation is included, gas gas-phase objects further include hydrogen fluoride.
Specifically, zircon sand includes: 92-96mas%ZrSiO in the present embodiment4, 1-2mas%HfSiO4, 1-2mas%
SiO2, 1-2mas%Al2O3, 0-1mas%Fe2O3, 0-1mas%TiO2, 0-0.1mas%UO2, 0-0.1mas%ThO2, 0-
0.1mas%CaO, 0-0.5mas%Y2O3, remainder is other impurity.
2) by gas gas-phase objects by the way that a small amount of moisture for removing and carrying in gas gas-phase objects is dried in anhydrous calcium chloride drier,
Gas gas-phase objects after drying enter compressor compresses to 2.5MPa, and compressed gas enters freon cooler and is cooled to -30 DEG C,
Hydrogen fluoride is removed, tetrafluoride silicon liquid is obtained, wherein the ocratation being collected into is 100kg；
3) by the liquid-solid mixture of the zircon sand of purification and concentrated sulfuric acid desiccant, separation is carried out by the method for filtering and is mentioned
Filter cake is washed to by zircon sand that is pure, being purified, the concentrated sulfuric acid waste liquid for being adsorbed with moisture for obtaining filter cake and separating
Property, it is dried to obtain the zircon sand of purification；Concentrated sulfuric acid waste liquid is improved concentration at least 90wt% by heating distillation；
4) zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, reaction temperature is 1160 DEG C, wherein purification
Zircon sand and the molar ratio of reaction raw materials active carbon be 1:4.7, generate zirconium chloride, wherein the zirconium chloride being collected into is
210kg。
Embodiment 7
The present embodiment provides a kind of zirconium chloride and the combined preparation process of ocratation, comprising the following steps:
1) by partial size be 100 mesh the zircon sand of 183kg mixed with the concentrated sulfuric acid desiccant of 70wt% concentration, zircon sand and
The weight ratio of concentrated sulfuric acid desiccant is 1:2, is passed through hydrogen fluoride, heating temperature into zircon sand and the mixture of concentrated sulfuric acid desiccant
It is 70 DEG C, under normal pressure, the silica in zircon sand and hydrogen fluoride reaction generate silicon tetrafluoride gas and water, and water is rapid after generating
It is absorbed by concentrated sulfuric acid desiccant, the mixture and gas gas-phase objects of the zircon sand and concentrated sulfuric acid desiccant that are purified, gas gas-phase objects packet
Ocratation is included, gas gas-phase objects further include hydrogen fluoride.
Specifically, zircon sand includes: 92-96mas%ZrSiO in the present embodiment4, 1-2mas%HfSiO4, 1-2mas%
SiO2, 1-2mas%Al2O3, 0.5-1mas%Fe2O3, 0.5-1mas%TiO2, 0.001-0.1mas%UO2, 0.001-
0.1mas%ThO2, 0.001-0.1mas%CaO, 0.001-0.5mas%Y2O3, remainder is other impurity.
2) by gas gas-phase objects by the way that a small amount of moisture for removing and carrying in gas gas-phase objects is dried in anhydrous calcium chloride drier,
Gas gas-phase objects after drying enter compressor compresses to 2.0MPa, and compressed gas enters freon cooler and is cooled to -40 DEG C,
Hydrogen fluoride is removed, tetrafluoride silicon liquid is obtained, wherein the ocratation being collected into is 95kg；
3) by the liquid-solid mixture of the zircon sand of purification and concentrated sulfuric acid desiccant, separation is carried out by the method for filtering and is mentioned
Filter cake is washed to by zircon sand that is pure, being purified, the concentrated sulfuric acid waste liquid for being adsorbed with moisture for obtaining filter cake and separating
Property, it is dried to obtain the zircon sand of purification；Concentrated sulfuric acid waste liquid is improved concentration at least 90wt% by heating distillation；
4) zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, reaction temperature is 1180 DEG C, wherein purification
Zircon sand and the molar ratio of reaction raw materials active carbon be 1:4, generate zirconium chloride, wherein the zirconium chloride being collected into is
215kg。
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (11)
1. the combined preparation process of a kind of zirconium chloride and ocratation, which comprises the following steps:
Zircon sand is mixed with desiccant, to hydrogen fluoride is passed through in the mixture of zircon sand and desiccant, is heated, in zircon sand
Silica and hydrogen fluoride reaction generate silicon tetrafluoride gas, the mixture and gas phase of the zircon sand and desiccant that are purified
Object, gas gas-phase objects include ocratation；
The mixture of the zircon sand of purification and desiccant is subjected to separating-purifying, the zircon sand purified；
The zircon sand of purification is reacted with chlorine, reaction raw materials active carbon, generates zirconium chloride.
2. the combined preparation process of zirconium chloride according to claim 1 and ocratation, which is characterized in that desiccant is
Solid or liquid.
3. the combined preparation process of zirconium chloride according to claim 2 and ocratation, which is characterized in that solid is dry
Agent is active carbon；Liquid drier is the concentrated sulfuric acid, and the concentration of the concentrated sulfuric acid is 70~98wt%.
4. the combined preparation process of zirconium chloride according to claim 2 or 3 and ocratation, which is characterized in that dry
Agent is solid, and desiccant is different from the partial size of zircon sand, is separated the zircon sand of purification with desiccant by the method for screening；
Desiccant is liquid, is separated the zircon sand of purification with desiccant by method either in filtering, being centrifuged.
5. the combined preparation process of zirconium chloride according to claim 4 and ocratation, which is characterized in that desiccant is
Solid, the partial size of zircon sand are 100~200 mesh, and the partial size of desiccant is 1~3mm.
6. the combined preparation process of zirconium chloride according to claim 2 or 3 and ocratation, which is characterized in that zirconium English
The weight ratio of the desiccant of sand and solid is 1:(0.2~1), alternatively, the weight ratio of the desiccant of zircon sand and liquid is 1:(1
~3).
7. the combined preparation process of zirconium chloride according to claim 1 and ocratation, which is characterized in that gas gas-phase objects are also
Including hydrogen fluoride, the preparation method is further comprising the steps of: by gas gas-phase objects by dry, compression, condensation, hydrogen fluoride is removed,
Obtain tetrafluoride silicon liquid.
8. the combined preparation process of zirconium chloride according to claim 7 and ocratation, which is characterized in that by gas gas-phase objects
By the way that in drying, compression, condensing steps, the pressure of compression is 2.0~3.0MPa, the temperature of condensation is -30~-40 DEG C.
9. according to claim 1~3, combined preparation process of zirconium chloride and ocratation described in 5,7,8 any one,
It is characterized in that, the heating temperature of silica and hydrogen fluoride reaction in zircon sand is 30~70 DEG C.
10. according to claim 1~3, combined preparation process of zirconium chloride described in 5,7,8 and ocratation, feature exist
In the zircon sand of purification and the molar ratio of reaction raw materials active carbon are 1:(4~5).
11. according to claim 1~3, combined preparation process of zirconium chloride described in 5,7,8 and ocratation, feature exist
In the zircon sand and chlorine reaction temperature of purification are 1100~1200 DEG C.
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