CN104326508B - Nanometer grade antimony trioxide preparation method - Google Patents
Nanometer grade antimony trioxide preparation method Download PDFInfo
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- CN104326508B CN104326508B CN201410554499.0A CN201410554499A CN104326508B CN 104326508 B CN104326508 B CN 104326508B CN 201410554499 A CN201410554499 A CN 201410554499A CN 104326508 B CN104326508 B CN 104326508B
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- antimony
- thorax
- trioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
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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
- C01P2006/80—Compositional purity
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Abstract
The present invention discloses a kind of nanometer grade antimony trioxide preparation method, and stibium trioxide stove is heated up, metallic antimony imported in white stokehold thorax and is melted by step 1；Step 2：Rotary blower is opened at the top of the thorax of stibium trioxide stokehold, antimony voloxidation is made, antimony oxide oxygen furnace gas is formed；Step 3：To the top blower at middle thorax and bottom blower air blast, step 4：Antimony oxide furnace gas is imported in reative cell and is reacted；Step 5：Antimony oxide furnace gas is imported into double-deck crystallizer, after being cooled down after natural air cooled and ring-type cooling pipe, is crystallized on crystallization baffle plate, most after Jing bagrooms collect antimony oxide.
Description
Technical field
The present invention relates to a kind of method prepared by antimony oxide, particularly nanometer grade antimony trioxide preparation method.
Background technology
Prepared by nanometer grade antimony trioxide is important source material in Chemical Manufacture, its as fire retardant during chemistry reflection,
It is required that the antimony oxide will not only have higher purity, and do not contain four antimony oxides of high price, and it is also desirable to have compared with
High flame retardant effect.
In existing antimony oxide equipment, some devices for preparing antimony oxide are disclosed,
Some open source literatures report the method for preparing antimony oxide in recent years, for example：
1st, Chinese patent, application number：CN201210097320.4, the applying date：2012.04.05 title：Catalyst grade three
Two antimony preparation facilities are aoxidized, is made a summary：A kind of catalyst grade antimony oxide preparation facilities of the disclosure of the invention, including stibium trioxide stove and anti-
Answer device, it is characterised in that：Front thorax and breech that in described stibium trioxide stove, thorax is communicated with, front thorax and breech are respectively equipped with blowing
Pipe, described blower one end are stretched in thorax through stibium trioxide furnace wall, and the other end is arranged on outside stibium trioxide stove；Connect at the top of the breech
There is reactor, the reactor head is provided with crystallizer.Present configuration is simple, low manufacture cost, prepares three using the present invention
Aoxidize two antimony and only need to compressed air, be not required to adopt pure oxygen, although the invention discloses the oxidation of a kind of catalyst grade three two
Antimony preparation facilities, but with scientific and technological progress, the antimony oxide purity which is produced still does not reach the demand of market progress.
2nd, Chinese patent, application number：The CN200910114079 applyings date：2009.05.19 title：A kind of production catalysis
The method and its special antimony white stove of agent level antimony oxide, before and after the burner hearth of special antimony white stove, both sides are installed with by body of heater is oblique
Many blast pipes；Reactor is fixedly installed on other furnace roof on the left of body of heater；The invention needs additional expensive thermal source or pure
Oxygen, the high cost of production, production capacity are low, and equipment is complicated, and production process is easily lost, plant maintenance cycle is short.
This is accomplished by a kind of low manufacture cost, can quickly prepare the preparation method of nanometer grade antimony trioxide, to solve
Above-mentioned problem.
The content of the invention
It is an object of the invention to provide a kind of nanometer grade antimony trioxide preparation method, reaches improving product purity, increase
The purpose of product flame retardant effect.
The solution of the present invention is by being achieved in that：A kind of nanometer grade antimony trioxide preparation method, it is characterised in that
Comprise the following steps：
Step 1, stibium trioxide stove is heated up, and metallic antimony is imported in white stokehold thorax and is melted；
Step 2：Rotary blower is opened at the top of the thorax of stibium trioxide stokehold, antimony voloxidation is made, antimony oxide oxygen stove is formed
Gas；
Step 3：To the top blower at middle thorax and bottom blower air blast,
Step 4：Antimony oxide furnace gas is imported in reative cell and is reacted；
Step 5：Antimony oxide furnace gas is imported into double-deck crystallizer, is carried out after natural air cooled and ring-type cooling pipe
After cooling, crystallization baffle plate on crystallize, most after Jing bagrooms collect antimony oxide.
In the step 1, stibium trioxide furnace temperature rises to 1100 DEG C.
In the step 2, stibium trioxide stokehold thorax furnace temperature is maintained at 1300 DEG C.
In the step 5, the temperature control of crystallisation by cooling is at 50～490 DEG C.
In the step 2, when antimony oxidation liquid level is higher than stibium trioxide furnace bottom ventilation shaft, bottom ventilation ducts are opened and are carried out
Blowing, air quantity are 50～150m3/ h, increases antimony oxidation rate with this.
In the step 2, when antimony oxidation liquid level is less than stibium trioxide furnace bottom ventilation shaft, opens air blast lumen and blown
Wind, air quantity are 40～160m3/ h, increases antimony oxidation rate with this.
The blow rate required of the rotary blower is 70～180m3/ h.
In the step 4, at the middle thorax top blast wind be compressed air, pressure be 0.2～0.8MPa, flow be 80～
250m3/ h.
In the step 4, the bottom blower blowing is compressed air, and pressure is 0.3～0.5MPa, and flow is 200
～700m3/ h.
In step 5, double-deck crystalliser feet natural wind cooling window was closed once per 1 second；Blast ring-type cooling pipe left
The wind flow that the air quantity of air intake vent is is 100～500m3/ h, right inlet air one's intention as revealed in what one says air quantity are 80～480m3/ h.
The principle of the invention is as follows：Thorax, three conversion zones of middle thorax and breech before by arranging so that front thorax is receiving rotation
During air blast air blast, surface produces ripples slightly so that metallic antimony liquid energy is enough sufficiently volatilized with air contact, then passes through
The bottom blower of middle thorax is blown into wind in antimony liquid so that rolls inside metallic antimony, is fully reacted with oxygen, and top is blown
Airduct can with when antimony liquid surface obtain maximized volatilization.When antimony oxide is in stibium trioxide stove, by changing temperature, it is to avoid
The antimony oxide furnace gas cold air indoor with reaction contact, finally in double-deck crystallizer, is reacted, by natural wind with
The cooling wind that convection current wind with different wind directions is formed is crystallized to crystal, collects antimony oxide crystal.
The present invention has the advantages that：
1. high using the nanometer grade antimony trioxide purity collected of the present invention, grain fineness is high, principal component Sb2O3>
99.83%、As2O3/ %≤0.04, EG transmitances>99%th, Se/%≤0.003, b values are less than 0.97, PbO/%≤0.04；It is super
The average level of nanometer grade antimony trioxide is in the market gone out.
2. present configuration is simple, by the way of three cavitys, realizes that antimony oxide is produced, and simple structure conveniently makes
With.
3. the present invention can carry out air blast using air or oxygen.
4., in the present invention, using double-deck crystallizer, collection rate is high, and collecting effect is good.
Specific embodiment
Following embodiment describes this nanometer grade antimony trioxide preparation method.
Embodiment 1：
With 400g metallic antimonies as raw material, its chemical composition is：Sb 99.44%、AS 0.02%、Pb 0.21%、Fe
0.011%, other elements 0.00021%.Stibium trioxide stove furnace temperature is risen to into 1100 DEG C, metallic antimony is put into into the front thorax of stibium trioxide stove, is made
Thawing, the rotary blower of thorax before starting so that rotary blower starts air blast, the air blast blow rate required are 70m3/ h, then divide
Air is not blasted to top blower and bottom blower, it is 0.2MPa that the top blower blow rate required is pressure, and flow is 80
M3/ h, it is 0.3MPa that the bottom blower blow rate required is pressure, and flow is 200m3/ h, makes antimony voloxidation, forms three oxidations two
Antimony furnace gas；Subsequently furnace temperature is increased to after 1300 DEG C, then antimony oxide furnace gas is imported into reactor, when liquid level leads to higher than bottom
During wind pipeline height, open bottom ventilation ducts and blow, air quantity is 50m3/ h；When liquid level is less than air blast lumen height,
Bottom ventilation ducts are closed, air blast lumen is opened and is blown, air quantity is 40m3/ h.Finally high-temperature oxydation antimony furnace gas is imported
Crystallizer, is cooled down by ring-type cooling pipe, and the wind flow for blasting ring-type cooling pipe is 150m3/ h, during crystallisation by cooling
Temperature control imports double-deck crystallizer, through the nature of bottom at 50 degree or so when finally crystallizing, by antimony oxide furnace gas
Air-cooled, natural wind cooling window was closed once per 1 second；The wind flow that the air quantity for blasting the left air intake vent of ring-type cooling pipe is is
100m3/ h, right inlet air one's intention as revealed in what one says air quantity are 80m3/ h so that product is crystallized, and finally collecting the antimony oxide quality for obtaining is
470 grams.
Through detection, its composition is obtained as follows：
Detection obtains chemical composition：Principal component Sb2O3>99.83%、As2O3/ %≤0.04, EG transmitances>99%、Se/%≤
0.003rd, b values are less than 0.97, PbO/%≤0.04
Embodiment 2：
With 30 kilograms of metallic antimonies as raw material, its chemical composition is：Sb 99.71%、AS 0.067%、Pb 0.13%、Fe
0.010%, stibium trioxide stove furnace temperature is risen to into 1100 DEG C, metallic antimony is put into into the front thorax of stibium trioxide stove, is allowed to melt, thorax before starting
Rotary blower so that rotary blower starts air blast, the air blast blow rate required is 180m3/ h, then respectively to top blower and
Bottom blower blasts air, and it is 0.8MPa that the top blower blow rate required is pressure, and flow is 250m3/ h, bottom blower drum
It is 0.5MPa that air quantity is pressure, and flow is 700m3/ h, makes antimony voloxidation, forms antimony oxide furnace gas；Subsequently by furnace temperature
After being increased to 1300 DEG C, then antimony oxide furnace gas is imported into reactor, when liquid level is higher than bottom ventilation ducts height, opened
Bottom ventilation ducts blow, and air quantity is 150m3/ h；When liquid level is less than air blast lumen height, bottom ventilation ducts are closed
Road, opens air blast lumen and is blown, and air quantity is 160m3/ h.High-temperature oxydation antimony furnace gas is imported into crystallizer finally, by ring
Shape cooling pipe is cooled down, and the wind flow for blasting ring-type cooling pipe is 600m3/ h, during crystallisation by cooling, temperature control is 490
Degree left and right, when finally crystallizing, by antimony oxide furnace gas, imports double-deck crystallizer, through the natural air cooled of bottom, natural air cooled
But window was closed once per 1 second；The wind flow that the air quantity for blasting the left air intake vent of ring-type cooling pipe is is 500m3/ h, right inlet air
One's intention as revealed in what one says air quantity is 480m3/ h so that product is crystallized, it is 470 grams finally to collect the antimony oxide quality for obtaining.Finally collect
The antimony oxide quality for obtaining is 36.8 kilograms.
Its testing result is as follows：
Principal component Sb2O3>99.73%、As2O3/ %≤0.05, EG transmitances>98.1%th, Se/%≤0.002, b values are less than
0.96, PbO/%≤0.03.
Claims (7)
1. a kind of nanometer grade antimony trioxide preparation method, it is characterised in that comprise the following steps：
Step 1, stibium trioxide stove is heated up, and metallic antimony is imported in white stokehold thorax and is melted；
Step 2：Rotary blower is opened at the top of the thorax of stibium trioxide stokehold, antimony voloxidation is made, antimony oxide oxygen furnace gas is formed；
Step 3：To the top blower at middle thorax and bottom blower air blast,
Step 4：Antimony oxide furnace gas is imported in reative cell and is reacted；
Step 5：Antimony oxide furnace gas is imported into double-deck crystallizer, is cooled down after natural air cooled and ring-type cooling pipe
Afterwards, crystallization baffle plate on crystallize, most after Jing bagrooms collect antimony oxide,
In step 2, when antimony oxidation liquid level is higher than stibium trioxide furnace bottom ventilation shaft, bottom ventilation ducts are opened and are blown, wind
Measure as 50～150m3In/h, step 2, when antimony oxidation liquid level is less than stibium trioxide furnace bottom ventilation shaft, opening air blast lumen is carried out
Blowing, air quantity are 40～160m3/ h,
In step 3, at the middle thorax at the top of blowing for compressed air, pressure is 0.2～0.8MPa, and flow is 80～250m3/h。
2. nanometer grade antimony trioxide preparation method according to claim 1, it is characterised in that in the step 1, stibium trioxide
Furnace temperature rises to 1100 DEG C.
3. nanometer grade antimony trioxide preparation method according to claim 1, it is characterised in that in the step 2, stibium trioxide
Stokehold thorax furnace temperature maintains 1300 DEG C.
4. nanometer grade antimony trioxide preparation method according to claim 1, it is characterised in that in the step 5, cooling
The temperature control of crystallization is at 50～490 DEG C.
5. nanometer grade antimony trioxide preparation method according to claim 1, it is characterised in that the rotary blower
The blow rate required is 70～180m3/h。
6. nanometer grade antimony trioxide preparation method according to claim 5, it is characterised in that in step 3, bottom blowing
Pipe blowing is compressed air, and pressure is 0.3～0.5MPa, and flow is 200～700m3/h。
7. nanometer grade antimony trioxide preparation method according to claim 5, it is characterised in that in step 5, double-deck crystallization
Device bottom natural air cooling window was closed once per 1 second；The air quantity for blasting the left air intake vent of ring-type cooling pipe is 100～500m3/
H, right air intake vent air quantity are 80～480m3/h。
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| CN104326508B true CN104326508B (en) | 2017-03-29 |
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Inventor after: Ma Yusheng Inventor before: Lin Tianxiang |
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Effective date of registration: 20170308 Address after: 515100 Guangdong city of Shantou Province Feng Gao Chaoyang District Industrial Zone of peace Applicant after: Shantou Shuangpeng Plastic Industrial Co.,Ltd. Address before: 530003 the Guangxi Zhuang Autonomous Region Development Zone, Nanning, Yongxing Road, No. 16 Applicant before: GUANGXI GAOZHONG VALVE MANUFACTURING CO., LTD. |