CN100393921C - Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment - Google Patents
Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment Download PDFInfo
- Publication number
- CN100393921C CN100393921C CNB2006100189911A CN200610018991A CN100393921C CN 100393921 C CN100393921 C CN 100393921C CN B2006100189911 A CNB2006100189911 A CN B2006100189911A CN 200610018991 A CN200610018991 A CN 200610018991A CN 100393921 C CN100393921 C CN 100393921C
- Authority
- CN
- China
- Prior art keywords
- air
- antimony
- furnace gas
- antimonous oxide
- antimony trioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a method for producing single-crystal type antimony trioxide with uniformly distributed grain diameters, and a device thereof. The present invention is a method for smelting by adopting a reflection type antimony white stove. The method comprises the following process: after antimony is melted in the reflection type antimony white stove, the air is forced into a molten antimony liquid level in a furnace cavity so that the antimony is oxidized into an antimony trioxide furnace gas which is then cooled, crystallized, exhausted from a furnace gas outlet pipe and collected by a dust collecting system. The present invention is characterized in that after led out, the furnace gas oxidized into the antimony trioxide firstly passes through an air-cooled type reactor, subsequently, the furnace gas oxidized into the antimony trioxide is cooled through three levels and is crystallized in a crystallizer, then, the furnace gas oxidized into the antimony trioxide is exhausted from the furnace gas outlet pipe, and finally, single-crystal type high-grade antimony trioxide with uniformly distributed and unimodal particle diameters, the particle diameter of 0.2 to 3.5 mu m on average, 99.6 percent of a main constituent Sb2O3, less than 0.003 percent of 325 mesh sieve residues and more than 98.5 percent of whiteness is obtained. The method has the advantages of high productivity, low energy consumption, long furnace service life, high automation level, stable produce-operation control and high raw material adaptability. The present invention which can produce antimony trioxide products of different specifications has obvious economic benefit.
Description
Technical field
The present invention relates to a kind of pyrogenic process and produce the uniform antimonous oxide production method of method, particularly monocrystalline type, size distribution and the device thereof of antimonous oxide ultrafine powder.
Background technology
Antimonous oxide (stibium trioxide) is a kind of important chemical material, and it has been widely used on modern industries such as building, plastics, rubber, paint, chemical fibre as the synergistic agent of Organohalogen compounds fire retardant.Yet, along with progress of science and technology, development and national economy, industrial quality to antimonous oxide has proposed more requirements, especially monocrystalline type, the uniform antimonous oxide of size distribution, because having good chemically reactive, good dispersity, tinting strength evenly reaches characteristics such as light stability is strong, favored by high-end user, its price also antimonous oxide than run-of-the-mill is high more than 10%.
At present industrial to produce the process application of antimonous oxide with the autothermal oxidation volatilization method the most extensive, and it is to be raw material with the metallic antimony, by dissolve, processes such as voloxidation, crystallisation by cooling, control of dust obtain the antimonous oxide product.As publication number is that described cubic crystal form antimony trioxide production method of CN1173468A patent and device thereof are the stibium trioxide stoves that adopts reverberatory furnace structure, making insulating covering agent with the inorganic salt of sodium or potassium or ammonium or aluminium covers antimony liquid surface in the stove, and the furnace gas that makes the stibium trioxide stove enters a mixing chilling apparatus, with a large amount of cooling airs furnace gas is carried out horizontal quenching, make the antimonous oxide quench crystallization of furnace gas generate cubic crystal form antimony trioxide, it is bigger that this method has output, energy consumption is low, technology is simple, advantages such as good product quality.But the cubic content of its product only can reach more than 99%, and exist size distribution wide, and be irregular peak shape, fluctuation range is big, particle diameter is many greater than the foreign matter (stain) of 0.1 μ m, adaptability to raw material is poor, generally can only be difficult to satisfy high-end customer requirements with defectives such as high-purity antimony slab productions.
Summary of the invention
The objective of the invention is to utilize the stibium trioxide stove of reverberatory furnace structure, energy manufacture order crystal formation, the uniform antimonous oxide of size distribution after improving.
Monocrystalline type of the present invention, the uniform antimonous oxide production method of size distribution, it is the method that adopts reflective stibium trioxide stove to smelt, antimony reflective stibium trioxide stove through the fusing after, air is blasted fused antimony liquid level in the burner hearth, make antimony be oxidized to the antimonous oxide furnace gas, cooling then, crystallization, discharge from the furnace gas export pipe, the process that captures with dust collecting system again, its technical characterstic is: after the furnace gas that is oxidized to antimonous oxide is drawn, earlier through air-cooled reactor, then in crystallizer through three grades of coolings and crystallizations, discharge from the furnace gas export pipe then, capture with dust collecting system again and obtain monocrystalline type, the uniform antimonous oxide ultrafine powder of size distribution product.
Described monocrystalline type, the uniform antimonous oxide production method of size distribution, the air that is to blast reflective stibium trioxide stove antimony liquid is 200～520m
3/ h; The cooling air that enters crystallizer divides three grades, and wherein the one-level cooling air is an air, and flow is controlled with induced draft fan, and the cooling air of secondary and three grades is a pressurized air, and pressure is 0.4～0.6MPa.
For realizing this inventive method, the present invention includes the stibium trioxide stove of reverberatory furnace structure, the furnace gas export pipe, and dust collecting system, be characterized in air-cooled stainless steel barrel type reactor of stibium trioxide stove installation, do not establish the secondary blast pipe in the reactor, but blast air through the some airduct fused antimony liquid levels in burner hearth that are installed on the furnace wall, make antimony be oxidized to the antimonous oxide furnace gas, air-cooled reactor is installed in the furnace gas export place of burner hearth top, air-cooled reactor upper end is provided with vertical mold, and it is made of sleeve and three grades of cooling ducts, and vertical mold is the hydraucone shape.Enter vertical equipment of crystallisation by cooling by air-cooled stainless steel barrel type reactor, make the antimonous oxide quench crystallization in the furnace gas become monocrystalline type, the uniform antimonous oxide of size distribution.
The described airduct that is installed on the furnace wall is three to eight.
Advantage of the present invention:
1, the product that obtains of the present invention be monocrystalline type, size distribution evenly and be unimodal, median size 0.2～3.5 μ m, principal constituent Sb
2O
399.6%, 325 screen residues are less than 0.003%, whiteness is greater than 98.5% senior antimonous oxide, the antimonous oxide product that this method has that production capacity is big, energy consumption is low, furnace campaign is long, level of automation is high, production operation control stabilization, raw material adaptive faculty are strong, can produce different size has remarkable economic efficiency.
2, the described airduct that is installed on the furnace wall is three to eight, can make in the stibium trioxide stove everywhere that temperature keeps evenly, and fluctuation is not more than 50 ℃, and the reactor temperature field distribution is even.
3, the present invention does not need to add insulating covering agent, adopted the air-cooled reactor of original creation, the retainer wall temperature is at 200～400 ℃, cancellation secondary blast pipe, furnace accretion is few in the production process, produce stable, safety coefficient is big, reach work-ing life more than 1 year, production technique is simpler, and the raw material adaptive faculty is strong, than publication number is that described cubic crystal form antimony trioxide production method of CN1173468A patent and device output thereof are big more than 80%, cost is low by 30～40%, and quality is better and stable, and tangible economic benefit is arranged.
4, equipment of crystallisation by cooling of the present invention is annular hydraucone, can make the cooling air that enters crystallizer become monocrystalline type, the uniform antimonous oxide of size distribution with furnace gas uniform mixing and complete quench crystallization, strengthens cooling area, and cooling evenly.
Description of drawings
Accompanying drawing is the front view of the inventive method using appts.
Embodiment
The device that the inventive method is used below in conjunction with accompanying drawing is described further.
Adopt diesel oil, heavy oil, raw material (metallic antimony) in fuel such as the Sweet natural gas heating stibium trioxide stove 1, after making it fusing and remaining on 900～1000 ℃, air is blasted fused antimony liquid level through three to eight airducts 9 that are installed on the furnace wall, make antimony be oxidized to the antimonous oxide furnace gas, furnace gas enters vertical equipment of crystallisation by cooling 4 by air-cooled stainless steel barrel type reactor 2, reactor 2 has cooling air blast inlet 3, one-level cooling air 7 enters crystallizer and furnace gas uniform mixing from the circular clearance of reactor and crystallizer, furnace gas evenly is quickly cooled to below 500 ℃, and then two, tertiary compressed air cooling air 5,6 inject crystallizer 4 and effectively mix once more with furnace gas from being distributed in spray tube on the sleeve, eliminate the crystallization dead angle rapidly, make the complete quench crystallization of antimonous oxide in the furnace gas become monocrystalline type, the uniform antimonous oxide product of size distribution is through capturing in the bag collection system behind the oarse-grained antimonous oxide of cooling tower sedimentation.
During the uniform antimonous oxide production method of above monocrystalline type, size distribution, with common 6m
2The stibium trioxide stove, the air that blasts reflective stibium trioxide stove antimony liquid is 200～520m
3/ h; The cooling air that enters crystallizer divides three grades, and wherein the one-level cooling air is an air, and flow is the furnace gas flow with 0.5～10 times of induced draft fan control, and the cooling air of secondary and three grades is a pressurized air, and pressure is 0.4～0.6MPa, and flow is 100～800m
3/ h; The cooling air that enters reactor is 1000～2000m
3/ h.
Embodiment
Be embodiments of the invention below:
Example 1 is at 6m
2The stibium trioxide stove on, use four airduct 9 blast volume to be 200m
3/ h, the cooling air that enters crystallizer divides three grades, and wherein the one-level cooling air is an air, and flow is 2.5 times of furnace gas, and two, three grades of cooling airs are pressurized air, and pressure is 0.4～0.6MPa, and flow is 100m
3/ h; The cooling air that enters reactor is 1000m
3/ h collects monocrystalline type, the uniform antimonous oxide of size distribution at sack cleaner.With Sb content is that 98.65% No. two antimony slabs are raw material, 19.5 tons of daily output antimonous oxide products, and single cubic is more than 99.5%, size distribution is normal distribution and is unimodal, Fei Shi median size 0.90 μ m, and 325 screen residues are 0.002%, whiteness is 99.1, and Chemical Composition is Sb
2O
399.6%, Pb 0.06%, the senior antimonous oxide of As 0.035%.
Example 2 all the other conditions are identical with example 1, are 360m except using six roots of sensation airduct 9 blast volume
3/ h, the cooling air that enters crystallizer divides three grades, and wherein the one-level cooling air is an air, and flow is 2 times of furnace gas, and two, three grades of cooling airs are pressurized air, and pressure is 0.4～0.6MPa, and flow is 200m
3/ h; The cooling air that enters reactor is 1000m
3/ h.With Sb content is that 98.65% No. two antimony slabs are raw material, 22 tons of daily output antimonous oxide products, and single cubic is more than 99.6%, size distribution is normal distribution and is unimodal, Fei Shi median size 1.02 μ m, and 325 screen residues are 0.002%, from degree is 99.0, and Chemical Composition is Sb
2O
399.6%, Pb 0.065%, the senior antimonous oxide of As 0.04%.
Example 3 all the other conditions are identical with example 1, are 360m except using eight airduct 9 blast volume
3/ h, the cooling air that enters crystallizer divides three grades, and wherein the one-level cooling air is an air, and flow is 2 times of furnace gas, and two, three grades of cooling airs are pressurized air, and pressure is 0.4～0.6MPa, and flow is 200m
3/ h; The cooling air that enters reactor is 1000m
3/ h.With Sb content is that 98.65% No. two antimony slabs are raw material, 22 tons of daily output antimonous oxide products, and single cubic is more than 99.7%, size distribution is normal distribution and is unimodal, Fei Shi median size 1.02 μ m, and 325 screen residues are 0.002%, whiteness is 99.0, and Chemical Composition is Sb
2O
399.6%, Pb 0.065%, the senior antimonous oxide of As 0.04%.
Claims (3)
1. monocrystalline type, the uniform antimonous oxide production method of size distribution, it is the method that adopts reflective stibium trioxide stove to smelt, antimony reflective stibium trioxide stove through the fusing after, air is blasted in the burner hearth under the fused antimony liquid level, make antimony be oxidized to the antimonous oxide furnace gas, cooling then, crystallization, discharge from the furnace gas export pipe, the process that captures with dust collecting system again, it is characterized in that: after the furnace gas that is oxidized to antimonous oxide is drawn, earlier through air-cooled reactor, then in crystallizer through three grades of coolings and crystallizations, discharge from the furnace gas export pipe then, capture with dust collecting system again and obtain monocrystalline type, the uniform antimonous oxide ultrafine powder of size distribution product;
Above-mentioned processing condition are: the air that blasts reflective stibium trioxide stove antimony liquid is 200～520m
3/ h; The cooling air that enters crystallizer divides three grades, and wherein the one-level cooling air is an air, and flow is controlled with induced draft fan, and the cooling air of secondary and three grades is a pressurized air, and pressure is 0.4～0.6MPa.
2. a monocrystalline type as claimed in claim 1, the uniform antimonous oxide production of size distribution device, the stibium trioxide stove (1) that comprises reverberatory furnace structure, the furnace gas export pipe, and dust collecting system, it is characterized in that: some airducts (9) are installed in the furnace wall of stibium trioxide stove (1), the furnace gas export of burner hearth top is installed air-cooled reactor (2), air-cooled reactor (2) upper end is provided with vertical mold (4), it is made of sleeve and three grades of cooling ducts (5,6,7), and vertical mold (4) is the hydraucone shape.
3. the described monocrystalline type of claim 2, the uniform antimonous oxide production of size distribution device, the airduct that it is characterized in that being installed on the furnace wall is three to eight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100189911A CN100393921C (en) | 2006-04-27 | 2006-04-27 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100189911A CN100393921C (en) | 2006-04-27 | 2006-04-27 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1873061A CN1873061A (en) | 2006-12-06 |
| CN100393921C true CN100393921C (en) | 2008-06-11 |
Family
ID=37483654
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100189911A Active CN100393921C (en) | 2006-04-27 | 2006-04-27 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100393921C (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559980B (en) * | 2009-05-19 | 2012-12-05 | 广西日星金属化工有限公司 | Method for producing catalyst level antimony oxide and special antimony white furnace thereof |
| CN102616846B (en) * | 2012-04-05 | 2014-09-24 | 广西华锑科技有限公司 | Gas-phase cooling crystallization device for antimony white furnace |
| CN102616845B (en) * | 2012-04-05 | 2014-11-12 | 广西华锑科技有限公司 | Production device for large-particle-size antimony trioxide |
| CN102616847B (en) * | 2012-04-05 | 2014-03-26 | 广西华锑科技有限公司 | Method for preparing catalyst grade antimony trioxide |
| CN102602995B (en) * | 2012-04-05 | 2014-07-23 | 广西华锑科技有限公司 | Production method of large-particle-size antimonous oxide |
| CN102602996B (en) * | 2012-04-05 | 2014-03-26 | 广西华锑科技有限公司 | Preparation device for catalyst-grade antimonous oxide |
| CN104310472B (en) * | 2014-10-20 | 2017-05-17 | 汕头市超越织造有限公司 | Method for preparing antimonous oxide for polyester |
| CN106669301B (en) * | 2016-09-13 | 2022-06-07 | 沈阳隆基电磁科技股份有限公司 | Vacuum dust removal equipment for single crystal growth furnace |
| CN108609654A (en) * | 2018-08-17 | 2018-10-02 | 云南木利锑业有限公司 | Superfine antimony trioxide production technology |
| CN112678869B (en) * | 2020-12-25 | 2023-04-07 | 广东宇星阻燃新材股份有限公司 | Preparation method of spherical antimony trioxide |
| CN113322507B (en) * | 2021-05-31 | 2022-04-01 | 湖南娄底华星锑业有限公司 | Antimony trioxide powder crystal collecting pipe |
| CN113720867B (en) * | 2021-10-11 | 2024-01-30 | 昆明理工大学 | Method for preparing antimony trioxide standard sample of scanning electron microscope |
| CN113896239A (en) * | 2021-10-26 | 2022-01-07 | 北京普利宏斌化工材料有限责任公司 | Preparation method of novel antimony trioxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102489A (en) * | 1985-04-01 | 1987-01-17 | 锡矿山矿务局 | The method for preparing antimonous oxide (stibium trioxide) with metallic antimony |
| CN1172769A (en) * | 1997-01-29 | 1998-02-11 | 锡矿山矿务局 | Method for producing particle diantimony trioxide and its device |
| CN1173468A (en) * | 1997-01-29 | 1998-02-18 | 锡矿山矿务局 | Method and appts. for prodn. of cubic crystal form antimony trioxide |
| CN1354137A (en) * | 2000-11-17 | 2002-06-19 | 刘伯龙 | Method for producing antimony white and its special equipment |
-
2006
- 2006-04-27 CN CNB2006100189911A patent/CN100393921C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102489A (en) * | 1985-04-01 | 1987-01-17 | 锡矿山矿务局 | The method for preparing antimonous oxide (stibium trioxide) with metallic antimony |
| CN1172769A (en) * | 1997-01-29 | 1998-02-11 | 锡矿山矿务局 | Method for producing particle diantimony trioxide and its device |
| CN1173468A (en) * | 1997-01-29 | 1998-02-18 | 锡矿山矿务局 | Method and appts. for prodn. of cubic crystal form antimony trioxide |
| CN1354137A (en) * | 2000-11-17 | 2002-06-19 | 刘伯龙 | Method for producing antimony white and its special equipment |
Non-Patent Citations (6)
| Title |
|---|
| 三氧化二锑粒度的控制. 唐仕祥.湖南冶金，第4期. 1997 |
| 三氧化二锑粒度的控制. 唐仕祥.湖南有色金属，第14卷第5期. 1998 |
| 三氧化二锑粒度的控制. 唐仕祥.湖南冶金，第4期. 1997 * |
| 三氧化二锑粒度的控制. 唐仕祥.湖南有色金属，第14卷第5期. 1998 * |
| 超细微粒三氧化锑的生长方法及设备. 刘启勋等.湖南化工，第1期. 1991 |
| 超细微粒三氧化锑的生长方法及设备. 刘启勋等.湖南化工，第1期. 1991 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1873061A (en) | 2006-12-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100393921C (en) | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment | |
| US20150101257A1 (en) | Abrasive material for shot blasting, and method for producing same | |
| CN109734129B (en) | Method for producing refined zirconium tetrachloride and byproduct silicon tetrachloride by zirconium silicate ball-making boiling chlorination process | |
| TW201445004A (en) | Reactor for producing polycrystalline silicon and method for removing a silicon-containing deposit on a component of such a reactor | |
| CN109205628A (en) | A kind of preparation process of glass sand | |
| CN207347181U (en) | Rafifinal atomization explosion method prepares the device of high-purity alumina powder | |
| JPH0925137A (en) | High-strength rock wool and its production | |
| CN101260472A (en) | Method and system for separating dissimilar dust in stainless steel smelting process | |
| CN101906663B (en) | Blue ssuperindividual corundum and preparation method thereof | |
| CN102616847A (en) | Method for preparing catalyst grade antimony trioxide | |
| CN110156301B (en) | Continuous melting device and method for quartz tube production | |
| CN217568765U (en) | Reactor for producing silicon tetrachloride by comprehensively utilizing superfine silicon powder | |
| CN110156352A (en) | A kind of preparation method of air quenching metallurgical slag microballon | |
| CN113897494B (en) | Preparation method of electric stranded wire | |
| CN102602995B (en) | Production method of large-particle-size antimonous oxide | |
| CN1609024A (en) | Short basalt fiber making method and apparatus | |
| CN110526287B (en) | Sieve plate-free fluidized bed chlorination furnace | |
| CN1207246C (en) | Method for producing electric smelting calcium zirconate | |
| CN103911664B (en) | A kind of synthetic method of lenticular potassium hexatitanate | |
| CN1052459C (en) | Method and appts. for prodn. of cubic crystal form antimony trioxide | |
| CN101306917B (en) | Boron-magnesium-calcium powder E glass formula | |
| CN205603449U (en) | A melting furnace device for producing basalt rock wool have an energy -efficient environmental protection | |
| RU2149841C1 (en) | Process of manufacture of mineral wool articles from basalt carrying rocks and technological line for its implementation | |
| CN110590169A (en) | Novel mineral wool multilayer processing preparation method | |
| CN1168664C (en) | Method for controlling grain size in preparation of antimony trioxide by using lead antimony alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: GUANGXI HUATI SCIENCE CO., LTD. Free format text: FORMER OWNER: WANG TAO; SHI JIANRONG; PAN SHANCHU Effective date: 20080905 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20080905 Address after: The Guangxi Zhuang Autonomous Region Nanning high tech Development Zone, 4 road and Technology Park Building Room 707 zip code: 530003 Patentee after: China Antimony Technology Co., Ltd. Address before: The Guangxi Zhuang Autonomous Region Nanning LIANG Qing District Nanning Coastal Economic Corridor Development Zone Private Industrial Park Guangxi Hua antimony Chemical Industry Co., Ltd. zip: 530221 Co-patentee before: Shi Jianrong Patentee before: Wang Tao Co-patentee before: Pan Shanchu |