CN102602996B - Preparation device for catalyst-grade antimonous oxide - Google Patents
Preparation device for catalyst-grade antimonous oxide Download PDFInfo
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- CN102602996B CN102602996B CN201210097320.4A CN201210097320A CN102602996B CN 102602996 B CN102602996 B CN 102602996B CN 201210097320 A CN201210097320 A CN 201210097320A CN 102602996 B CN102602996 B CN 102602996B
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Abstract
The invention discloses a preparation device for catalyst-grade antimonous oxide, which comprises an antimony white furnace (1) and a reactor (8). The preparation device for the catalyst-grade antimonous oxide has the characteristics that the inner chamber of the antimony white furnace (1) is provided with a front chamber (2) and a rear chamber (3) which are communicated; the front chamber (2) and the rear chamber (3) are respectively provided with a blowpipe; one end of the blowpipe passes through the antimony white furnace wall to extend into the chamber; the other end of the blowpipe is arranged out of the antimony white furnace (1); the top of the rear chamber (3) is connected with the reactor (8); and the top of the reactor (8) is provided with a crystallizer. The preparation device for the catalyst-grade antimonous oxide has the advantages of simple structure and low manufacture cost. When the preparation device for the catalyst-grade antimonous oxide is used for preparing the antimonous oxide, only air needs to be compressed, and pure oxygen is omitted.
Description
Technical field
The present invention relates to a kind of pyrogenic process and produce the device, method, particularly catalyst grade antimonous oxide preparation facilities of antimonous oxide.
Background technology
Catalyst grade antimonous oxide is a kind of important industrial chemicals, it is during as catalyzer in polyester polycondensation reaction process, require this catalyzer not only will have higher purity, and do not contain four weisspiessglanzs of high price, also require to have higher catalytic activity simultaneously.Catalyst grade antimonous oxide is mainly to adopt pyrogenic process and wet processing to be prepared at present,
Some open source literatures have been reported the method for preparing antimonous oxide in recent years, for example:
1, Chinese patent, application number: CN200510031323.8, the applying date: 2005.03.11 title: catalyst grade super high purity Sb 2 O 3 production method and device thereof, summary: a kind of production method of catalyst grade super high purity Sb 2 O 3 and device thereof, its production method is from stibium trioxide stove furnace roof to antimony liquid surface, to spray into the pressurized air of 0.1-0.8MPa, and adopt following the two one: (1) is by the mode of electrical heating element indirect heating supply part heat, make burner hearth conversion zone everywhere temperature bring up to more than 1100 ℃, conversion zone central authorities temperature is more than 1200 ℃, (2) burner hearth flue gas is imported to a high-temperature gasification reactor, make antimonous oxide flue gas be warming up to rapidly 1100-1600 ℃, then high temperature antimonous oxide flue gas is cooling through quenching equipment, bag collection obtains antimonous oxide product, and this equipment needs electrical heating element as utility appliance, and production cost is improved.
2, Chinese patent, application number: the CN99117587.5 applying date: 1999.09.08 title: a kind of method and apparatus of producing superfine antimony trioxide, summary: a kind of method and apparatus of producing superfine antimony trioxide for low-temperature surface oxidation style, use containing antimony multicomponent alloy (Pb-Sb-Ag-Au-Bi), (Ph-Sb-Ag) be raw material, in special crucible, to being blown into air through the molten alloy surface of external heating fusing in advance, set 90-350 ℃ of surface oxidation temperature, and utilize oxidizing temperature constant control molten alloy temperature, regulate freezing air feed rate simultaneously, can produce ultra-fine stibium trioxide Fsss granularity 0.1-0.35 μ m, the equipment that this method is used needs the extra oxygen that adds, and the cold wind that this equipment enters reactor easily makes antimonous oxide shift to an earlier date crystallization.
3, Chinese patent, application number: the CN200910114079 applying date: 2009.05.19 title: a kind of method and special antimony white stove thereof of producing catalyst grade weisspiessglanz, before and after the burner hearth of special antimony white stove, both sides are installed with many blast pipes by body of heater is oblique; On the other furnace roof in body of heater left side, be fixedly installed reactor; This invention needs thermal source or the pure oxygen of additional costliness, and production cost is high, and production capacity is low, and equipment is complicated, the easy loss of production process, and the maintenance of the equipment cycle is short.
This just needs a kind of cost of manufacture low, does not need the antimonous oxide equipment of external thermal source and pure oxygen, to solve the above problems.
Summary of the invention
The object of this invention is to provide a kind of catalyst grade antimonous oxide Preparation equipment, overcome in prior art capacity consumption high, the shortcoming of the antimonous oxide purity deficiency of producing, reach reduction equipment cost, increase equipment life, improve product purity high, low object reduces production costs.
The solution of the present invention is by such realization: a kind of catalyst grade antimonous oxide preparation facilities, comprise stibium trioxide stove and reactor, it is characterized in that: in described stibium trioxide stove, thorax is provided with front thorax and the breech of connection, front thorax and breech are respectively equipped with blowpipe, described blowpipe one end is stretched in thorax through stibium trioxide furnace wall, and it is outside that the other end is arranged on stibium trioxide stove; Described breech top is connected with reactor, and described reactor head is provided with crystallizer.
Principle of work of the present invention is as follows: in the present invention, the stibium trioxide stove adopting is provided with front thorax and breech, and metallic antimony is smelted into metallic antimony liquid at stibium trioxide stokehold thorax, and blasts air by the blowpipe at front thorax, make metallic antimony liquid can contact fully volatilization with air, form antimonous oxide furnace gas; Subsequently antimonous oxide furnace gas is imported to back cavity, then by being arranged on the blowpipe of back room, blast air in back cavity, what make that antimony can continue contacts with air.Finally antimonous oxide furnace gas is imported to reactor sustained reaction, antimonous oxide imports the crystallizer at top the most at last, blasts cold wind and makes antimonous oxide furnace gas cooling, and crystallization, finally collects antimonous oxide by bagroom.
Above-described blowpipe is separately positioned on top and the sidepiece of front thorax and breech.
Above-described front thorax top and sidepiece are respectively equipped with top blast airduct a and side-blown airduct a, and described breech top and sidepiece are respectively equipped with top blast airduct b and side-blown airduct b.By the top at front thorax and breech and sidepiece, be respectively equipped with blowpipe, can so that metallic antimony when front thorax and breech, can comprehensively contact with air, avoid because blowing mouth is single, metallic antimony can not get fully reacting with oxygen, can only be by adopting pure oxygen to replace air to react with antimonous oxide.
Above-described crystallizer is ring-type jet-type crystallizer, and described ring-type jet-type crystallizer top is provided with cooling duct, and ring-type jet-type crystallizer can more large-arealy contact with antimonous oxide furnace gas, makes antimonous oxide crystallization faster; By cooling duct, inject secondary cold wind, can make the high purity sb2o3 steam that enters crystallizer be mixed rapidly by first and second cooling air, eliminate crystallization dead angle, and quench crystallization becomes high-purity, high activated catalyst level antimonous oxide completely.
The present invention has following beneficial effect:
1. the antimonous oxide purity that adopts the present invention to collect is high, and particle is thin, active high, median size 0.1～0.5 μ m, principal constituent Sb
2o
3>99.9%, 325 screen residues are less than 0.002%, EG transmitance >98%, whiteness are greater than 99, b value is lower than 0.92; Meet the requirement of catalyst grade antimonous oxide completely.
2. the present invention is simple in structure, only need repack existing single chamber stibium trioxide stove into two-chamber, then at cavity top and sidepiece, some blowpipes is set.
3. the present invention is air to the wind blasting, and does not need outer oxygen, thereby has saved manufacturing cost.
4. in the present invention, be provided with two chambers stibium trioxide stove, Double Tops blowpipe and the combination of bilateral blowpipe, while making antimony in stove, can be more fully oxidized, guarantee that antimonous oxide furnace gas can premature crystallization, finally make the antimonous oxide particle collected little, purity and active high.
Accompanying drawing explanation
Fig. 1 is the structural representation of catalyst grade antimonous oxide preparation facilities of the present invention;
Component title and sequence number in figure:
Stibium trioxide stove 1, front thorax 2, breech 3, top blast airduct a4, side-blown airduct a5, top blast airduct b6, side-blown airduct b7, reactor 8, ring-type jet-type crystallizer 9, cooling duct 10.
Embodiment
Below tie embodiment and describe this catalyst grade antimonous oxide preparation facilities:
As shown in Figure 1, this invention catalyst grade antimonous oxide preparation facilities, comprises stibium trioxide stove 1 and ring-type jet-type crystallizer 9, is provided with front thorax 2 and the breech 3 of connection in stibium trioxide stove 1, and the top of front thorax 2 is provided with top blast airduct a4, and sidepiece is provided with side-blown airduct a5; Breech 3 tops are connected with reactor 8, and breech 3 tops are provided with top blast airduct b6, and breech 3 sidepieces are also provided with side-blown airduct b7; Described top blast airduct a4, side-blown airduct a5, top blast airduct b6 and side-blown airduct b7, their one end are stretched in thorax through stibium trioxide furnace wall respectively, and the other end is connected with gas blower separately; The top of reactor 8 is connected with ring-type jet-type crystallizer 9, and ring-type jet-type crystallizer 9 tops are provided with cooling duct 10.
Embodiment 1:
Take 300g metallic antimony as raw material, stibium trioxide stove 1 furnace temperature is risen to 1000 ℃, to the interior input metallic antimony of front thorax 2 of stibium trioxide stove 1, make it to melt, the top top blast airduct a4 of thorax 2 and side-blown airduct a5 blast respectively top blast wind and primary side blowing forward, make antimony voloxidation, form antimonous oxide furnace gas; Antimonous oxide furnace gas is imported to breech 3, and blast respectively secondary top blast wind and secondary side blowing to top blast airduct b6 and the side-blown airduct b7 of breech 3, make furnace gas continuous contact oxygen; Stibium trioxide stove 1 temperature degree is further promoted to after 1200 ℃, then antimonous oxide furnace gas is imported to reactor 8, and keep the temperature-stable of reactor 8; Finally high temperature oxidation antimony furnace gas is imported to ring-type jet-type crystallizer 9, add cooling air one time respectively in ring-type jet-type crystallizer 9 bottoms, at cooling duct 10, add secondary cooling air, finally by bagroom, collect antimonous oxide, quality is 350 grams.
Embodiment 2:
The 50 kilograms of metallic antimonies of take are raw material, stibium trioxide stove 1 furnace temperature is risen to 1000 ℃, the interior input metallic antimony of front thorax 2 to stibium trioxide stove 1, make it to melt, the top top blast airduct a4 of thorax 2 and side-blown airduct a5 blast respectively top blast wind and primary side blowing forward, make antimony voloxidation, form antimonous oxide furnace gas; Antimonous oxide furnace gas is imported to breech 3, and blast respectively secondary top blast wind and secondary side blowing to top blast airduct b6 and the side-blown airduct b7 of breech 3, make furnace gas continuous contact oxygen; Stibium trioxide stove 1 temperature degree is further promoted to after 1300 ℃, then antimonous oxide furnace gas is imported to reactor 8, and keep the temperature-stable of reactor 8; Finally high temperature oxidation antimony furnace gas is imported to ring-type jet-type crystallizer 9, in ring-type jet-type crystallizer 9 bottoms, add cooling air one time respectively, at cooling duct 10, add secondary cooling air, finally by bagroom, collect antimonous oxide, quality is 58.3 kilograms.
Embodiment 3:
The 20 kilograms of metallic antimonies of take are raw material, stibium trioxide stove 1 furnace temperature is risen to 1000 ℃, the interior input metallic antimony of front thorax 2 to stibium trioxide stove 1, make it to melt, the top top blast airduct a4 of thorax 2 and side-blown airduct a5 blast respectively top blast wind and primary side blowing forward, make antimony voloxidation, form antimonous oxide furnace gas; Antimonous oxide furnace gas is imported to breech 3, and blast respectively secondary top blast wind and secondary side blowing to top blast airduct b6 and the side-blown airduct b7 of breech 3, make furnace gas continuous contact oxygen; Stibium trioxide stove 1 temperature degree is further promoted to after 1250 ℃, then antimonous oxide furnace gas is imported to reactor 8, and keep the temperature-stable of reactor 8; Finally high temperature oxidation antimony furnace gas is imported to ring-type jet-type crystallizer 9, in ring-type jet-type crystallizer 9 bottoms, add cooling air one time respectively, at cooling duct 10, add secondary cooling air, finally by bagroom, collect antimonous oxide, quality is 23.3 kilograms.
Claims (2)
1. a catalyst grade antimonous oxide preparation facilities, comprise stibium trioxide stove (1) and reactor (8), it is characterized in that: the described interior thorax of stibium trioxide stove (1) is provided with front thorax (2) and the breech (3) of connection, front thorax (2) and breech (3) are respectively equipped with blowpipe, described blowpipe one end is stretched in thorax through stibium trioxide furnace wall, and the other end is arranged on stibium trioxide stove (1) outside; Described breech (3) top is connected with reactor (8), and described reactor (8) top is provided with crystallizer.Described blowpipe is separately positioned on top and the sidepiece of front thorax (2) and breech (3), described front thorax (2) top and sidepiece are respectively equipped with top blast airduct a(4) and side-blown airduct a(5), described breech (3) top and sidepiece are respectively equipped with top blast airduct b(6) and side-blown airduct b(7).
2. catalyst grade antimonous oxide preparation facilities according to claim 1, is characterized in that: described crystallizer is ring-type jet-type crystallizer (9), and described ring-type jet-type crystallizer (9) top is provided with cooling duct (10).
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103332730B (en) * | 2013-07-17 | 2014-10-29 | 柳州百韧特先进材料有限公司 | Production system for preparing stannic oxide with gasification method |
| CN104326508B (en) * | 2014-10-20 | 2017-03-29 | 汕头市双鹏塑料实业有限公司 | Nanometer grade antimony trioxide preparation method |
| 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 |
| CN104310473B (en) * | 2014-10-20 | 2016-05-25 | 广西高中阀门制造有限责任公司 | Nanometer grade antimony trioxide preparation facilities |
| CN104355332B (en) * | 2014-10-20 | 2017-01-11 | 郑香萍 | Preparation device of antimony trioxide for polyester |
| CN108622933B (en) * | 2018-06-08 | 2020-02-11 | 广东宇星阻燃新材股份有限公司 | Antimony trioxide powder crystal system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078266A (en) * | 1992-05-03 | 1993-11-10 | 南宁锑品厂 | Plasma antimony oxide furnace with reflection type dual-reaction chamber |
| CN1382815A (en) * | 2002-03-11 | 2002-12-04 | 阎祖军 | Process and equipment for preparing antimory oxide from PbSb alloy |
| CN1873061A (en) * | 2006-04-27 | 2006-12-06 | 王涛 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
| CN202492377U (en) * | 2012-04-05 | 2012-10-17 | 广西华锑科技有限公司 | Catalyst-grade grading antimony trioxide preparation device |
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- 2012-04-05 CN CN201210097320.4A patent/CN102602996B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078266A (en) * | 1992-05-03 | 1993-11-10 | 南宁锑品厂 | Plasma antimony oxide furnace with reflection type dual-reaction chamber |
| CN1382815A (en) * | 2002-03-11 | 2002-12-04 | 阎祖军 | Process and equipment for preparing antimory oxide from PbSb alloy |
| CN1873061A (en) * | 2006-04-27 | 2006-12-06 | 王涛 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
| CN202492377U (en) * | 2012-04-05 | 2012-10-17 | 广西华锑科技有限公司 | Catalyst-grade grading antimony trioxide preparation device |
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