CN1052459C - Method and appts. for prodn. of cubic crystal form antimony trioxide - Google Patents
Method and appts. for prodn. of cubic crystal form antimony trioxide Download PDFInfo
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- CN1052459C CN1052459C CN 97107947 CN97107947A CN1052459C CN 1052459 C CN1052459 C CN 1052459C CN 97107947 CN97107947 CN 97107947 CN 97107947 A CN97107947 A CN 97107947A CN 1052459 C CN1052459 C CN 1052459C
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- furnace gas
- antimony
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- antimony trioxide
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Abstract
The present invention relates to a method and apparatus for producing cubic crystal antimony trioxide. An antimony white furnace with a reflecting furnace structure is used, and the high-temperature furnace gas discharge end of a cylindrical reaction chamber in the antimony white furnace is provided with a mixture quenching device. The surface of antimony liquid is added with an inorganic salt covering agent, and an antimony trioxide product of which the cubic crystal content is more than 99% can be obtained by controlling the quenching condition of high-temperature furnace gas containing the antimony trioxide. The method has easily controlled conditions, has the advantages of low energy consumption, large yield capability, and good and stable product quality and has obvious economic benefits.
Description
The present invention relates to a kind of production method and device thereof of cubic crystal form antimony trioxide.
Antimonous oxide is a kind of important chemical material, is widely used in the retardant synergist of inflammable substance such as plastics, rubber, paint, chemical fibre, ramie cotton fabric, the important source material of industry such as polyester synthetic catalyzer and pigment, enamel.Cubic crystal form antimony trioxide particularly, because it has good chemically reactive and light stability, physicochemical properties such as high whiteness receive praises from customers.
The method of producing cubic crystal form antimony trioxide is at present mainly used two kinds of wet method and pyrogenic processes.Wet method mainly is the antimonous oxide hydrolysis method, number is 92114236.6 described methods as Chinese patent application.Pyrogenic process mainly contains the low-temperature oxidation method of plasma method and metallic antimony, is the particle diantimony trioxide product that CN1038444A adopts plasma method to produce as publication number, and cubic content can reach more than 99%.Preparation method as JP79108798 and the described cubic crystal form antimony trioxide of JP80114418 patent is the low-temperature oxidation method of metallic antimony.This method is that metallic antimony and lead are mixed by a certain percentage, and oxidized metal antimony at a lower temperature after fusing in the electric furnace obtains cubic crystal form antimony trioxide.More than these methods all can obtain cubic crystal form antimony trioxide, but wet method has the contaminated wastewater environment, equipment corrosion is serious, pyrogenic process then has the energy consumption height, yields poorly, working condition is difficult to defectives such as control.Chinese patent 85102489.0 " a kind of stibium trioxide stove of reverberatory furnace structure " is to be raw material with the metallic antimony, blasting first and second air makes fused antimony liquid autothermal oxidation become antimonous oxide steam, through a large amount of cooling air quenchings, trap the production method of antimonous oxide then through the bag collection system, it is simple to have technology, processing ease, and energy consumption is low, output is big, advantages such as constant product quality.But its product is not single cubic, and the content of its cubic has only 60～80%, is difficult to satisfy user's requirement.
The objective of the invention is to utilize the stibium trioxide stove of reverberatory furnace structure, after improving, can produce the antimonous oxide of single cubic.
For realizing this purpose, the present invention adopts the stibium trioxide stove of 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 the cylindrical reaction chamber that makes the stibium trioxide stove is discharged enters a mixing chilling apparatus, with a large amount of cooling airs furnace gas is carried out quenching, make the antimonous oxide quench crystallization in the furnace gas, generate the antimonous oxide of full cubic crystal model.
Insulating covering agent of the present invention be a kind of can be under 950～1100 ℃ of the normal running temperatures of stibium trioxide stove, form the mineral compound that the runny tectum of one deck covers antimony liquid surface on antimony liquid surface, preventing or to reduce the antimony liquid oxidation volatilization in non-oxide zone in the burner hearth and the high temperature phase crystallisate that forms, promptly iris type antimonous oxide enters in the reaction chamber and influences end product quality.As the inorganic salt of insulating covering agent is the oxysalt or the hydrochloride of silicon, boron, phosphorus, sulphur, carbon, and preferably their potassium or sodium or ammonium or aluminium salt can be any or the mixtures more than two kinds in them.As pure aluminium silicate, borax, sodium phosphate, sodium sulfate, ammonium phosphate, soda ash, salt, salt of wormwood, vitriolate of tartar etc.
The device that the inventive method is used below in conjunction with accompanying drawing is described further.
Accompanying drawing is the front view of the inventive method using appts.
Mixing chilling apparatus 6 of the present invention is discharged with the furnace gas of the cylindrical reaction chamber 7 of stibium trioxide stove 1 End closely links to each other, and this mixes chilling apparatus, by cylindrical tube 2, is arranged at the cooling of cylindrical shell 2 one sides Wind upper blast pipe 5 is arranged at air intake under the mixing furnace gas outlet 3 of cylindrical shell 2 opposite sides and the cooling air Mouthful 4 compositions, lower air inlet 4 be positioned at mix furnace gas outlet 3 below. When containing antimony oxide When the furnace gas of steam enters mixing chilling apparatus 6 from cylindrical reaction chamber 7, be subjected to immediately from enterprising Fierce " pincer attack " of the cooling-air of airduct 5 and lower air inlet 4 makes it effectively mix with cooling-air And quick cooling, control cooling air total amount is interior 1-5 times of discharging the furnace gas total amount of stove, makes high-temperature furnace gas Suddenly be down to below 500 ℃, the antimony oxide instant steam crystal phase transition temperature interval of jumping over, thereby The antimony oxide product that condenses into full cubic crystal model captures in the bag collection system.
The present invention is big except the output with reverberatory furnace structure stibium trioxide stove, and energy consumption is low, the simple advantage of technology Outward, the stibium trioxide product quality is better. The cost of the full cubic crystal model antimony oxide of producing compares plasma Method, electric furnace process is hanged down 20-40%, and significant economic benefit is arranged.
Further specify with embodiment below:
Example 1 is at 5.4m
2Cylindrical reaction chamber 7 tops of stibium trioxide stove 1 closely connect mixing quencher 6 of the present invention, upper blast pipe 5 is communicated with former stibium trioxide stove cooling duct, adding soda ash covers antimony liquid surface, controlled chilling air intake total amount is 2 times of furnace gas export total amount, collects the antimonous oxide product of cubic then in the cloth bag chamber.With No. two star metals meeting national standard is raw material, 11.8 tons of daily output antimonous oxide products, and the product cubic is 99.2%, and the Fei Shi mean particle size is 0.95 micron, and chemical ingredients is Sb
2O
399.75%, AS
2O
30.04%, PbO0.08%.
Example 2 is removed the adding primary ammonium phosphate antimony liquid surface is covered, the cooling air total amount is outside 4 times of the high-temperature furnace gas total volume of exports, all the other conditions are identical with example 1, obtain 11 tons of antimonous oxide products every day in the cloth bag chamber, the product cubic is 99.5%, 0.84 micron of Fei Shi mean particle size, and Chemical Composition is Sb
2O
399.68%, AS
2O
30.04%, PbO0.07%.
Example 3 is except that insulating covering agent is pure aluminium silicate and soda ash, and all the other conditions are identical with example 1, obtains 11.6 tons of antimonous oxide products every day in the cloth bag chamber, and the product cubic is 99.6%, the Fei Shi mean particle size is 0.92 micron, and Chemical Composition is Sb
2O
399.72%, AS
2O
30.04%, PbO0.06%.
Claims (3)
1, a kind of production method of cubic crystal form antimony trioxide, adopt the stibium trioxide stove of reverberatory furnace structure, it is characterized in that making insulating covering agent with the inorganic salt of sodium or potassium covers antimony liquid surface in the stove, and the furnace gas that makes trioxygen-containingization two antimony of stibium trioxide stove cylindrical reaction chamber discharge enters a mixing chilling apparatus, with a large amount of cooling airs furnace gas is carried out quenching, make the antimonous oxide quench crystallization in the furnace gas generate cubic crystal form antimony trioxide, the 1-5 that feeds the cooling air volume that mixes in the chilling apparatus and be the furnace gas amount that cylindrical reaction chamber discharges doubly.
2, the production method of cubic crystal form antimony trioxide according to claim 1 is characterized in that as the sodium of insulating covering agent or the inorganic salt of potassium be the oxysalt or the hydrochloride of silicon, sulphur, carbon, can be any or the mixture more than two kinds in them.
3, the employed device of the production method of the described cubic crystal form antimony trioxide of claim 1, the stibium trioxide stove [1] that comprises reverberatory furnace structure, the furnace gas outlet end that it is characterized in that stibium trioxide stove [1] round tube type reaction chamber [7] is provided with mixing chilling apparatus [6], it is made up of blast inlet [4] under cylindrical tube [2], the cooling air upper blast pipe [5] that is arranged at cylindrical shell [2] one sides, the mixing furnace gas outlet pipe [3] that is arranged at cylindrical shell [2] opposite side and the cooling air, following blast inlet [4] be positioned at mix furnace gas outlet pipe [3] below.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97107947 CN1052459C (en) | 1997-01-29 | 1997-01-29 | Method and appts. for prodn. of cubic crystal form antimony trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97107947 CN1052459C (en) | 1997-01-29 | 1997-01-29 | Method and appts. for prodn. of cubic crystal form antimony trioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1173468A CN1173468A (en) | 1998-02-18 |
| CN1052459C true CN1052459C (en) | 2000-05-17 |
Family
ID=5169987
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97107947 Expired - Lifetime CN1052459C (en) | 1997-01-29 | 1997-01-29 | Method and appts. for prodn. of cubic crystal form antimony trioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1052459C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100393921C (en) * | 2006-04-27 | 2008-06-11 | 王涛 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
| 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 |
| CN104355332B (en) * | 2014-10-20 | 2017-01-11 | 郑香萍 | Preparation device of antimony trioxide 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 |
-
1997
- 1997-01-29 CN CN 97107947 patent/CN1052459C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1173468A (en) | 1998-02-18 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: XIKUANGSHAN SHANXING ANTIMONY INDUSTRY CO., LTD. Free format text: FORMER NAME OR ADDRESS: TIN MINE MINING AFFAIRS BUREAU |
|
| CP03 | Change of name, title or address |
Address after: 417502 Lengshuijiang, Hunan Province Patentee after: Tinnery Shanxing Antimony Industry LLC Address before: 417502 Lengshuijiang, Hunan Province Patentee before: Tin Mine Mining Affairs Bureau |
|
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20000517 |