2. The invention relates to a method for controlling particle size in preparing antimony trioxide from lead-antimony alloy. In this method, air is heated by the heater 8, and then evenly blown into the metal surface in the furnace through the bellows 4, the air distribution plate 7 and the air duct 3, thus directly heating the alloy melt containing Pb 10-90% and Sb90- 10%. Under the condition that the melt temperature is stabilized below 700℃, metallic antimony volatilizes and oxidizes, and the antimony trioxide obtained by oxidation is cooled and crystallized at the adjustable cavity temperature (150-550℃) to obtain antimony trioxide with an average particle size of 0.3-5 microns. ..
Method for preparing antimony trioxide (antimony white) from metallic antimony A method for preparing antimony trioxide (antimony white) from metallic antimony belongs to metallurgical technology. This method is to produce antimony trioxide by oxidation and volatilization in an antimony white furnace, which is like a small reverberatory furnace with two cylindrical reaction chambers. The lower part of the chamber is provided with an air pipe, which is inserted into the antimony melt to blow; An air pipe with a downward outlet is installed in the reaction chamber to blow air to antimony melt. When antimony melts, it is oxidized by oxygen in the air in the reaction chamber to produce Sb.
Method for preparing ultrafine antimony trioxide The invention uses SbCl.
5 preparation of ultrafine antimony trioxide by alkoxide-ammonolysis this patent uses alkoxide-ammonolysis to prepare high-purity ultrafine antimony trioxide. In this method, antimony trichloride, ethanol and concentrated ammonia water are used as raw materials, and alcoholization, hydrolysis and ammonolysis are completed in one step in the same container to obtain ultrafine antimony white with a particle size of about 1 μ. The product has good whiteness and high purity. The reaction conditions are not harsh, the reaction period is short, the energy consumption is low, the equipment is simple, and the excessive raw material ethanol can be recovered. Excess NH
The invention belongs to the field of technology and equipment for producing antimony trioxide ultrafine powder by plasma method. The vortex stabilized DC arc plasma generator uses pure air as working gas, which has high electrothermal conversion efficiency and obviously reduces investment. The invention can use different grades of antimony white or antimony oxide, or directly use antimony sulfide concentrate as raw material, Sb
7. A method for producing high-purity and high-fineness antimony trioxide from stibnite. A method for producing high-purity and high-fineness antimony trioxide from stibnite consists of stibnite (main component Sb)
8. The invention relates to a process and equipment for simultaneously producing antimony trioxide with different particle sizes. The process is that refined antimony reacts with air in antimony white furnace to prepare antimony trioxide. Under the action of two exhaust fans, antimony trioxide flows through two classifiers and three dust collection chambers, and four kinds of antimony trioxide with different particle sizes are obtained. The key equipment is a long cylindrical classifier and a dust chamber. A conical rotor (6) is designed at the upper part of the classifier, and a suction bag made of 100-200 mesh nylon cloth, 250-350 mesh nylon cloth and 208 # polyester flannel is installed in the dust collection room.
9 preparation method of cubic antimony trioxide A preparation method of cubic antimony trioxide includes the following steps: directly hydrolyzing antimony trichloride solution in alkaline aqueous solution, washing and drying to obtain cubic antimony trioxide. Characterized in that tartaric acid or tartrate is used as complexing agent in the hydrolysis reaction, and the molar ratio of antimony trichloride to tartaric acid or tartrate is1~ 26:1. The method of the invention has short reaction time and simple operation, and the obtained cubic crystal antimony trioxide has complete and single crystal form, high purity and good color, and is a good catalyst for polyester production. The method can be used for mass production of cubic antimony trioxide.
10 pyrometallurgical production method of ultrafine antimony trioxide A pyrometallurgical production method of ultrafine antimony trioxide, which is especially suitable for producing ultrafine antimony trioxide as a flame retardant additive, is improved on the basis of antimony white furnace with reverberatory furnace structure. Characterized in that an efficient air-cooled mixer is installed at the top of the furnace, and high-temperature quenching is directly realized at the top of the furnace. The dust removal system is equipped with a classifier, which has large output, low energy consumption, uniform and stable product quality, and the product Fisher is average.
1 1 A method for producing antimony trioxide powder from antimony oxide ore and sulfur-oxygen mixed antimony ore The invention discloses a method for producing antimony trioxide powder from antimony oxide ore and sulfur-oxygen mixed antimony ore. It adopts Webster's zinc-oxygen furnace smelting method to smelt antimony oxide ore or sulfur-oxygen mixed antimony ore at 950- 1250℃. Entering a bag-type antimony collector through an oxidation chamber, a settling chamber and a surface cooling tube to obtain antimony.
12 cubic antimony trioxide production method and device A cubic antimony trioxide production method and device adopt an antimony white furnace with a reverberatory furnace structure, a mixed quenching device is installed at the high-temperature furnace gas discharge end of a cylindrical reaction chamber in the antimony white furnace, an inorganic salt covering agent is added to the surface of antimony liquid, and the quenching conditions of the high-temperature furnace gas containing antimony trioxide are controlled, so that an antimony trioxide product with cubic crystal content of more than 99% can be obtained.
13 production method and device for coarse-grained antimony trioxide A production method and device for preparing coarse-grained antimony trioxide are provided. A grain coarsening device is installed at the upper end of a cylindrical reaction chamber of an antimony white furnace with a reverberatory furnace structure, the condensation speed of antimony trioxide vapor in the coarsening device is controlled, and an air separator is equipped in a dust removal system, thereby obtaining coarse-grained antimony trioxide with an average particle size of 2.5-3.5 microns. The method has the advantages of large output, low energy consumption, simple operation and obvious economic benefits.
14 method and device for producing granular antimony trioxide A method and device for producing granular antimony trioxide adopts an antimony white furnace with a reverberatory furnace structure, a high-temperature gasification reaction chamber is installed at the upper end of a cylindrical reaction chamber of the antimony white furnace, a burner is arranged in the high-temperature gasification reaction chamber, the fuel supply is adjusted, and the temperature of the gasification reaction chamber is maintained at 900-1800 DEG C, By controlling the ratio of the volume of high-temperature furnace gas containing antimony trioxide to the volume of quenching air in the quenching mixer, ultrafine antimony trioxide with an average particle size of 0.05 ~ 0.2 micron and full cubic crystal form can be obtained, and ultra-high purity antimony trioxide with a main component of 99.85% and a whiteness of over 98% can also be obtained. This method has the advantages of large output, low energy consumption and good economic benefit.
15 a process for preparing high-purity ultrafine antimony trioxide. The process for preparing high-purity ultrafine antimony trioxide includes melting refined antimony in a vertical blowing furnace, adding a certain amount of purified air antimony oxide into fermented soybean at the constant temperature of antimony liquid, separating coarse particles from the obtained reaction product by a cyclone, cooling and settling by a herringbone condenser tube, and finally filtering by an electric vibration reverse suction bag filter to obtain the product with no black spots, no impurities and aluminum content below 0.09%.
16 a method and equipment for producing ultrafine antimony trioxide a method and equipment for producing ultrafine antimony trioxide by surface oxidation at low temperature, in which antimony-containing multicomponent alloys (Pb-Sb-Ag-Au-Bi) and (Ph-Sb-Ag) are used as raw materials, and air is blown into the surface of molten alloy melted by external heating in a special crucible, and the surface oxidation temperature is set at 90-350. Ultrafine antimony white Fsss with particle size of 0. 1-0.35 μ m can be produced by controlling the temperature of alloy liquid with constant oxidation temperature and adjusting the supply of cold air. Compared with airflow crushing method and plasma method, this method has lower cost, more stable quality and lower equipment investment. The process equipment is used to recover high lead antimony ore and antimony gold arsenic ore, which has obvious economic benefits.
Application of 17 nanometer antimony trioxide as polyester polycondensation catalyst The present invention relates to the application of nanometer antimony trioxide as catalyst in polyester polycondensation reaction, which is a molecular polycondensation reaction after esterification of terephthalic acid or transesterification of dimethyl terephthalate. The nano antimony trioxide catalyst has the characteristics of small average particle size, uniform dispersion in polyester polycondensation reaction, good solubility, high catalytic activity and low cost.
18 decomposition method for preparing high-purity antimony trioxide The invention discloses a decomposition method for preparing high-purity antimony trioxide, which comprises the following steps: preparing antimony oxide powder and water into a suspension, removing impurities, introducing into a reactor, preparing nitric acid and water in the suspension into 5% dilute nitric acid, heating with steam, stirring for reaction, filtering, washing to neutrality, drying at high temperature, and pulverizing to obtain a finished product. The raw material antimony oxide powder used in the invention is easily available and cheap, the fixed investment is only one tenth of that of the indirect method, and the cost is lower than one third of that of the indirect method, and the product quality can reach or even exceed the standard of the indirect method. In addition, no "three wastes" are discharged into the environment, and the process is simple and practical.
19 method for preparing high-purity ultrafine antimony trioxide by gas phase method A method for preparing high-purity ultrafine antimony trioxide by gas phase method comprises the following steps: taking crude antimony oxide, industrial hydrochloric acid and ammonia as raw materials, distilling antimony trichloride dissolved in crude antimony oxide out of the kettle in a gaseous state, and distilling at atmospheric pressure to obtain distillate at135℃-226℃, or distilling at reduced pressure to obtain distillate at corresponding temperature range. Decompressed antimony trichloride reacts with ammonia-containing steam in cocurrent contact, the reaction temperature is 120℃ ~ 145℃, the pressure is 0.007 ~ 0.6 MPa, the reaction time is 2 ~ 30 minutes, and the flow ratio of antimony trichloride to ammonia-containing steam is1:10. Ammonia gas and water vapor are recovered under heating and pressure, the generated antimony trioxide and ammonium chloride are separated by cyclone separator, and the mixed crystals sublimate ammonium chloride at 300℃ ~ 400℃ to obtain high-purity fine-grained antimony trioxide. The method has the advantages of low cost, low equipment investment, low requirements for raw materials and remarkable economic benefits.
Method and device for producing 20 nanometer antimony trioxide. According to the invention, antimony oxide or antimony oxide ore powder is used as raw materials, air plasma is used as a heat source, a production device consisting of a horizontal reactor and a secondary gasification production method are adopted, and a product with a specific surface area of 48-75m is obtained.
2 1 method and device for producing catalyst grade ultra-high purity antimony trioxide The invention discloses a method and device for producing catalyst grade ultra-high purity antimony trioxide. The production method is to spray 0. 1-0.8MPa compressed air from the top of the antimony white furnace to the surface of antimony liquid, and adopt one of the following two methods: (1) indirect heating with electric heating elements to provide partial heat, so as to raise the temperature of each part of the reaction zone in the furnace to above 1 100℃, and the central temperature of the reaction zone is at/. (2) introducing the flue gas in the furnace into the high-temperature gasification reaction chamber, so that the temperature of the antimony trioxide flue gas can be rapidly increased to1100-1600 DEG C; Then, the high-temperature antimony trioxide flue gas is cooled by a quenching mixing device, and the antimony trioxide product is obtained by bag dust removal. The production equipment used is an improved antimony white furnace. Compared with the known plasma production methods and devices, the energy consumption of the products produced by the invention is reduced by more than 70%, the furnace output can reach 6- 15t/d, and the production cost can be reduced by more than 30%. The method has the advantages of simple operation, easy control of process parameters, stable and reliable product quality and the like.
Method and device for producing single-crystal antimony trioxide with uniform particle size distribution A method and device for producing single-crystal antimony trioxide with uniform particle size distribution adopts reflective antimony white furnace smelting method. After antimony is melted in the reflective antimony white furnace, air is blown into the surface of the molten antimony in the furnace to oxidize antimony into antimony trioxide furnace gas, which is then cooled and crystallized, discharged from the furnace gas outlet pipe, and then collected by the dust collection system. Characterized in that after the furnace gas oxidized into antimony trioxide is led out, it first passes through an air-cooled reactor, and then undergoes three-stage cooling crystallization in a crystallizer, and then it is discharged from the furnace gas outlet pipe, and then it is captured by a dust removal system to obtain a single crystal with uniform particle size distribution and a single peak, with an average particle size of 0.2-3.5 μ m and Sb as the main component.
23. The invention relates to a method for manufacturing inorganic filler and antimony trioxide master batch. (weight percentage) 20-70% of inorganic powder material with particle size distribution between1.0-10.0 micron, 20-70% of antimony trioxide powder material with particle size distribution between 0.5-2.0 micron, 4-20% of carrier, 4-10% of dispersant. Heat and stirring in a high-speed stirr or a continuous modifying unit, fully mixing, adding into a twin-screw extrude, granulating and molding by a water ring granulating device, automatically identifying the specifications of the master batch by a vibrating screen after molding, dehumidifying by a dryer, and packaging. The total powder content of inorganic filler and antimony trioxide in the invention is 70-90%. By selecting dispersant and coupling agent reasonably and selecting different carriers according to different processing substrates and performance requirements, the masterbatch suitable for plastic processing industry was manufactured.
24. The invention relates to a manufacturing method of antimony trioxide master batch. 70-90% of antimony trioxide powder material with particle size distribution of 0.4-2.0μ m, 4-20% of carrier, 4- 10% of dispersant and 0.1%of titanate or silane coupling agent are heated and stirred in a high-speed mixer or a continuous modification device. The invention can not only fundamentally solve the dust problem in the secondary modification processing of polymers, but also improve the compatibility of powder materials and plastic matrix, the interface bonding and crystallization behavior and morphology of fillers and polymer materials, improve the fluidity, mechanical properties and flame retardant function of materials, and reduce the decline of plastic mechanical properties.
25. Method for manufacturing decabromodiphenyl ether and antimony trioxide master batch The present invention relates to a method for manufacturing decabromodiphenyl ether master batch. 70-90% of decabromodiphenyl ether powder with particle size distribution of 0.4-2.0μ m, 4-20% of carrier, 4- 10% of dispersant, 0.1%of titanate or silane coupling agent are heated and stirred in a high-speed mixer or a continuous modification device, and fully stirred. The content of decabromodiphenyl ether powder in the invention is 70-90%. According to different processing substrates and performance requirements, the masterbatch suitable for plastic processing industry is made by reasonably selecting dispersants and coupling agents and selecting different carriers.
26. The invention relates to a method for manufacturing decabromodiphenyl ethane and antimony trioxide master batches. (weight percentage) 50-70% of decabromodiphenyl ethane powder with particle size distribution of 0.4-2.0μ m, 20-40% of antimony trioxide powder, 4-20% of carrier, 4- 10% of dispersant, and 0.1%of titanate or silane. The flame-retardant master batch of the invention is directly added into resin for extrusion or injection molding. It can simplify the production process, reduce dust flying and equipment wear, save raw materials, make the mixing of raw materials convenient and uniform, thus improving the production efficiency and product performance indicators.