546results about "Halogenated silanes" patented technology

The utility model discloses a device for removing impurities in trichlorosilane, relates to the technical field of polycrystalline silicon production, and mainly aims to improve the removal efficiency of the impurities in the trichlorosilane on the basis of not increasing the cost. According to the main technical scheme, the device for removing the impurities in the trichlorosilane is characterized in that an inlet of a first mixer is connected to one end of a first feeding pipe and a second feeding pipe, a plurality of baffle plates are arranged in a reaction tank in a staggered mode and used for forming a baffle channel in the reaction tank, and one end of the baffle channel is connected to an outlet of the first mixer; the other end of the baffling channel, the filter and an inlet of the separating tower are sequentially connected, the inlet of the separating tower is further connected to a siloxane conveying pipe, a tower kettle of the separating tower is connected to the other end of the first feeding pipe and used for guiding siloxane to the first mixer, and a top collecting pipe of the separating tower is connected to the rectifying unit; wherein the second feeding pipe is used for guiding a trichlorosilane and dichlorosilane mixture containing impurities to the first mixer.

The invention discloses a preparation method of high-purity diiodosilane, which comprises the following steps: firstly, preparing a p-phenylsilane solution from phenyl trichlorosilane and sodium hydride as raw materials, rectifying and purifying the p-phenylsilane solution, directly reacting the p-phenylsilane solution with iodine to generate diiodosilane, and reacting phenylsilane with iodine to directly generate diiodosilane; in the process of preparing diiodosilane from phenylsilane, conditions are mild, the reaction process is controllable, the reaction time is shortened by controlling the temperature in the synthesis process and increasing the pressure of a reaction system, hydrogen iodide overflow is reduced, sodium hydride is adopted as a reducing agent in the reaction process, and the yield of diiodosilane is increased. The solid waste can be recycled, the cost can be effectively reduced, and industrialization of diiodosilane is facilitated.

The present invention refers to a SiC and Chlorosilane production system 2540, comprising at least one CVD SiC production reactor 850, in particular SiC fluidized bed reactor 850a, in particular according to claim 9, and a Chlorosilane production unit 2550, wherein the Chlorosilane production unit 2550 comprises at least a bed reactor 2416, in particular a fixed bed reactor or a fluidized bed reactor, for generating Chlorosilanes by reacting at least one fraction of the vent gas mixture provided via the vent gas outlet 216 of the CVD SiC production reactor 850 and Si, wherein further fractions of the vent gas mixture at least comprise H2 and a C-bearing molecule, in particular methane, and wherein Si is provided as solid 2398 inside the bed reactor 2416.

The utility model relates to the technical field of polycrystalline silicon production equipment, in particular to a trichlorosilane purification system in a polycrystalline silicon production process, which is characterized in that a coarse distillation primary tower is communicated with a cold hydrogenation primary separation tower; the low-boiling-point recovery tower is communicated with the primary crude distillation tower; the crude distillation secondary tower is communicated with the crude distillation primary tower; the rectification primary tower is communicated with the crude distillation secondary tower; the high-boiling recovery tower is communicated with the rectification primary tower; the rectifying secondary tower is communicated with the rectifying primary tower; the rectification secondary tower is communicated with the crude distillation primary tower; the third-stage rectification tower is communicated with the second-stage rectification tower; a tower kettle of the third-stage rectification tower is communicated with the first-stage rectification tower; the light component removal tower is communicated with the low-boiling-point recovery tower and the high-boiling-point recovery tower; the heavy component removal tower is communicated with the light component removal tower; the high-boiling recovery tower is communicated with the tower kettle of the de-heavy tower; a gas phase outlet of the heavy component removal tower is sequentially connected with a gas phase adsorption device and a light component tower; a reflux inlet of the light component tower is communicated with the light component removal tower; and the heavy separation tower is communicated with the light separation tower. According to the utility model, the stability and reliability of large-load operation of the rectification system can be improved.

The present invention relates to an integrated silane gas reaction device, including: a buffer tank for reducing the exhaust gas flow rate; a reactor, in which the exhaust gas undergoes a spontaneous combustion reaction; a dust collector for removing dust particles mixed in the exhaust gas; an exhaust pipe installed on one side of the dust collector and interconnected with the inside of the dust collector; a notch provided on the exhaust pipe, the number of which is set to two; a filter plate slidably arranged in the notch, the number of which is the same as the number of notches; a fixed frame installed on one side of the dust collector; a switching component provided on the fixed frame, used to drive two filter plates to engage with the notch in turn; a positioning component provided under the exhaust pipe, used to position the filter plate engaged with the notch. The integrated silane gas reaction device provided by the present invention realizes that the incomplete gear can alternately drive the two filter plates to abut and release the corresponding notches when it rotates one circle through the cooperation of multiple components such as incomplete gears, driving gears, screw rods, and lifting cylinders, thereby ensuring that the filter plates can be cleaned regularly.

The present invention relates to a purification method, device and application for efficiently obtaining silane and disilane. The method adopts a single-stage multi-layer adsorption combined with a first-stage multi-layer separation tower distillation method to thoroughly remove impurities such as hydrogen, nitrogen, oxygen, ammonia, metals, etc. in a silane and disilane mixed gas, so that the total impurity content is less than 1ppm, and silane and disilane gases with a purity of 99.9999% or above are obtained at the same time. The device of the present invention mainly comprises a multi-layer adsorption tower (5), a regeneration gas storage tank (16), a multi-layer separation tower (23), a silane product storage tank (28) and a disilane product storage tank (35). The device of the present invention is suitable for the separation of two substances with a boiling point difference of 30°C or above, and is particularly suitable for the separation of silane and disilane. The present invention simultaneously obtains high-purity silane and disilane with a purity of 99.9999% or above. The method is easy to realize industrial production.

The invention discloses a preparation method of diiodosilane, and belongs to the technical field of material synthesis. The preparation method of diiodosilane comprises the following steps: adding a first iodine source and a second iodine source into a closed reactor in an inert gas atmosphere, and dissolving the first iodine source and the second iodine source in a solvent to form a uniform solution; and reducing the temperature, and adding liquid dichlorosilane. Raising the temperature to 30 to 80 DEG C and reacting; and after the reaction is finished, heating at reduced pressure, rectifying and purifying to obtain the high-purity electronic-grade diiodosilane. The first iodine source is lithium iodide, the second iodine source is at least one of sodium iodide or potassium iodide, and the solvent comprises at least one of acetonitrile, acetone, diethyl ether or ethanol. Lithium iodide and sodium iodide or potassium iodide are compounded, a specific solvent is matched, and a one-step method is used for testing, so that the input cost of raw materials is reduced, the experimental steps are simplified, the reaction rate of a reaction system can be improved, and the purity of a diiodosilane product is improved.

The invention relates to the technical field of hazardous waste resource utilization, in particular to a method for synergistically recovering valuable elements of overhaul slag and chromium-containing aluminum mud. The method comprises the following steps: mixing inorganic acid, chromium-containing aluminum mud and overhaul slag to obtain a decyanation material; carrying out a precipitation reaction on the decyanation material by using an alkaline component to obtain a precipitation material; mixing the first preheated silicon tetrachloride with the precipitation material to obtain first chlorinated flue gas and first chromium-containing chlorinated slag; mixing the second preheated silicon tetrachloride with the first chromium-containing chlorinated slag to obtain second chlorinated flue gas and second chromium-containing chlorinated slag; respectively separating and purifying the first chlorinated flue gas and the second chlorinated flue gas to obtain an aluminum-containing solid phase, an iron-containing solid phase and silicon tetrafluoride; and washing the second chromium-containing chloride slag to obtain a trivalent chromium-containing solution. According to the method, the removal rate of toxic elements of the overhaul slag and the chromium-containing aluminum mud can be synchronously increased to 99.95% or above, and the recovery rate of valuable elements such as aluminum, iron and chromium can be synchronously increased to 95% or above.

The invention provides a rectification system and a rectification method for trichlorosilane multi-tower differential pressure coupling. In the rectification system, a tower kettle outlet of a primary coarse distillation tower is communicated with a raw material inlet of a secondary coarse distillation tower; a tower top outlet of the crude distillation secondary tower is communicated with a first reboiler and a fourth reboiler respectively and then is communicated with a raw material inlet of the crude distillation tertiary tower; a tower top outlet of the crude distillation third-stage tower is communicated with a raw material inlet of the rectification first-stage tower, a tower kettle outlet of the rectification first-stage tower is communicated with a raw material inlet of the rectification second-stage tower, and a tower kettle outlet of the rectification second-stage tower is communicated with a raw material inlet of the crude distillation third-stage tower; a tower top outlet of the primary reduction tower is communicated with a fifth reboiler, and a tower top outlet of the secondary rectification tower is communicated with a third reboiler and then is subjected to a reduction process. According to the system, the reflux ratio of the primary crude distillation tower to the primary rectification tower can be reduced, the energy consumption in the trichlorosilane rectification process can be effectively saved, and the equipment investment and operation cost can be reduced.

The invention relates to a phosphorite wet processing method, and belongs to the technical field of chemical engineering. The phosphorite wet processing method comprises the following steps: A, phosphorite acid leaching: carrying out acidolysis leaching on a phosphorite raw material, and carrying out solid-liquid separation to obtain wet-process phosphoric acid; b, removing metal ions from wet-process phosphoric acid; and C, wet-process phosphoric acid defluorination: extracting fluosilicic acid in wet-process phosphoric acid at 10-70 DEG C by adopting a wet-process phosphoric acid defluorination extraction agent, and carrying out phase splitting to obtain defluorinated purified phosphoric acid and an organic phase loaded with fluosilicate. According to the invention, high-value utilization of low-grade phosphorite resources is realized. According to the method, impurities can be fully removed, the loss rate of phosphoric acid is low, the purity of the finally obtained phosphate product reaches 97% or above, the product quality is high, and the requirements of different fields for high-quality phosphate can be met. The method is simple in process, low in energy consumption and low in cost.

The invention relates to the technical field of polycrystalline silicon system catalysts, in particular to a preparation method of a polycrystalline silicon catalyst for new energy, which comprises the following steps: preparing mesoporous polystyrene microspheres; the preparation method comprises the following steps: dispersing mesoporous polystyrene microspheres in a metal salt solution for precipitation reaction, dispersing the obtained supported polystyrene microspheres in ethanol, then adding stronger ammonia water and tetraethyl orthosilicate for stirring reaction to obtain supported silicon dioxide microspheres; and calcining in a carbon monoxide atmosphere to prepare the polycrystalline silicon system catalyst. According to the preparation method, loading and precipitation of metal salt are carried out by dissolving a large number of mesopores in polystyrene microspheres, then the polystyrene microspheres loaded with metal precipitation particles are fixed by a sol-gel method, and the interior and the surface of the generated silicon dioxide microspheres are mingled with the loaded polystyrene microspheres; and high-temperature reduction calcination is carried out in the atmosphere of carbon monoxide, so that the prepared polycrystalline silicon system catalyst has relatively high tetrachlorosilane conversion rate and long-time use stability.

The invention discloses a catalyst for preparing trichlorosilane and a catalytic preparation method of trichlorosilane. The catalyst is prepared from the following components in percentage by mass: weighed copper nitrate, zinc nitrate, aluminum nitrate, lanthanum nitrate and the balance of a carrier, the preparation method comprises the following specific steps: S1, filling a catalyst; S2, purifying raw material gas; S3, reacting; and S4, separating and purifying a product, namely discharging a reacted gas product from an outlet of a reactor, and condensing through a condenser. In the prepared catalyst, the activity and selectivity of the catalyst are remarkably improved through the synergistic effect of the copper-zinc-aluminum composite oxide and the rare earth element lanthanum, the electronic structure and the surface acid-base property of the catalyst can be adjusted through doping of lanthanum, the reaction of silicon powder and hydrogen chloride is promoted, meanwhile, side reactions are inhibited, and the service life of the catalyst is prolonged. And the yield of trichlorosilane is improved.

The present invention discloses a method for separating nickel and iron from a nickel-iron alloy by chlorination roasting: (1) placing the nickel-iron alloy in a roasting furnace; (2) introducing a gaseous chlorinating agent into the roasting furnace for staged roasting to obtain roasting slag and a roasting gas phase; wherein the gaseous chlorinating agent is a mixture of chlorine and gaseous ferric chloride; and (3) condensing the roasting gas phase obtained in step (2) in stages to obtain solid ferric chloride and liquid silicon tetrachloride, respectively. The present invention controls the composition of the chlorinating agent during the chlorination roasting process to achieve selective and directional volatilization of iron into the gas phase while preventing nickel from being chlorinated. Thus, nickel and iron in the nickel-iron alloy can be separated in a single step, and the process flow is short.

The invention belongs to the technical field of trichlorosilane purification, and discloses an adsorbent for adsorbing phosphorus impurities in trichlorosilane and a preparation method and application thereof.The preparation method comprises the steps that activated carbon is immersed in a solution containing ammonium metavanadate and oxalic acid, ultrasonic treatment and drying are conducted, and a vanadium oxide / carbon material mixture is obtained; calcining the vanadium oxide / carbon material mixture, and performing reduction treatment to obtain the oxygen vacancy-rich activated carbon loaded vanadium oxide adsorbent. The activated carbon loaded vanadium oxide adsorbent rich in oxygen vacancies is prepared by using a dipping-calcining-reducing method, and phosphorus impurities are adsorbed and removed by using the interaction of the activated carbon loaded vanadium oxide adsorbent and PCl3. The active carbon loaded vanadium oxide adsorbent rich in oxygen vacancies interacts with PCl3, so that trace PCl3 can be efficiently removed.

The invention discloses a rectification and purification method of electronic-grade diiodosilane, and the rectification and purification method of the electronic-grade diiodosilane provided by the invention treats a diiodosilane crude product through rectification-adsorption combination, and some low-boiling-point substances can be removed through reduced-pressure rectification light component removal treatment. An organic solvent such as an aromatic organic solvent, hydrogen iodide, phenylsilane, monoiodobenzene silane; a polymer or macromolecular structure formed in the reaction process can be removed through vacuum distillation heavy component removal treatment; however, in the rectification process, benzene in a diiodosilane crude product can form an azeotrope with diiodosilane, so that a part of impurity benzene cannot be separated from diiodosilane all the time, and the residual benzene and metal impurities in diiodosilane are adsorbed and separated by adopting an adsorption treatment method, so that the electronic-grade diiodosilane is obtained.

A method for preparing diiodosilane, according to one aspect of the present invention, may comprise: a step of injecting an iodine source into a reaction vessel; a step of injecting an inert gas into the reaction vessel and purging same; a first synthesis step of adding a non-coordinating solvent and an ethylene diamine-based catalyst to the reaction vessel, and then stirring same to synthesize a reaction solution; a second synthesis step of maintaining the temperature inside the reaction vessel at a predetermined temperature, injecting dichlorosilane (DCS) into the reaction solution for a predetermined period of time, and then stirring same to increase the yield; a step of filtering out solids from the reaction solution and washing same; and a step of concentrating and reducing the pressure of the reaction filtrate obtained after the washing step, thereby recovering diiodosilane, and can prepare diiodosilane with high yield and / or high purity at low cost.

The invention provides an efficient trichlorosilane synthetic furnace and an intelligent temperature control method thereof. The efficient trichlorosilane synthetic furnace comprises a reactor body and an intelligent temperature control module, the reactor body comprises a shell; the shell comprises a conical area and a cylindrical area; the cylindrical area sequentially comprises a lower-section reaction area, a middle-section reaction area and an upper-section reaction area from bottom to top, and cooling devices are independently arranged on the outer sides of the reaction areas respectively; an internal part is arranged in the lower section reaction area; the intelligent temperature control module comprises a temperature sensor unit, an intelligent control unit and a flow adjusting unit. According to the invention, by arranging the internal part and the intelligent temperature control module, intelligent temperature control is realized, the temperature uniformity of each reaction area in the trichlorosilane synthetic furnace is effectively improved, and the conversion rate of trichlorosilane is greatly improved.

The invention relates to the technical field of trichlorosilane processing, in particular to equipment and method for removing boron and phosphorus impurities from trichlorosilane, the equipment comprises an adsorption column used for adsorbing trichlorosilane, the adsorption column is filled with an adsorbent, and the adsorbent is specially used for removing the boron and phosphorus impurities in trichlorosilane; the jacket is arranged on the outer wall of the adsorption column and is used for regulating and controlling the temperature in the adsorption column, a pipeline connected with the jacket is divided into an inlet part and an outlet part, and the inlet part and the outlet part are respectively provided with a regulating valve and a stop valve and are used for controlling a medium and flow which are introduced into the jacket. A multi-section adsorbent and a jacket temperature control system are adopted, so that boron and phosphorus impurities in trichlorosilane are efficiently removed. The design of the multi-section adsorbent allows different types of adsorbents to selectively adsorb specific impurities, so that the removal efficiency is improved. And each adsorbent can exert the optimal performance under different temperature and pressure conditions.

The invention relates to the technical field of semiconductor materials, in particular to a method for preparing a semiconductor material from high-purity quartz sand. The method comprises the following steps: firstly, grafting and modifying the surface of quartz sand through 3-aminopropyltriethoxysilane, complexing metal impurities by using amino functional groups, and improving the purity of a precursor from the source; secondly, hydrogen / deuterium gas pulse back-and-forth switching is adopted, surface hydrogen atom dynamics is regulated and controlled through the isotope effect, and an etching-nucleation synergistic window is created; and finally, through sequential alternate supply of silane and disilane, time separation of a weak bond etching period and a high-activity nucleation period is realized. The prepared semiconductor material shows excellent performance, and compared with a traditional method, the technical problem of low-temperature deposition of a high-quality semiconductor film is solved through full-process optimization from a material source to a deposition end.

The invention discloses a silicon tetrafluoride reduction process and application of sodium aluminum hydride wrapped by linear polymer resin to isolate outside air in the silicon tetrafluoride reduction process. The silicon tetrafluoride reduction process comprises the following steps: preparing a sodium aluminum hydride solution: measuring a required amount of sodium aluminum hydride which is wrapped by linear polymer resin to isolate outside air, and dissolving the sodium aluminum hydride in an organic solvent to obtain the sodium aluminum hydride solution; and reacting silicon tetrafluoride with the sodium aluminum hydride solution. The feeding safety of the sodium aluminum hydride can be guaranteed, the sodium aluminum hydride is prevented from being in contact with air to cause failure, the required sodium aluminum hydride can be accurately measured according to the designed amount, and the accuracy of the feeding ratio of the reaction raw materials in the silicon tetrafluoride reduction process is guaranteed.

The invention discloses a method for co-producing triphenylphosphine and silicon tetrachloride, which comprises the following steps: S1, mixing triphenylphosphine oxide with a solvent, heating to 90-110 DEG C, and dropwise adding trichlorosilane to carry out reduction reaction; the reaction pressure is controlled to be 0.12 to 0.20 Mpa absolute pressure; s2, the reaction temperature is kept not lower than 90 DEG C, preferably 90-110 DEG C, meanwhile, the system pressure is adjusted to be negative pressure, and the reaction continues for 0.5-3 h; and after the reaction is completed, rectifying and separating out silicon tetrachloride, adding water into the residual reaction liquid for quenching, filtering out insoluble substances, and removing the solvent to obtain the triphenylphosphine. According to the method, high-purity triphenylphosphine can be obtained with high yield, the electronic-grade silicon tetrachloride is co-produced, the generation of silicon dioxide is reduced, the gel coating problem of the silicon dioxide and the product loss are reduced, the post-treatment is more convenient, and the method is suitable for industrial production.

The invention belongs to the field of inorganic chemical industry, and particularly relates to a method and a system for efficiently utilizing a phosphate fertilizer byproduct, the method comprises the following steps: carrying out acidolysis on fluosilicic acid with the concentration of more than or equal to 45% wt and concentrated sulfuric acid to generate a mixed solution of silicon tetrafluoride gas and fluorosulfonic acid; the mass ratio of the fluosilicic acid to the concentrated sulfuric acid is controlled to be 1: (4-15); pyrolyzing the obtained fluorosulfonic acid to generate dilute sulphuric acid, hydrogen fluoride and water vapor, forming 98% concentrated sulphuric acid from part of dilute sulphuric acid and fuming sulphuric acid, drying hydrogen fluoride to obtain crude hydrogen fluoride gas, and condensing and rectifying to obtain anhydrous hydrogen fluoride; the rest dilute sulphuric acid is partially compounded and then returned for acidolysis, and the rest dilute sulphuric acid is used for producing white carbon black and flows back to a wet-process phosphoric acid system; and circularly absorbing the obtained silicon tetrafluoride gas by using secondary concentrated fluosilicic acid to obtain fluosilicic acid with the mass concentration of more than or equal to 45%, recycling the fluosilicic acid for acidolysis reaction, and modifying the concentrated by-product silicon dioxide to obtain the high-activity white carbon black. The problems of energy consumption and cost are solved, and efficient circulation and poly-generation of fluorine and silicon resources are achieved in the whole process.

The utility model provides a system for synthesizing trichlorosilane. The system for synthesizing trichlorosilane comprises a trichlorosilane synthesis reaction device, a first gas-solid separation unit, a first tail gas treatment unit, a silicon tetrachloride hydrogenation reaction device, a second gas-solid separation unit, a second tail gas treatment unit and a product separation and purification unit. According to the system, through the technological process of fusing the trichlorosilane synthesis reaction and the silicon tetrachloride hydrogenation reaction, efficient utilization of silicon powder, hydrogen and silicon tetrachloride is achieved, the investment and operation cost is saved, and meanwhile the raw material consumption is reduced.

The utility model discloses a slag slurry treatment system, which belongs to the technical field of slag slurry treatment in polycrystalline silicon production and comprises a transfer tank, a cryogenic stirring tank I, a coarse filter I, a fine filter I and a high-boiling-off tower which are sequentially connected, and the top of the high-boiling-off tower is connected with a cooler and then connected with a product liquid storage tank; the bottom of the high-boiling removal tower is sequentially connected with a cooling stirring tank, a cryogenic stirring tank II, a coarse filter II and a fine filter II through pipelines, a clear liquid outlet of the fine filter II is connected with a feeding hole of the high-boiling cracking device through a pipeline, and a light component outlet in the top of the high-boiling cracking device is connected with a material inlet of the high-boiling removal tower through a pipeline I; a slag discharging opening I in the bottom of the fine filter I is connected with a feeding opening I of the cryogenic stirring tank I through a pipeline II. The problems that in the prior art, when an evaporator or / and rotary drum equipment is / are adopted for treating slag generated in the cold hydrogenation process, the number of related equipment is large, pipelines are complex, the overhaul difficulty is large, and the silane recovery rate is low are solved.

The present invention relates to the technical field of hydrogen fluoride preparation, and particularly to a method for separating a mixed solution containing hydrogen fluoride and sulfuric acid. The separation method includes: A) Concentrated fluorosilicic acid and concentrated sulfuric acid react in a reaction device to generate silicon tetrafluoride gas and a sulfuric acid solution containing hydrogen fluoride; B) The first part of the sulfuric acid solution containing hydrogen fluoride is subjected to two-stage separation to obtain hydrogen fluoride gas; the second part of the sulfuric acid solution containing hydrogen fluoride is heated and recycled to the reaction device. The present invention adopts two-stage separation; another path of the sulfuric acid solution containing hydrogen fluoride led out after the main reaction enters the reaction device again after being heated, with relatively low energy consumption. Therefore, the separation method provided by the present invention separates hydrogen fluoride from the sulfuric acid solution with relatively low energy consumption and can reduce fluorine loss.

The utility model relates to a trichlorosilane adsorption tower in the technical field of adsorption equipment, which comprises a tower body, an air inlet pipe and an emptying pipe are arranged at the bottom of the tower body, and an exhaust pipe is arranged at the top of the tower body; the interior of the tower body is divided into a spraying area and an adsorption area from bottom to top, a spraying pipe is arranged at the top of the spraying area, a spherical gas distribution plate is arranged at the bottom of the spraying area, gas distribution holes are fully distributed in the gas distribution plate, and the gas inlet pipe is located below the gas distribution plate; the adsorption area comprises a filler layer, the filler layer is an activated carbon layer, a heat exchange assembly is arranged in the filler layer, the heat exchange assembly comprises a coiled pipe, and the coiled pipe is connected with a medium inlet pipe and a medium outlet pipe. According to the utility model, trichlorosilane can be subjected to impurity removal and purification after spraying and adsorption in sequence, the efficiency is high, and the effect is good; the temperature of the filler area can be flexibly adjusted according to needs, the adsorption effect can be improved, the filler can be purified, and the next adsorption effect is not affected.

The electronic-grade silane gas continuous production preparation system comprises a cold hydrogenation treatment device, an inlet of the cold hydrogenation treatment device is connected with a raw material supply system, and an outlet of the cold hydrogenation treatment device is connected with a cold hydrogenation rectifying tower through a pipeline. The cold hydrogenation rectifying tower is sequentially connected with the boron and phosphorus removal adsorption column, the first-stage disproportionator, the first tower, the second tower, the second-stage disproportionator, the third tower and the fourth tower through pipelines, and electronic-grade silane in the fourth tower is used for being conveyed to a silane tank area; the first tower is used for removing silicon tetrachloride produced after the disproportionation reaction of the first-stage disproportionator; the second tower is used for separating the extracted chlorosilane material; the third tower is used for separating silane from chlorosilane; and the fourth tower is used for discharging light impurities and heavy impurities and conveying gas-phase electronic-grade silane into a silane tank area. The device and the method realize continuous, efficient and high-purity production of the electronic-grade silane gas, and have the advantages of low energy consumption, low cost, thorough impurity removal and the like.

The invention relates to a method for selectively recovering germanium from germanium-containing smoke through flash boiling chlorination, belongs to the field of comprehensive recovery of scattered metals, and solves the problems of high acid consumption, high reaction temperature, high energy consumption, low germanium recovery rate and the like of a process for recovering germanium from germanium-containing smoke in the prior art. The invention relates to a method for selectively recovering germanium from germanium-containing smoke through flash boiling chlorination, which comprises the following steps: (1) chlorination: adding the germanium-containing smoke into a reactor, introducing chlorine into the reactor, and carrying out boiling chlorination reaction at a certain temperature; (2) dust collection: mixed flue gas obtained in the step (1) enters a cyclone separator along with airflow; (3) condensation: introducing the mixed flue gas subjected to dust collection treatment in the step (2) into a multi-stage condensation device to obtain a GeCl4 and SiCl4 liquid phase mixture and tail gas; and (4) refining: introducing the GeCl4 and SiCl4 liquid-phase mixture obtained in the step (3) into rectification equipment, and separating to obtain high-purity liquid-phase GeCl4. And the germanium in the germanium-containing smoke dust is efficiently recycled.

A method of making a trihalodisilane, the method comprising: combining a reductive effective amount of an alkylaluminum hydride, a halodisilane comprising at least 4 halogen atoms, and a solvent at a temperature <80° C. and reducing the halodisilane to form a reaction product mixture comprising a trihalodisilane and an alkylaluminum halide.

The present disclosure relates to a method or producing silicon tetrafluoride from fluorosilicic acid. In one implementation, a first stream comprising fluorosilicic acid and a second stream comprising sulfuric acid are reacted in a pressure regulator to produce an outgoing liquid stream comprising silicon tetrafluoride. The outgoing liquid is then fed into at least one separator which outputs at least one gas stream containing silicon tetrafluoride and at least one liquid stream. The at least one gas stream is fed into at least one additional separator which separates the at least one gas stream into at least one stream of purified silicon tetrafluoride gas. In some implementations, the at least one liquid stream is recycled back into the at least one separator.