155results about "Halogenated silanes" patented technology

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 application discloses a kind of feed dynamic regulation methods of synthesizing trichlorosilane, through multispectral synergistic detection, through the accurate calculation of key parameters such as hydroxyl inhibition factor, amorphous phase activity gain and metal impurity inhibition factor, the activity condition of silicon powder in fluidized bed can be accurately and real-time reflected, the technical bottleneck that silicon powder activity cannot be monitored on line is broken through, and then in industrial production, for the proportion of fluidized bed feed etc. Real-time regulation provides control basis.Through feed dynamic regulation mechanism, silicon powder feed rate, H2 / SiCl4 ratio and catalyst addition amount can be optimized in real time, ensure that silicon powder is always in high activity state, promote the reaction to proceed, improve trichlorosilane yield and purity, solve the problem that traditional fixed regulation mode and silicon powder dynamic activity do not match, and then improve regulation accuracy.

This invention provides a system and method for removing high and low boiling points in polysilicon production. The system includes a first distillation column comprising a top rectifying section, a bottom stripping section, and a separation section between the rectifying and stripping sections, all of which are sequentially interconnected. The separation section includes a pre-fractionation section and a main fractionation section arranged side-by-side but not interconnected. The main fractionation section includes, from top to bottom, a first main fractionation section and a second main fractionation section that are interconnected. The pre-fractionation section has a low-boiling material inlet, the stripping section has a bottom outlet, and the first main fractionation section has a first outlet. The outlet of the disproportionation fixed-bed reactor is connected to the low-boiling material inlet. The second distillation column has a high-boiling material inlet and a top outlet, and the bottom outlet of the stripping section is connected to the high-boiling material inlet. The first outlet and the top outlet of the second distillation column are respectively connected to an adsorption column.

The application relates to a method for synthesizing and refining electronic-grade hexachloroethyldisilane, and specifically, trichlorosilane raw material is mixed with protective gas into a raw material buffer tank, a mixed gas obtained through the mixing is subjected to a catalytic synthesis reaction under the irradiation of an ultraviolet light source, a product obtained through the reaction is subjected to condensation separation, gaseous trichloromethane returns to the raw material buffer tank to continuously participate in the synthesis reaction, the mixed liquid in the cold trap is warmed and vaporized, hexachloroethyldisilane is obtained through two-step refining, and the purity of the product hexachloroethyldisilane can reach the electronic grade. The application takes trichlorosilane as the initial raw material, the price of the raw material is low; the photo-catalysis is used as the synthesis process, the synthesis process is simple, the reaction yield is high, energy is saved, and the environment is protected; the two-step method is used for refining and purifying the product, the depth of the refining and the efficiency of the refining are high, large-scale production is suitable, the monopoly of foreign enterprises is broken, and the application has important significance.

The invention provides a method for recovering tail gas generated in production of carbon nanotubes. The method comprises the following steps: compression: introducing tail gas containing methane and hydrogen into a compressor for pressurization; first-stage separation: the pressurized tail gas is introduced into a first-stage membrane separator for separation, methane and first-stage tail gas are obtained, and the main component of the first-stage tail gas is hydrogen; and second-stage separation: introducing the first-stage tail gas into a second-stage membrane separator for separation to obtain hydrogen and second-stage tail gas containing hydrogen. Through two-stage membrane separation, methane and hydrogen are recovered, the methane separated in the first stage can return to the continuous furnace to be continuously used as a raw material for producing carbon nanotubes, and the hydrogen separated in the second stage can be used for producing trichlorosilane, so that the recovery and utilization of resources can be realized.

A halotrisilane preparation method may include providing a reactant that contains halotrisilane including M halogen atoms (where, M may be a natural number from 2 to 8), reducing the halotrisilane in the reactant by using a mixed reducing agent that includes a first reducing agent represented by Formula 1-1 and a second reducing agent represented by Formula 2-1, and obtaining a product that contains the reduced halotrisilane that includes N halogen atoms, where N may be a natural number from 1 to 7 and where N<M.(RA)a-Al-Hb[Formula⁢ 1-1]In Formula 1-1 above, RA may represent an alkyl group, a and b each may be either 1 or 2, and a+b=3.(RS)p-Sn-Hq[Formula⁢ 2-1]In Formula 2-1 above, RS may represent an alkyl group or an aryl group, p and q each independently may be a natural number from 1 to 3, and p+q=4.

The utility model provides an impurity removal system for preparing disproportionation reaction silane gas, which comprises a dehydrogenation tower (1) for preparing silane, and further comprises a side production pipeline (5) arranged in the middle of the side of the dehydrogenation tower (1), the other end of the side production pipeline (5) is in fluid connection with a circulating water condenser (6), and the other end of the circulating water condenser (6) is in fluid connection with the dehydrogenation tower (1). A liquid phase outlet of the circulating water condenser (6) is in fluid connection with a buffer tank (7), and the buffer tank (7) is in fluid connection with a silane reaction tower (9) through a pump (8). According to the device, the content of heavy phosphorus impurities in silane gas can be reduced, and the quality of the product silane gas is improved; the dehydrogenation tower is transformed to reduce the influence of phosphorus impurities on the activity of the catalyst in the reaction tower.

A production system, production method and application of general-purpose high-purity chemicals are disclosed. The production system includes a raw material tank, and an adsorption system, a crystallizer, a first light-impurity removal tower, a first heavy-impurity removal tower, a second light-impurity removal tower, a motorized tower, a second heavy-impurity removal tower, a vapor permeation device, a membrane separation system and a filling system connected with the raw material tank in sequence. The high-purity chemicals produced by the above system have high purity and excellent quality. Compared with the prior art, the system and method designed by the present disclosure have more pertinence, integrity, progressiveness, energy-saving, precision, high safety coefficient and great industrial promotion value. And the products produced are of excellent quality, which can meet the standards applied to the manufacturing of integrated circuit electronic components and meet the high-end needs of the semiconductor industry market.

The utility model provides a device for improving the conversion rate of cold hydrogenated silicon powder. The device comprises an external dust remover (2) in fluid connection with a top discharge hole (13) of a fluidized bed (1) in a cold hydrogenation production process; a bottom outlet of the external dust remover (2) is in fluid connection with a top inlet of the reactor (3); a top outlet of the reactor (3) is in fluid connection with a top inlet of the chlorosilane storage tank (5) after sequentially passing through a first heat exchange channel of the heat exchanger (4) and a condensation channel of the condenser (6); a top outlet of the chlorosilane storage tank (5) is connected with a second heat exchange channel outlet of the heat exchanger (4) in parallel and then is in fluid connection with a bottom inlet of the reactor (3).

The invention belongs to the technical field of aluminum smelting solid hazardous waste recycling, and particularly relates to a recycling method of aluminum oxide-rich complex electrolyte hazardous waste. According to the method, the complex aluminum electrolyte hazardous waste, aluminum salt and silicon-containing oxide are mixed and then subjected to segmented roasting-leaching treatment, fluorine in the electrolyte is converted into aluminum fluoride firstly and then converted into silicon tetrafluoride gas, separation of fluorine and aluminum and separation of gas and solid are achieved, and sodium and lithium elements are converted into soluble salt and further separated and recycled. According to the process, collaborative recovery and high-value utilization of various valuable elements in the complex aluminum electrolyte hazardous waste are achieved. The whole technological process is environment-friendly, toxic and harmful gas emission is avoided, secondary solid waste residues are not generated, the method has the advantages of being simple in process, high in recovery rate, high in product additional value and the like, and a feasible technical scheme is provided for resource utilization of the aluminum electrolysis solid waste.

The invention belongs to the technical field of cold hydrogenation synthesis, and particularly relates to a treatment method of slag slurry generated in a cold hydrogenation synthesis process, the slag slurry generated in the cold hydrogenation process is sequentially subjected to primary filtration, secondary diatomite precoating filtration, drying evaporation and rectification purification treatment, so that the recovery rate of chlorosilane (mainly silicon tetrachloride) is up to 99%, and the recovery rate of chlorosilane is up to 99%. Resource waste and environmental pollution are avoided, meanwhile, an alkali washing tank is omitted, the process is simplified, and energy consumption is reduced; in addition, physical separation (filtration, drying and rectification) and solid slag neutralization are adopted in the treatment method, no wastewater is generated, a matched sewage treatment system is not needed, and the environmental protection cost and energy consumption are remarkably reduced.

This invention relates to a pyrolysis method for fluorosilicates, belonging to the field of fluorochemical technology. The pyrolysis method includes the following steps: mixing fluorosilicates and alkali metal fluorides in a molar ratio of 1:(0.5-4) and granulating to obtain composite particles; then, the composite particles are subjected to static pyrolysis to prepare SiF4; the particle size of the composite particles is less than 10 mm. This invention mixes and granulates fluorosilicates and alkali metal fluorides. At high temperatures, the alkali metal fluorides achieve trace solid dissolution with fluorosilicates, increasing the melting point of fluorosilicates. During granulation, the alkali metal fluorides are uniformly distributed around the fluorosilicate particles. Since the melting point of the alkali metal fluorides is higher than that of fluorosilicates, the fluorosilicate particles reaching their melting point are blocked by the alkali metal fluorides, preventing localized melting and improving pyrolysis efficiency. Furthermore, the alkali metal fluorides are pyrolysis products of fluorosilicates and, as additives, do not introduce other impurities.

This invention provides a system and method for removing high and low boiling points in polysilicon production. The system includes a first distillation column comprising a top rectifying section, a bottom stripping section, and a separation section between the rectifying and stripping sections, all of which are sequentially interconnected. The separation section includes a pre-fractionation section and a main fractionation section arranged side-by-side but not interconnected. The main fractionation section includes, from top to bottom, a first main fractionation section and a second main fractionation section that are interconnected. The pre-fractionation section has a low-boiling material inlet, the stripping section has a bottom outlet, and the first main fractionation section has a first outlet. The outlet of the disproportionation fixed-bed reactor is connected to the low-boiling material inlet. The second distillation column has a high-boiling material inlet and a top outlet, and the bottom outlet of the stripping section is connected to the high-boiling material inlet. The first outlet and the top outlet of the second distillation column are respectively connected to an adsorption column.

The invention provides a preparation method of a silicon-copper composite catalyst, which comprises the following steps: pretreatment: uniformly mixing a copper-containing raw material and excessive silicon powder, putting the mixture into a reaction container, and feeding the reaction container into a heating furnace; the heating furnace is controlled to be heated to 1400-1500 DEG C, the silicon powder and the copper-containing raw materials are melted and react, and a mixture of Cu3Si and the remaining silicon powder is obtained; after the reaction step is completed, a mixture of Cu3Si and silicon powder is taken out of the heating furnace, naturally cooled to the room temperature and solidified into a blocky structure, and the blocky structure is crushed into powder; wherein the copper-containing raw material is elemental copper, copper-containing metal salt or copper oxide. According to the preparation method of the silicon-copper composite catalyst provided by the invention, the silicon powder and the copper-containing raw material are subjected to direct melting reaction, and the preparation is simple. And the silicon powder is controlled to be excessive based on cost consideration, so that the raw material silicon powder for producing the catalyst can also be used as a raw material in a cold hydrogenation process, and the excessive raw material silicon powder and the product Cu3Si do not need to be separated.

A system and method for separating aluminum trichloride from cold-hydrogenated silicon tetrachloride includes a pressure-reducing tank, a condenser, a first extraction tank, a second extraction tank, a clear liquid filter, and a clear liquid tank. The system is characterized by: a silicon tetrachloride inlet pipe at the top of the pressure-reducing tank; the bottom of the pressure-reducing tank being connected to the first and second extraction tanks via pipes; the bottoms of the first and second extraction tanks being connected to a dryer via pipes; the side walls of the first and second extraction tanks being connected to the clear liquid filter via pipes; the tops of the first and second extraction tanks being connected to the condenser via pipes; the bottom of the condenser having a liquid outlet pipe connected to the top of the clear liquid tank; and the bottom of the clear liquid tank having a silicon tetrachloride recovery pipe; and the clear liquid filter being connected to the liquid outlet pipe via a pipe. This invention improves the clogging situation of the entire cold hydrogenation system, solves the problem of long-term operation of the cold hydrogenation system, and reduces the equipment failure rate.

The invention discloses a trichlorosilane deep rectification composite impurity removal process, and belongs to the technical field of polycrystalline silicon production raw material purification. According to the process, deep purification of crude trichlorosilane is achieved through the steps of pre-protection and primary adsorption, directional rectification enrichment of methyl dichlorosilane narrow fractions, concentration, mixing with silicon tetrachloride, catalytic reaction rectification conversion, differential pressure thermal coupling rectification purification, double-tank parallel deep purification, tail gas treatment and the like. According to the method, the impurity methyl dichlorosilane difficult to remove is precisely separated through side extraction, the impurity methyl dichlorosilane is converted into a component easy to separate through a catalytic reaction, and the boron and phosphorus impurities are deeply removed in combination with differential pressure thermal coupling energy saving and double-tank alternate adsorption. The process can efficiently remove moisture, metals and key impurities boron and phosphorus, obviously improves the purity of the trichlorosilane product, realizes gradient utilization of energy and hydrogen circulation, and has the advantages of high purity, low energy consumption and continuous production.

The invention relates to a method for recovering silicon in the form of silicon tetrachloride, in which biochar having a silicon content of at least 1% by weight, expressed as% by weight of elemental silicon, is reacted with elemental chlorine at a temperature of 350 to 900 DEG C and the formed silicon tetrachloride is separated from the exhaust gas stream, preferably by condensation.

The utility model provides a polycrystalline silicon cold hydrogenation system and aims to solve the technical problem that a pipe orifice is easily blocked due to a vertical mounting mode of a liquid level meter and a flushing pipe orifice in the existing polycrystalline silicon cold hydrogenation system. The system comprises a washing tower and a plurality of horizontally arranged washing branch pipes, wherein a tower tray group is arranged in the washing tower; the washing branch pipe is connected with a connecting pipeline of the washing tower and is used for conveying chlorosilane washing liquid; the connecting pipeline is positioned below the tray group and is provided with a first control valve; a liquid level meter is horizontally mounted on a connecting pipeline between the first control valve and the flushing branch pipe; and a second control valve and a check valve are arranged on the flushing branch pipe. Through the design that the liquid level meter is horizontally installed and flushing liquid horizontally enters the connecting pipeline, it can be guaranteed that the flushing liquid can generate enough flushing force, sediments are effectively removed, the damage risk of a membrane is reduced, the service life of the liquid level meter is prolonged, meanwhile, the unblocking effect of the flushing liquid is improved, and frequent unblocking operation caused by blocking can be avoided.

The invention relates to a process for the production of chlorosilanes by hydrochlorination of silicon in a fixed bed, in which particulate agglomerates of secondary silicon are added to the fixed bed, a process for the production of the particulate agglomerates, the particulate agglomerates themselves, and their use as a starting material in the hydrochlorination of silicon. The object of the invention was to provide a fixed-bed process for the production of chlorosilanes using secondary silicon, in which the secondary silicon can be handled with less effort. A fundamental idea of ​​the process according to the invention is to use particulate secondary silicon with a larger particle size. More precisely, the median particle size distribution of the secondary silicon D50S should be between 0.1 mm and 5 mm. Water glass is used as a binder within the agglomerates.

The utility model discloses a structure of a funnel cap bearing plate of a hydrogenation furnace, and aims to solve the problems of penetrability damage and sealing failure caused by silicon powder erosion in an abutted seam area of a bearing plate in the prior art. The structure comprises a splicing type bearing plate, a supporting cross beam and a sealing assembly, an air inlet pipe is vertically arranged on the bearing plate, an air outlet of the air inlet pipe is sleeved with an air cap, and inclined air holes are formed in the side wall of the air cap to optimize airflow distribution. The lower portion of a bearing plate abutted seam is welded to a supporting cross beam through an angle steel sealing plate, and thermal expansion stress dispersion and high-precision sealing are achieved in combination with the design of a sealing rubber strip and a sliding groove clamping rail. In addition, flow guide pipes are inserted into the air holes, and the airflow guide stability is enhanced through threaded connection. Through structural optimization and process improvement, the sealing performance and the erosion resistance are remarkably improved, silicon powder deposition and airflow scouring damage are reduced, the service life of equipment is prolonged, meanwhile, the maintenance process is simplified, and the sealing device is suitable for various hydrogenation furnace working conditions and has high practicability and popularization value.

The application discloses a system and method for separating crude organosilicon monomers by six-tower heat integration rectification, and is characterized by comprising a high-removing tower, a low-removing tower, a light separation tower, a hydrogen-containing tower, a trimethyl tower, a dimethyl tower, a separator and a mixer; the high-removing tower is connected with a preheater through a pipeline; a gas phase outlet at the top of the high-removing tower is connected with an inlet of the separator through a first heat exchanger; one outlet of the separator is connected with an inlet of the mixer through a second heat exchanger; another outlet of the separator is connected with the inlet of the mixer through a third heat exchanger; an outlet of the mixer is connected with the high-removing tower and the low-removing tower respectively; the low-removing tower is connected with the light separation tower; the low-removing tower is connected with the dimethyl tower through a preheater; a bottom product outlet of the dimethyl tower is connected with an auxiliary reboiler and the third heat exchanger respectively; the light separation tower is connected with the hydrogen-containing tower through the first heat exchanger; the hydrogen-containing tower is connected with the trimethyl tower through the second heat exchanger; and the method has the advantages of realizing high-purity separation of crude organosilicon monomers and greatly reducing energy consumption in production.

The invention provides a recovery method and a recovery system for electronic grade dichlorosilane and helium, and belongs to the field of tail gas treatment.The recovery method comprises the steps that tail gas containing dichlorosilane and helium is filtered, and then solid particle impurities are removed; performing multistage gas-liquid separation and condensation on the tail gas from which the solid particle impurities are removed by utilizing the difference between boiling points of dichlorosilane and helium, so as to obtain liquid dichlorosilane and primarily separated gaseous helium; after the primarily separated gaseous helium is subjected to multi-stage adsorption, residual organic impurities and inorganic impurities in the helium are removed; and separating and purifying the impurity-removed helium through a multi-stage membrane, and removing residual impurities to obtain the high-purity helium. Harmless treatment of tail gas can be achieved, tail gas emission is reduced to the maximum extent, and energy consumption and environmental pollution are reduced; meanwhile, useful substances in the tail gas are recycled, and helium is purified to reach the purity standard which can be used for producing electronic-grade products again, so that the aim of recycling resources is fulfilled, the production cost is reduced, and the economic benefits of enterprises are improved.

The invention relates to a method for trace analytical detection and quantification of compounds of boron and / or aluminium in a gas or liquid flow containing at least one chlorosilane, comprising the steps of a) removing a sample from the gas flow and mixing with an inert gas to form a gaseous sample or removing a liquid sample from the liquid flow, wherein the liquid sample is mixed with an inert gas in an evaporator unit and evaporated to form a gaseous sample; b) transferring the gaseous sample obtained in step a) into the reaction chamber of a mass spectrometer, wherein electrons generated in an ion source by means of plasma discharge react with the chlorosilane to form chloride ion species and wherein the chloride ion species react with the compounds of boron and / or aluminum via chemical ionization to form boron and / or aluminum chloride ion species; c) separating and detecting the boron and / or aluminum chloride ion species.

The utility model relates to the technical field of chemical gas recovery, and provides a device for separating trichlorosilane tail gas and co-producing fumed silica, which adopts a combined process to treat the trichlorosilane tail gas and is provided with a rectification separation seat provided with a low-temperature cold energy recovery mechanism. Hydrogen, hydrogen chloride and chlorosilane in the tail gas are separated step by step through the rectification separation assembly, the hydrogen chloride and the chlorosilane are directly conveyed to the combustion assembly, the purity of the hydrogen chloride is recycled to the trichlorosilane tail gas treatment assembly, recycling after separation is achieved, and the purposes of further saving energy consumption and improving the purity are achieved; a fumed silica combustion furnace suitable for low-boiling-point chlorosilane is adopted, so that the chlorosilane and hydrogen are mixed and combusted to generate fumed silica and hydrogen chloride, and the fumed silica can be directly discharged through a fumed silica discharge pipe; and the generated hydrogen chloride is recovered into the trichlorosilane tail gas treatment seat through a second hydrogen chloride return pipe, and closed-loop utilization is realized.

The application provides a device and a method for preparing trichlorosilane, and the device comprises a trichlorosilane synthesis system, a dry dust removal system, a wet dust removal system, a heavy component removal and purification system and a slag slurry treatment system; the trichlorosilane synthesis system comprises a trichlorosilane reactor; the dry dust removal system comprises a cyclone separator; the wet dust removal system comprises a spray tower, a reboiler, a heat exchanger and a first condenser; and the heavy component removal and purification system comprises a heavy component removal tower and a carbon adsorption tower. The device combines the pneumatic conveying of silicon powder in the entire polysilicon industry, and combines the energy-saving technology of condensing mixed gas as the liquid phase of spray washing by using the heat exchanger, the energy-saving means of bidirectional extraction of trichlorosilane and tetrachlorosilane components, and the technology of slag slurry concentration and recovery, so that the effective resource integration of the entire system is achieved, the technical effects of low energy consumption and cyclic reuse are fully realized, and a high-purity trichlorosilane production system which can run independently and self-compensate is created.

The utility model provides a high-boiling cracking system for polycrystalline silicon production. The high-boiling cracking system comprises: a cracking generator comprising a plurality of raw material input ends and a product output end; the pressure relief pipeline is communicated with the cracking generator; and the filtering device is arranged on the pressure relief pipeline and is used for filtering the gas flowing through the pressure relief pipeline. According to the high-boiling cracking system for polycrystalline silicon production disclosed by the utility model, during pressure relief, gas flowing through the pressure relief pipeline is filtered through the filtering device, and a liquid material is prevented from being discharged along with the gas, so that the pressure relief pipeline is prevented from being blocked, the influence on the production process is reduced, and the production efficiency is improved.

The invention relates to the technical field of polycrystalline silicon preparation, and discloses an integrated multi-stage adsorption and impurity removal treatment device for polycrystalline silicon preparation, which comprises a primary crude distillation tower, a first adsorption assembly, a second adsorption assembly, a primary rectification tower, a secondary rectification tower and a cold hydrogenation device, the raw material chlorosilane in the cold hydrogenation device enters a primary crude distillation tower for primary separation, light impurities in the raw material chlorosilane in the primary crude distillation tower are extracted from the top and enter a second adsorption assembly, and the second adsorption assembly adsorbs and removes the light impurities through a renewable adsorbent and then enters the cold hydrogenation device. According to the invention, a series integrated design of adsorption-rectification coupling-deep purification is adopted, the first adsorption assembly and the second adsorption assembly are additionally arranged to form a stage treatment unit, and through differential adsorption configuration of double adsorption columns, precise step-by-step removal of two impurities of boron and phosphorus is realized, the overall impurity removal efficiency is greatly improved, and the product quality is improved. Meanwhile, running rectification equipment is reduced, and equipment investment and production energy consumption are reduced.

The invention discloses cold hydrogenation chlorosilane online detection equipment and method, and a cold hydrogenation production system and method. The equipment comprises a primary pretreatment unit, a secondary pretreatment unit, a heat preservation unit and a detection unit, the primary pretreatment unit comprises a sample inlet pipeline, a silicon powder filter and a pressure reducing valve; the heat preservation unit comprises a heat tracing piece and a heat tracing box body, and the secondary pretreatment unit is arranged in the heat tracing box body and comprises a first pipeline, a first coil pipe, a first filter, a vaporizer and an adsorber; and the detection unit is communicated with the gas outlet of the adsorber. According to the method, silicon powder and metal chloride impurities such as aluminum chloride and ferric chloride in the cold hydrogenated chlorosilane can be removed before detection, so that online detection on the components and concentration of the cold hydrogenated chlorosilane is effectively realized, and a real-time basis is provided for adjusting the raw material ratio and reaction conditions in the cold hydrogenated production process; therefore, the raw material ratio and the reaction conditions in the cold hydrogenation production process are adjusted in time according to the online detection result, and the conversion rate of the cold hydrogenation reaction is improved.

The present application provides a method for fluorine separation and recovery from phosphate rock enhanced with a microbubble coupled silicon additive, which includes: mixing the phosphate rock, phosphoric acid, and an active silicon additive, and subjecting the mixture to reaction to obtain a slurry; subjecting the slurry to microbubble generation treatment to obtain a microbubble slurry, and subjecting the microbubble slurry to recycling and returning to the reaction, where a released volatile fluoride is recovered; and after completing the reaction, a defluorinated slurry is obtained; and subjecting the obtained defluorinated slurry to acid-decomposition reaction and then solid-liquid separation to obtain phosphoric acid and phosphogypsum. In the method provided by the present application, a synergistic effect of microbubbles and the active silicon additive is used in the phosphoric acid acid-decomposition of phosphate rock, enhancing the fluorine impurities in phosphate rock to convert into volatile fluoride SiF4 and HF, achieving the highly efficient separation and recovery of fluorine, and a recovery rate of fluorine reaches 43.9% or more; moreover, the fluorine impurities are separated from the source in the acid decomposition of phosphate rock, thereby preventing fluorine from entering the subsequent wet phosphoric acid process.

The invention relates to the field of silane chlorides, and particularly discloses a monochlorosilane preparation method which comprises the following steps: S100, preparation of a catalyst: loading the catalyst on a porous carrier to obtain an immobilized catalyst; s200, preparation of monochlorosilane: taking silane and hydrogen chloride as raw materials, and carrying out hydrochlorination reaction by adopting an immobilized catalyst to obtain monochlorosilane; wherein the catalyst comprises palladium salt. According to the preparation method of the monochlorosilane by using the immobilized catalytic system, the mild selective chlorination reaction is realized, so that the selectivity and yield of the monochlorosilane are remarkably improved, meanwhile, the safety risk is reduced, and the preparation method is suitable for continuous industrial production.