32results about "Hydrogen phosphides" patented technology

The invention discloses a synthesis and purification method of electronic grade phosphorane, which relates to the technical field of phosphorane synthesis, and has the advantages that impurities such as metal oxides and carbides in a silicon carbide ceramic substrate are removed by selecting the silicon carbide ceramic substrate and performing high-temperature annealing treatment, so that the atomic arrangement of the substrate is more regular and ordered; compared with the prior art, the method has the advantages that the gallium phosphide crystal structure is more complete, so that the gallium phosphide crystal structure has higher structural stability, meanwhile, after impurities are removed, the interaction between the substrate and reactants in a high-temperature reaction environment is more controllable, the chemical stability is enhanced, a firm and reliable base is provided for growth of gallium phosphide crystals, and by adopting the ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, the yield of the gallium phosphide crystal is increased. The production of waste gas is reduced by utilizing the extremely low volatility of the gallium phosphide, and meanwhile, the reaction rate between hydrogen phosphide and hydrogen is accelerated by introducing glucose oxidase for catalytic reaction, so that the gallium phosphide crystal is promoted to efficiently and directionally grow on the silicon carbide ceramic substrate, and the product quality and the production efficiency are improved.

The utility model discloses a phosphine gas generating system. According to the technical scheme, the device comprises a material storage module, a material distribution module, a generation module, a processing module, a measurement and control module and a rack box body. According to the scheme provided by the utility model, the stored grain fumigation insect killing can be more effectively realized, the safety risk of dosing by personnel is completely avoided, the labor intensity is reduced, the workload is reduced, and the medicine can be stored for a long time as long as being placed in the bin once and can be released for multiple times according to the fumigation requirement; the generation opportunity and the dosage of the phosphine can be selected timely and reasonably, and the drug release concentration can be regulated and controlled according to actual conditions, so that the effective optimal CT value of the pest lethal concentration is achieved, and the dosage is reduced to the greatest extent; fumigating residues are subjected to innocent treatment, and residual gas is sent back to a grain pile, so that zero emission of poison gas is realized, the pesticide effect is fully utilized, and the environmental pollution is reduced; the whole fumigation operation and the circulation process are all carried out under the inner film of the granary pile, so that poison gas leakage is avoided, and grains are better protected.

The present invention discloses a process for recovering hydrogen and silane from HJT solar cell production waste gas, which belongs to the field of waste gas treatment technology and includes the following steps: the waste gas is sequentially input into a combined adsorption tower through a vacuum pump and a blower to remove the silane or phosphine components in the waste gas; the gas after adsorption is sent to a deep cold box to liquefy the silane or phosphine that has not been completely removed and the nitrogen in the mixed gas; and is transported to a gas-liquid separator, which separates hydrogen + a small amount of nitrogen. The high nitrogen liquid after separation refluxes in a heat exchanger and performs heat exchange with the waste gas flowing in. The refluxed high nitrogen liquid is vaporized and transported to a combined adsorption tower; step five, hydrogen purification and recovery. The present invention realizes the recovery of hydrogen and silane gas from the waste gas discharged from the production of HJT solar cells by rationally designing the process of waste gas treatment and proposing a new molecular sieve configuration, and reuses them after purification.

The utility model relates to the technical field of reaction kettles, and particularly discloses an electronic-grade phosphine synthesizing and refining device which comprises a reaction kettle, a conveying pipe and a communicating pipe are arranged at the top of the reaction kettle, the reaction kettle is communicated with a water inlet pipe, a discharging pipe is arranged at the bottom of the reaction kettle, and a rotating shaft is rotatably mounted on a bottom plate of the reaction kettle. The rotating shaft and the material conveying pipe are coaxially arranged, an umbrella-shaped flow guide table is arranged on the rotating shaft, the discharging end of the material conveying pipe faces the flow guide table, the rotating shaft is driven by a first driving source to rotate, the flow guide table is driven by the rotating shaft to rotate, and an electric air cylinder used for driving the flow guide table to ascend and descend is arranged in the rotating shaft. According to the invention, the flow guide table is arranged, so that the speed of phosphide falling into water from the edge of the flow guide table is slowed down, the generation speed of phosphine can be effectively controlled, the risk of sudden pressure increase caused by a large amount of gas generated due to too high speed is avoided, and the phosphide falls to the flow guide table and is dispersed around, so that the phosphide falls into water in a dispersed manner, and the contact surface area of the phosphide and the water is increased.

The system comprises a control pipeline assembly, a gas-liquid separation cold trap and a recovery cold tank, the gas-liquid separation cold trap is provided with a feeding pipe and a discharging pipe, the feeding pipe is communicated with the other end of the control pipeline assembly to receive the phosphine mixed gas in a torpedo car, and the discharging pipe is communicated with the control pipeline assembly to receive the phosphine mixed gas in the torpedo car; the gas-liquid separation cold trap is used for refrigerating the received phosphorane mixed gas in the torpedo car to obtain liquid phosphorane and non-condensable gas, the gas-liquid separation cold trap is used for liquefying phosphorane in the phosphorane mixed gas, the non-condensable gas is discharged through the exhaust pipeline, and meanwhile, the recovery bottle is used for recovering and storing the phosphorane. Meanwhile, spiral refrigeration channels are arranged outside the recovery bottle and the recovery cold tank, so that vortex can be generated when a gaseous refrigeration medium performs water bath refrigeration on the recovery bottle, the heat exchange refrigeration efficiency is improved, and the heat exchange efficiency of the recovery bottle is improved by utilizing the pressure of a gaseous refrigeration medium column on the inner wall of a first heat exchange channel on the recovery bottle; therefore, the recovery bottle is more stable during phosphorane recovery and does not shake.

The invention discloses a method and system for separating and recycling phosphorus and iron in ferrophosphorus waste residues, and relates to the technical field of solid waste utilization. The method comprises the following steps: crushing the ferrophosphorus waste residue, and heating and melting in an inert environment; the molten ferrophosphorus waste residues are sprayed into a reaction furnace in a blowing mode, the inert atmosphere is kept in the reaction furnace, and meanwhile water is introduced into the reaction furnace; the temperature of the reaction furnace is increased to 400-1000 DEG C, heat preservation is conducted for 10-60 min, the ferrophosphorus waste residues react with water, and hydrogen phosphide gas and iron oxide are obtained; and introducing the obtained phosphine gas into a collection device for collection, and collecting the obtained iron oxide from the bottom of the reaction furnace. The method disclosed by the invention has the advantages of simple process flow, small wastewater generation amount, high phosphorus element recovery rate and high phosphine purity.

The invention provides a phosphine preparation system, preparation method, equipment and medium, and relates to the technical field of industrial production control, the phosphine preparation system comprises a controller, a reaction unit, a water removal unit, a compressed air collection unit, a refining unit and a post-treatment unit; the controller is respectively connected with the reaction unit, the water removal unit, the compressed air collection unit, the refining unit and the post-treatment unit; a first feed port of the reaction unit is connected with a first discharge port of the water removal unit; a first discharging hole of the reaction unit is connected with a feeding hole of the water removal unit; a second discharging opening of the water removal unit is connected with a feeding opening of the collecting and air compressing unit; a first discharging hole of the compressed air collecting unit is connected with a first feeding hole of the refining unit; and a second discharge port of the collecting compressed air unit and a first discharge port of the refining unit are respectively connected with a first feed port and a second feed port of the post-treatment unit. The hydrogen phosphide preparation process can be intelligently controlled, the reaction efficiency is improved, and the obtained hydrogen phosphide is high in purity and stable in quality.

The utility model provides a production device of electronic-grade hydrogen phosphide. The production device comprises a full-automatic aluminum phosphide feeding system, a sulfuric acid metering tank, a constant-temperature reaction kettle, a purification cooling system, a heavy component removal purification column, a cold trap collection device, a light component removal purification column, a low-temperature filling system, an inert gas purging system, a vacuum system and a tail gas treatment system. The method comprises the following steps: quantitatively adding aluminum phosphide into a constant-temperature reaction kettle, slowly adding sulfuric acid into the constant-temperature reaction kettle through a metering tank, reacting to generate hydrogen phosphide gas, and removing particulate matters, acid mist, moisture, arsenic hydride, hydrogen sulfide, carbon dioxide, carbon monoxide, alkane, silane and ethylene in the hydrogen phosphide gas through pre-cooling, deep cooling, heavy component removal, cold trap and light component removal to obtain the electronic-grade hydrogen phosphide special gas with the purity of 99.9999%. And feeding tail gas generated in the purification process into a tail gas treatment system, absorbing the tail gas through a two-stage tower, and discharging the tail gas after reaching the standard.

The present invention discloses a phosphine gas purification apparatus, and particularly relates to phosphine gas purification equipment, the phosphine gas purification apparatus comprises a combined purification sieve arranged in a housing, the combined purification sieve comprises: a movable support member, the movable support member comprises a base and a sliding sleeve vertically sliding along the base; the movable filtering bins are slidably connected to the sliding sleeve in a linear array mode, and molecular sieves of different specifications are contained in the multiple movable filtering bins respectively. Molecular sieves of different specifications are placed in the multiple movable filtering bins respectively, during use, the multiple movable filtering bins are attached to one another to form a phosphine gas moving channel, different impurities in phosphine gas are separated, when the molecular sieves need to be replaced, only the whole combined purification sieve needs to be taken out, overall replacement is carried out, and the cost is reduced. The molecular sieves in the movable filtering bins do not need to be taken out one by one, and in the regeneration step of the molecular sieves, the sliding sleeves are driven to move, so that the tops are opened while the movable filtering bins are far away from one another, and the regenerated molecular sieves are conveniently heated.

The invention provides a phosphine automatic production method and device based on parallel reaction kettles, and relates to the technical field of phosphine preparation, and the phosphine automatic production method comprises the following steps: obtaining feeding proportions of different materials for producing phosphine and production plans of different reaction kettles; aiming at any reaction kettle, determining the feeding amount of each material in the reaction kettle according to the feeding proportion of different materials and the total feeding amount of the reaction kettle; controlling a feeding assembly to feed the materials into the reaction kettle and controlling a stirring assembly to stir the materials in the reaction kettle according to the feeding amount, feeding control parameters and operation control parameters of the materials in the reaction kettle, so that different materials react to generate hydrogen phosphide; monitoring real-time environment data in the reaction kettle; and according to the real-time environment data, adjusting the feeding control parameters and the operation control parameters to control the reaction of different materials until the reaction of the different materials is completed. According to the invention, the production process of phosphine can be automatically and intelligently controlled, and accurate control of feeding and operation in the reaction kettle is realized.

The invention provides a phosphine gas refining method and device, electronic equipment and a medium, relates to the field of phosphine refining, and systematically solves the three technical bottlenecks of difficulty in deep separation of multiple components, easiness in interruption of continuous production and poor manual control stability in the phosphine refining process. The high-efficiency separation of components with approximate boiling points is realized; a redundant adsorption system dynamic switching technology is adopted, so that the interruption risk of shutdown regeneration every 48 hours in the traditional process is eliminated; all-parameter automatic interlocking control is established, the heavy component carrying risk is reduced, and meanwhile, the safety and environmental friendliness are remarkably improved through nitrogen protection and waste gas directional treatment.

The invention discloses a modified organic metal ligand, a preparation method of the modified organic metal ligand, an adsorbent for removing methane and hydrogen phosphide in recycle hydrogen and a preparation method of the adsorbent, and the preparation method of the modified organic metal ligand comprises the following steps: 1) adding a first metal salt and terephthalic acid into a first solvent, and heating for reaction to generate an organic metal ligand MOF; and 2) separating the organic metal ligand MOF, mixing the organic metal ligand MOF with an N, N-dimethylformamide solution of 2-sulfonic acid group monosodium terephthalate, and reacting to generate the organic metal ligand MOF modified by the 2-sulfonic acid group terephthalic acid carboxyl. According to the invention, a metal organic framework material is firstly synthesized, then electrophilic functional groups, namely sulfonic groups and carboxyl groups, are introduced to modify the metal organic framework, and the process of introducing the electrophilic functional groups not only ensures that the pore channels and the structure of the metal organic framework are not changed, but also can strengthen the adsorption process of the adsorbent on hydrogen phosphide.

The invention discloses an adsorption column device and a process for continuously producing ultra-pure phosphorane through the adsorption column device, and relates to the technical field of phosphorane adsorption purification, the adsorption column device comprises an adsorption mechanism, the adsorption mechanism comprises a shell, an adsorption column assembly, an annular plate, a lantern ring, a wedge block, a limiting assembly and a transmission assembly, the adsorption column assembly is installed in the shell, and the annular plate is installed in the shell; the transmission assembly is installed on the surface of the shell, the annular plate is installed on the surfaces of the transmission assembly and the shell, and the lantern ring is arranged on the surface of the adsorption column assembly in a sleeving mode. According to the invention, phosphine can be subjected to multi-stage adsorption purification through the adsorption mechanism, and meanwhile, the adsorption column which is used for a long time can be quickly disassembled, assembled and replaced, so that high-pressure gas is not easily blocked in transmission when entering the adsorption column, and the operation efficiency of the whole production line is further improved; the filtering mechanism can be used for preliminarily filtering the phosphorane before entering the adsorption device, so that large impurities and particulate matters possibly entering the adsorption column are intercepted, the service life of the adsorption column is prolonged, and the purity of the prepared phosphorane is improved.

The invention discloses a method for producing hypophosphorous acid, comprising the following steps: 1) adding an ether-based organic solvent and distilled water into a reaction kettle, adding yellow phosphorus under a nitrogen flow, heating at normal pressure to melt the yellow phosphorus, and stirring at high speed to emulsify the yellow phosphorus; 2) dropwise adding a reactant into the reaction kettle to react with the yellow phosphorus until the solution is stirred into a transparent solution, and distilling the transparent solution product under reduced pressure to remove the solvent and the reactant to produce a crude product salt; 3) acidifying the crude product salt with hydrochloric acid to a pH of 2-3, and then extracting with n-butanol and water, and distilling off the organic phase to obtain hypophosphorous acid. The method uses an excess of water-soluble amine to change the disproportionation reaction of yellow phosphorus under alkaline conditions. Compared with traditional alkaline methods and ion exchange resin methods, the method can achieve recycling of raw materials, reduce costs, and is environmentally friendly.

The invention discloses a process for recovering hydrogen and silane from HJT solar cell production waste gas, and belongs to the technical field of waste gas treatment, and the process comprises the following steps: the waste gas is input into a combined adsorption tower through a vacuum pump and a fan in sequence, and silane or hydrogen phosphide in the waste gas is removed; the adsorbed gas is fed into a deep-cooling cold box, and silane or hydrogen phosphide which is not thoroughly removed and nitrogen in the mixed gas are liquefied; hydrogen and a small amount of nitrogen are separated by the gas-liquid separator, separated high-nitrogen liquid flows back in the heat exchanger and exchanges heat with waste gas flowing forwards, and the high-nitrogen liquid flowing back is vaporized and then conveyed to the combined adsorption tower; and 5, hydrogen purification and recovery. By reasonably designing the waste gas treatment process and providing a novel molecular sieve configuration, hydrogen and silane gas are recovered from the waste gas discharged in HJT solar cell production and are purified and reused.

The invention discloses a synthesis and purification device and a synthesis and purification method for electronic grade phosphorane, and relates to the technical field of phosphorane synthesis, the synthesis and purification device comprises a reaction kettle and a liquid nitrogen tank, the top of the reaction kettle is provided with an input pipeline, and the side face of the reaction kettle is connected with a condenser by arranging a pipeline. The synthesis and purification method of the electronic grade phosphorane comprises the following steps: injecting a raw material into a reaction kettle through an input pipeline, carrying out corresponding synthesis operation, starting a servo motor, driving a power sleeve to rotate clockwise, and matching with a hydraulic bin I, a turntable, a torsion spring, an extrusion block, a stress rod I, a half gear ring, a rotating rod I, a rotating rod II, a gear, a bevel gear I and a bevel gear II to synthesize the electronic grade phosphorane. The stirring plate rotates in the horizontal direction, and the mixing plate rotates in the vertical direction, so that the stirring effect of the device is improved, and the synthesis and purification efficiency of the device is improved.

The utility model discloses a phosphine gas reaction device for fumigating and killing tobacco pests, which is characterized by comprising a cylinder body, an atomizer is arranged at one end of the cylinder body, the atomizer is communicated with the cylinder body, a circulating pipe is arranged on the atomizer, one end of the circulating pipe is communicated with the atomizer, and the other end of the circulating pipe extends into the cylinder body; a feeding hole is formed in one end, far away from the atomizer, of the cylinder body, a detection device is arranged on one side of the feeding hole, and the detection device extends into the cylinder body and is fixedly connected with the cylinder body; a water outlet and an air outlet are formed in one side of the feeding hole; a fixing groove is formed in the lower end of the barrel, and a fixing seat is arranged at the lower end of the fixing groove; the reaction device is good in safety, adjustable in reaction rate, capable of accurately and quantitatively controlling the reaction rate, uniform in contact area and capable of reducing high temperature and improving the safety of equipment.

The invention relates to the field of phosphorane low-temperature water removal, in particular to a self-cleaning type low-temperature water removal tower for removing combined phosphorus, which comprises a tower body and a low-temperature pipe, a plurality of low-temperature pipes are arranged in the tower body in the vertical direction, cleaning units are arranged above and below each layer of low-temperature pipes, each cleaning unit comprises a coating shell rotating around the axis of the tower body, each coating shell is of a cylindrical structure, the axis of each coating shell is parallel to the radial direction of the tower body, an opening is formed in each coating shell and vertically faces the corresponding low-temperature pipe, and each coating shell is of a cylindrical structure. A shielding plate is rotationally arranged in the coating shell, the shielding plate is of an arc-shaped structure, the shielding plate can shield the opening in the rotating process, a cleaning plate rotating around the axis of the coating shell is further arranged in the coating shell, when the shielding plate shields the opening, the cleaning plate stops rotating, and when the shielding plate is withdrawn from the opening, the cleaning plate continuously rotates. According to the low-temperature pipe cleaning device, the low-temperature pipe is automatically cleaned, and the workload is reduced.

The application belongs to the field of organic phosphorus chemistry and phosphorus chemical industry, and particularly relates to a preparation method of phosphine. The method comprises the following steps: adding P4, Bu3SnH, a free radical initiator and an organic solvent into a test tube with a plug, sealing the test tube, wrapping the test tube with aluminum foil to avoid light, and stirring the test tube for a period of time; and then adding an acid into the reaction mixture to obtain phosphine. The application has mild reaction conditions, good safety and is suitable for industrial production.

The method comprises the following steps: mixing a phosphine raw material gas and an added azeotropic component in a mixing tower, feeding the mixture into an azeotropic tower, extracting the azeotropic component from the top of the azeotropic tower, extracting an azeotropic component from a side line of the azeotropic tower, feeding the azeotropic component into a product tower, extracting an electronic-grade phosphine product from the top of the product tower, and feeding the electronic-grade phosphine product into the product tower. Heavy components are extracted from a tower kettle of the product tower. Meanwhile, the invention discloses an efficient azeotropic distillation purification device for electronic-grade phosphine, which comprises a mixing tower, an azeotropic tower, an azeotropic tower condenser, an azeotropic tower reboiler, a product tower, a product tower condenser and a product tower reboiler. By adopting the efficient azeotropic distillation purification method and the efficient azeotropic distillation purification device for the electronic-grade phosphine, the purity of the processed phosphine product is greater than 99.99999%, the ethane content is less than 10ppb, and the ethylene content is less than 10ppb.

The utility model belongs to the field of semiconductor material manufacturing, and particularly relates to an arsenic hydride and phosphine adsorption tower, which comprises a tower body and a circulation port at the bottom of the tower body, a sealing box is mounted at the bottom of the tower body, the sealing box is hermetically connected with the circulation port through a filter cartridge, a cleaning groove is mounted in the sealing box, and a push block is mounted at the output end of the cleaning groove; an annular powerful magnet is installed on the push block, a synchronous sleeve is installed on the outer side of the filter cylinder in a sliding mode, an iron sheet is installed in the synchronous sleeve, and the iron sheet and the powerful magnet are attracted. According to the spraying circulating system, manganese crystals are prevented from entering the spraying circulating system in the mode that the filter cylinder is additionally arranged on the circulating opening, the cleaning groove is started to push the powerful magnet to slide in the filter cylinder, the powerful magnet on the push block can attract the powerful magnet in the synchronous sleeve, the push block can drive the synchronous sleeve to move synchronously, and therefore the manganese crystals are prevented from entering the spraying circulating system. And the synchronous sleeve moves to clean manganese crystals blocked on the outer wall of the filter cartridge, so that the circulating efficiency of the spraying liquid is improved.

The invention provides a method for producing electronic-grade phosphine by using sodium hypophosphite byproduct tail gas. The method comprises the working procedures of sodium hypophosphite tail gas purification, industrial phosphine pretreatment, anhydrous phosphine deep purification, phosphine catalytic decomposition, high-purity red phosphorus preparation and the like. The method is characterized by comprising the following steps: firstly, spraying and washing by-product tail gas generated in the production of sodium hypophosphite by using organic solvents such as carbon disulfide, then sufficiently filtering by using a sintered filter element with the precision of 1 micron, and carrying out two-stage cryogenic treatment to obtain industrial-grade hydrogen phosphide; performing four-stage adsorption on the industrial-grade phosphine to remove moisture, acetylene, ethylene and hydrogen sulfide, fully filtering by adopting a three-stage filter with the filtering precision of 1 micron, 10 nanometers and 3 nanometers, and removing particulate matters to obtain anhydrous phosphine; and finally, reducing the rest heavy components, light components and metal ions to below 10ppb through three-stage rectification to obtain the electronic-grade phosphine.

The application discloses a device for preparing electronic-grade sodium hypophosphite dearsenicated salt sodium salt, and belongs to the technical field of electronic chemical preparation. The device realizes the efficient dispersion of phosphine gas into micron-sized bubbles through a membrane dispersion reaction system, realizes the full and stable reaction of the phosphine gas with sodium hypochlorite solution, guarantees the high efficiency and uniformity of the main synthesis reaction from the source, and provides a composition-stable crude product liquid for subsequent continuous purification. Through a bypass arsenic removal unit integrated in a buffer adjustment system, the on-line circulation oxidation-precipitation-separation of arsenic impurities is realized without interrupting the main synthesis process, and the problem of the interruption of the synthesis route caused by the intermittent arsenic removal in the traditional process is solved. By arranging yellow phosphorus storage tanks in parallel and alternately working, the continuous and stable supply of the raw material yellow phosphorus to the phosphine reaction kettle is realized. The device ensures the long-term continuous and stable operation of the synthesis route and the high consistency of product batches, and is particularly suitable for the large-scale continuous production of electronic-grade sodium hypophosphite.

The utility model discloses a deliquescence type hydrogen phosphide gas generating device. According to the technical scheme, the phosphine generating device comprises a plurality of phosphine generating chambers, the phosphine generating chambers are fixed together through a top fixing plate and a bottom fixing plate, and each phosphine generating chamber comprises a keel mechanism playing a supporting role. A generating mechanism for generating phosphine gas, a material closing mechanism for preventing powder from falling and a powder collecting mechanism for collecting the powder are fixedly arranged in the keel mechanism, and a dust isolation mechanism for sealing the phosphine generating chamber is further arranged outside the keel mechanism. The scheme provided by the utility model is used for generating hydrogen phosphide gas, that is, the hydrogen phosphide gas is fully subjected to deliquescence reaction with moisture in flowing air, and residues are automatically fed into the treatment unit, so that the contact between people and medicines and the contact between the medicines and the environment are minimized, the harm of toxic gas in the environment is reduced, and the personal safety is ensured.

The utility model relates to the technical field of gas purification, and particularly discloses a phosphine gas purification device which comprises a tank body, a gas chamber and a purification cavity are arranged in the tank body, a drying layer and an adsorption filter layer are fixedly mounted in the purification cavity, the adsorption filter layer is positioned between the gas chamber and the drying layer, a plurality of gas outlets are formed in the top of the gas chamber in a penetrating manner, and the gas outlets are communicated with the gas chamber. A plurality of air outlets are formed in the tank body, the air outlets are communicated with the purification cavity and the air chamber, fan blades are rotationally arranged in the air chamber, the fan blades are driven by a transmission assembly to intermittently rotate and are in sliding fit with the air outlets, the fan blades are attached to a top plate of the air chamber, and an air inlet pipe and a return pipe are inserted into the air chamber; according to the gas purification device, gas can alternately enter the purification cavity through the gas outlet, and a gas outlet path is staggered, so that the gas which is reacted with a catalyst cannot be extruded out of the adsorption filter layer by the gas which subsequently enters the purification cavity, and sufficient time for the gas to react with the catalyst is ensured.

The present invention discloses a phosphine gas purification device, and specifically relates to a phosphine gas purification device, including a combined purification screen arranged in a shell, wherein the combined purification screen includes: a movable support, which includes a base and a sliding sleeve that slides vertically along the base; a mobile filter bin that is slidably connected to the sliding sleeve in a linear array, and multiple mobile filter bins respectively contain molecular sieves of different specifications. The invention places molecular sieves of different specifications in multiple mobile filter bins respectively. When in use, multiple mobile filter bins are fitted together to form a moving channel for phosphine gas, and different impurities in the phosphine gas are separated. When the molecular sieve needs to be replaced, it is only necessary to take out the entire combined purification screen and replace it as a whole, and it is not necessary to take out the molecular sieves in the mobile filter bins one by one. In the regeneration step of the molecular sieve, the sliding sleeve is driven to move, so as to move the mobile filter bins away from each other while opening the top to facilitate heating and regenerating the molecular sieve.

The utility model provides a device for producing ultrapure phosphorane through differential pressure thermal coupling rectification. A first condensation reflux device is arranged at the top of a first rectifying tower, and a first reboiler is arranged at the bottom of the first rectifying tower; a second condensation reflux device is arranged at the top of the second rectifying tower, and a second reboiler is arranged at the bottom; the top of the first rectifying tower is sequentially connected with a second reboiler, a first condensation reflux device and a second rectifying tower through a conveying pipeline; a third condensation reflux device is arranged at the top of the third rectifying tower, and a third reboiler is arranged at the bottom; the bottom of the second rectifying tower is connected with the third rectifying tower. A diaphragm compressor is arranged at the top of the third rectifying tower, the pressure of a product is increased, normal-temperature filling can be guaranteed, and meanwhile, an outlet of the diaphragm compressor is connected with a first reboiler B, so that heat of a gas phase at the top of the third rectifying tower is fully utilized. The system and the device can effectively remove impurities such as H2O, O2, H2, C2H6, CH4, CO, SiH4, C2H4 and AsH3 in industrial hydrogen phosphide to obtain electronic-grade hydrogen phosphide; meanwhile, the energy consumption in the operation process is reduced, and the annual operation cost is reduced.

The invention provides a method for preparing phosphorane by pyrolyzing sodium hypophosphite based on raw material pretreatment, the pretreatment method comprises the following steps: carrying out mechanical activation and dry granulation on sodium hypophosphite, and firstly, carrying out intermittent ball milling treatment on sodium hypophosphite powder in an inert atmosphere to form primary activated sodium hypophosphite; and then granulating by the steps of tabletting, crushing, screening and the like to obtain the granular sodium hypophosphite with the particle size of 0.8-1.2 mm, the porosity of 20-35% and the bulk density of 0.75-0.95 g / cm < 3 >. According to the pyrolysis method, on the basis of pretreatment, staged heating is carried out, a pyrolysis reaction is carried out under inert gas protection, the product phosphine is subjected to multi-stage condensation and low-temperature rectification purification, and then high-purity phosphine gas is obtained, the pyrolysis starting temperature can be remarkably reduced, the phosphine release rate and yield are increased, side reactions and impurity entrainment are reduced, and the method is suitable for industrial production. The method has the advantages of high raw material utilization rate, centralized and controllable pyrolysis reaction, high product purity and the like, and is suitable for efficient and safe preparation of phosphorane.

The invention belongs to the field of organic phosphorus chemistry and phosphorus chemical industry, and particularly relates to a preparation method of phosphorane. Comprising the following steps: adding P4, Bu3SnH, a free radical initiator and an organic solvent into a test tube with a plug, sealing the test tube, wrapping the test tube with an aluminum foil to keep away from light, and stirring to react for a period of time; and adding acid into the reaction mixture to obtain phosphorane. The method is mild in reaction condition, good in safety and suitable for industrial production.

The invention provides a method for producing ultrapure phosphine through differential pressure thermal coupling rectification, which comprises the following steps: industrial phosphine is fed from the middle of a first rectifying tower for purification, a tower top gas phase is condensed by a second reboiler and a first condensation reflux device, one part of the gas phase flows back into the first rectifying tower, and the other part of the gas phase enters a second rectifying tower; condensing and totally refluxing the tower top gas phase purified by the second rectifying tower into the second rectifying tower through a third reboiler and a second condensation reflux device, and extracting from the tower bottom of the second rectifying tower and conveying to a third rectifying tower; and after purification in the third rectifying tower, condensing and refluxing one part of a tower top gas phase into the third rectifying tower through a third condensing and refluxing device, and extracting the other part of the tower top gas phase as an electronic-grade hydrogen phosphide product. A diaphragm compressor is arranged at the top of the third rectifying tower, the product pressure is increased, normal-temperature filling can be guaranteed, and by means of the system and method, impurities such as H2O, O2, H2, C2H6, CH4, CO, SiH4, C2H4 and AsH3 in industrial phosphine can be effectively removed, and the electronic-grade phosphine is obtained.