CN209128044U - Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely - Google Patents

Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely Download PDF

Info

Publication number
CN209128044U
CN209128044U CN201820599360.1U CN201820599360U CN209128044U CN 209128044 U CN209128044 U CN 209128044U CN 201820599360 U CN201820599360 U CN 201820599360U CN 209128044 U CN209128044 U CN 209128044U
Authority
CN
China
Prior art keywords
ammonia
silicomethane
tower
connects
silicon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201820599360.1U
Other languages
Chinese (zh)
Inventor
谢嵩岳
李腾智
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Taiwan Special Product Chemistry Limited-Liability Co
Original Assignee
Taiwan Special Product Chemistry Limited-Liability Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Taiwan Special Product Chemistry Limited-Liability Co filed Critical Taiwan Special Product Chemistry Limited-Liability Co
Priority to CN201820599360.1U priority Critical patent/CN209128044U/en
Application granted granted Critical
Publication of CN209128044U publication Critical patent/CN209128044U/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/52Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Landscapes

  • Silicon Compounds (AREA)

Abstract

The utility model provides a kind of catalyst and promotes the system that silane reaction generates and its process byproducts recycle entirely, wherein: the utility model with design newly developed isolate and purify system and technology carries out the silane of reaction generation and mixes separating for gas and the solid raw material that participates in reacting, again by silicomethane by carrying out low temperature gas-liquid separation according to its physical characteristic in mixed gas, and the removal of the recycling of ammonia raw material and the purifying of silicomethane and its impurity in silicomethane is carried out using the silicomethane fractionating system, and the silicon ethane and ammonia raw material through gas-liquid separation also carry out fractionation purifying with silicon ethane Distallation systm, developed unique catalyst is cooperated to carry out the promotion of silicon ethane conversion using technology, and implement the equipment of new feeding mode and exploitation, and by recovery ammonia to be used again as reaction raw materials, the production capacity and purification process for making silicomethane and silicon ethane whereby are stablized.

Description

Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely
Technical field
The utility model system about a kind of silane process system, it is espespecially a kind of with catalyst promoted silane reaction generate and its The system that process byproducts recycle entirely.
Background technique
Nowadays, Si-Mg alloy method is industrialization process known to one of which, is partly led for producing silicomethane and silicon ethane etc. The synthetic method of body special gas raw material, it is known to use Si-Mg alloy method carries out the production of silane, the selecting response of silicon ethane Rate is too low and progressing greatly and reducing with cost with high purity silicon methane production technology, and reaction slag charge stores caused environment The problem of influence and the complicated and energy consume big processing routine, therefore are difficult to meet with the technique of Si-Mg alloy method production silane Economic benefit.Thus the Si-Mg alloy method of shortcoming, improvement gradually develops, and promotes the selection in the reaction production of silicon ethane Rate, yield and purity, but its handling problems for reacting slag charge still obstruction of production of silane method thus, and in production technology according to So there are many derivatives of technology relevant issues, as silane is because of the operating condition of technical process and oxidation reaction generates dioxy due to environment SiClx powder or crystallization lead to the reduction of equipment effectiveness and production efficiency and tear clear maintenance frequency increase open.Therefore the utility model The advanced production technology and device systems to be designed and developed makes up and improves the Si-Mg alloy method using improvement for producing silane Technology and technologic defect, and then developing is perfect high purity silane production method and system.
Utility model content
Utility model aims to solve above-mentioned missings of the existing technology, and it is anti-to provide a kind of catalyst promotion silane It should generate and its system that process byproducts recycle entirely, promote the reactivity of raw material and reduce reaction system and hindered by solid powder The influence of plug problem promotes the production capacity of silicon ethane by the silane reaction build environment of optimization.
One silane reaction system includes that a magnesium silicide inhales powder bucket, a magnesium silicide automatic feeder, jacket type reaction Slot, a condenser and an air driven pump, and the magnesium silicide automatic feeder is connected to magnesium silicide suction powder bucket and the jacket type is anti- Answer between slot, and the jacket type reactive tank is installed with a blender, and the top of the jacket type reactive tank connect the condenser and The bottom end of jacket type reactive tank connects one end of the air driven pump, and the other end of the air driven pump connects a slag charge dashpot, a gas-liquid Separating tank is connected to the condenser, and the silicomethane by the upper end of gas-liquid separation slot connection one for storing vaporization silicomethane is temporary Slot is deposited, and gas-liquid separation slot connection one is for storing the silicon ethane temporary tank of liquefaction silicon ethane and liquefied ammonia, silicon ethane distillation System includes a desiliconization ethane tower, an ammonia purification column and a silicon ethane purification column, which connects the desiliconization second Alkane tower, which connects the ammonia purification column, and the desiliconization ethane tower lower end connects the one of the silicon ethane purification column End, the other end of the silicon ethane purification column is connected with a liquefaction silicon ethane buffer barrel, and the ammonia purification column and the silicon ethane purify The separated ammonia of tower is stored in a liquefied ammonia dashpot, and the liquefied ammonia dashpot connects the jacket type reactive tank, and the ammonia purification column Upper end connects the silicomethane temporary tank.
Wherein, which is sequentially connected with one second condenser and a third condenser, and with third condenser company Connect the gas-liquid separation slot.
Wherein, a filter is installed between the condenser and second condenser.
Wherein, which is connected with a silicomethane fractionating system, which includes a silicon Methane recovery tower, a silicomethane molecular sieve and a silicomethane purification column, the silicomethane temporary tank are connected to the silicomethane recovery tower, And the silicomethane recovery tower upper end connects the silicomethane molecular sieve and silicomethane recovery tower lower end connects the liquefied ammonia dashpot, and by The silicomethane molecular sieve connects the silicomethane purification column, and the silicomethane purification column connects a liquefaction silicomethane buffer barrel.
Wherein, which uses interior outer double-layer structure, by the liquefaction silicomethane buffer barrel outer layer in true Empty shape is simultaneously arranged with a ring body coil pipe, and the liquefaction silicomethane buffer barrel is connected with a vaporizer, and the vaporizer is connected to one Finished product pressuring machine.
Wherein, which is serially connected with a centrifugal filter, an ammonia spirit dashpot, a magnesium hydroxide in order Filter and an ammonium hydroxide buffer barrel, and the centrifugal filter and the magnesium hydroxide filter are connected with a dry milling dress simultaneously It sets, and a high-pressure molding brick making system is connected with the drying milling device.
Wherein, which is connected with an ammonia separation recovery system, and the ammonia separation recovery system is with a recovery ammonia tower The ammonium hydroxide buffer barrel is connected, and an ammonia rectifying column is connected with by the recovery ammonia tower upper end, and the ammonia rectifying column connects one in tower top Ammonia Raw material pail, and the ammonia rectifying column is connected to the ammonium hydroxide buffer barrel in tower bottom, the another recovery ammonia tower is connected to a multiple-effect by tower bottom Vapo(u)rization system, and the multi-effect evaporation system is connected with a drying machine and a recycle-water dashpot, and the ammonia Raw material pail, the drying machine The jacket type reactive tank is connected to the recycle-water dashpot.
It wherein further include having an exhaust treatment system, which is connected to the silicon with multiple exhaust emissions pipelines Alkane reaction system, the silicon ethane Distallation systm, the silicomethane fractionating system, the slag charge dashpot, the ammonia separation recovery system and The multi-effect evaporation system, the exhaust treatment system include a scrubbing tower, a tail gas fluid-tight buffer barrel, a high-temperature oxydation device and one Filter plant, and the tail gas fluid-tight buffer barrel is connected between the tower top of the scrubbing tower and the high-temperature oxydation device one end, and with this The other end of high-temperature oxydation device connects the filter plant, and the scrubbing tower is separately connected to the ammonia spirit dashpot.
First main purpose of the utility model is that production of silane mode is using the Si-Mg alloy method of improvement, and cooperation is Unique catalyst of exploitation carries out the promotion of silicon ethane conversion using technology, and implements the equipment of new feeding mode and exploitation, It is influenced with promoting the reactivity of raw material and reducing reaction system by solid powder obstructing problem, and with the production operation of improvement Technology effectively controls and optimizes the environment of silane reaction generation, to promote the production capacity of silicon ethane.
Second main purpose of the utility model is, isolates and purifies system and technology progress instead by design newly developed The silane that should generate mixes the separation of gas with the solid raw material for participating in reacting, then by silicomethane by mix in gas according to its physical characteristic into Row low temperature gas-liquid separation, and using the silicomethane fractionating system carry out silicomethane in ammonia raw material recycling and silicomethane purifying and The removal of its impurity, then as the storage of silicomethane in a manner of cryogenic vacuum, and silicon ethane and ammonia raw material through gas-liquid separation Also fractionation purifying is carried out with silicon ethane Distallation systm, and by recovery ammonia to use again as reaction raw materials, makes silicomethane whereby And the production capacity and purification process of silicon ethane are stablized, and production cost can be effectively reduced.
The third main purpose of the utility model is, generated slag charge is reacted after silane reaction, with addition Enter water as solvent, part slag charge content is enable to be converted into salts substances and be dissolved in ammonium hydroxide, and is able to after pulpous state fluid does Continuous separation and recovery disposition, and newly-designed separation method is adopted, the separation of solid and liquid of pulpous state slag charge is carried out with centrifugal separation technology, and make Solid product after separation is after drying as the exploitation of brick-making raw material.And the fluid of liquid keeps its conversion anti-by addition ammonia Should be recyclable salt ammonia spirit, reuse Distallation systm carry out ammonium chloride saline solution, ammonia and water isolate and purify and Recycling.Ammonium chloride saline solution then reuses the processing and drying that high-efficiency evaporating system carries out moisture removal, and raw as silane Reaction raw materials recycling is produced to use.By means of so that storing the influence for environment and the consuming of production cost so that slag charge is effectively reduced.
4th main purpose of the utility model is that tail (useless) gas that technique generates uniformly collects through exhaust emissions pipeline Exhaust treatment system is imported, absorbs to remove and recycle by the ammonia in tail gas by ammonia absorption removal technology and does saline solution addition Liquid use, and other silicone hydride waste gas then by exhaust treatment system carry out oxidation reaction processing, be converted into not dangerous property gas or Slag charge is disposed, to reduce the pollution and harm of environment.
Detailed description of the invention
Fig. 1 is the structure and flow chart of the silicon ethane technique of the utility model.
Fig. 2 is the structure and flow chart of the silicomethane technique of the utility model.
Fig. 3 is the structural schematic diagram of the liquefaction silicomethane dashpot of the utility model.
Fig. 4 is the structure and flow chart of the slag charge recovery process of the utility model.
Fig. 5 is the structure and flow chart of the solvent recovery technology from vent gas of the utility model.
In figure:
Silane reaction system --- -11;
Magnesium silicide inhales powder bucket --- and -111;
Magnesium silicide automatic feeder -112;
Jacket type reactive tank --- -113;
Condenser --- --- -114;
Air driven pump --- --- -115;
Blender --- --- -116;
Second condenser --- -- 117;
Third condenser --- -- 118;
Filter --- --- -119;
Gas-liquid separation slot --- -- 12;
Silicon ethane Distallation systm --- 13;
Desiliconization ethane tower --- -- 131;
Ammonia purification column --- --- 132;
Silicon ethane purification column --- -133;
Liquefied ammonia dashpot --- -- 134;
Slag charge dashpot --- -- 14;
Silicon ethane temporary tank --- -15;
Liquefy silicon ethane buffer barrel -- and 16;
Steel cylinder --- --- -- 17;
Silicomethane temporary tank --- -21;
Silicomethane fractionating system --- 22;
Silicomethane recovery tower --- -221;
Silicomethane molecular sieve --- -222;
Silicomethane purification column --- -223;
Liquefy silicomethane buffer barrel -- and 23;
Vaporizer --- --- -231;
Ring body coil pipe --- --- 232;
Finished product pressuring machine --- -- 24;
Steel cylinder --- --- -- 25;
Tank car --- --- -- 26;
Centrifugal filter --- -- 31;
Ammonia spirit dashpot --- 32;
Magnesium hydroxide filter --- 33;
Ammonium hydroxide buffer barrel --- -- 34;
Dry milling device --- -35;
High-pressure molding brick making system -- 351;
Ammonia separation recovery system --- 36;
Recovery ammonia tower --- --- 361;
Ammonia rectifying column --- --- 362;
Ammonia Raw material pail --- --- 37;
Multi-effect evaporation system --- -38;
Drying machine --- --- -381;
Recycle-water dashpot --- -39;
Exhaust emissions pipeline --- -41;
Exhaust treatment system --- -42;
Scrubbing tower --- --- -421;
Tail gas fluid-tight buffer barrel --- 422;
High-temperature oxydation device --- -- 423;
Filter plant --- --- 424;
Magnesium silicide and catalyst --- -51;
Ammonium chloride --- --- -52;
Recycle-water --- --- -53.
Specific embodiment
The utility model is described in further detail in the following with reference to the drawings and specific embodiments, so that those skilled in the art The utility model can be better understood and can be practiced, but illustrated embodiment is not as the restriction to the utility model.
A kind of catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely comprising have: a silane is anti- System 11, a gas-liquid separation slot 12 and a silicon ethane Distallation systm 13 are answered, a silane reaction system 11 includes that a magnesium silicide is inhaled Powder bucket 111, a magnesium silicide automatic feeder 112, a jacket type reactive tank 113, a condenser 114 and an air driven pump 115, should Magnesium silicide inhales powder bucket 111 and stores magnesium silicide (Mg with anaerobic state2Si) and catalyst 51, anaerobic state are closed laggard in loading Row is vacuumized replaces with nitrogen, and the mixed proportion of the catalyst is the 15% to 30% of magnesium silicide, and the catalyst is by 20 ~ 50wt%'s The metal powder of silicon powder (Si) and 50 ~ 80wt% constitute bimetallic compound, and alkali metal group, alkali can be used in metal powder material therein The metallic element in transition metal also can be used in the metallic element of earth metal race, such as the member in iron (Fe) or the A of III A ~ VI group The alloys such as element, and the magnesium silicide automatic feeder 112 is connected to the magnesium silicide and inhales powder bucket 111 and the jacket type reactive tank 113 Between, and the jacket type reactive tank 113 is installed with a blender 116, and the top of the jacket type reactive tank 113 connects the condensation The bottom end of device 114 and jacket type reactive tank 113 connects one end of the air driven pump 115, and the other end of the air driven pump 115 connects a slag Expect dashpot 14, and the jacket type reactive tank 113 first puts into 52 (NH of ammonium chloride4Cl) powder, and carry out closed nitrogen displacement and Deaeration in condenser operation, then import pure ammonia (NH3) condensation of -30 DEG C of refrigerants of control forms liquid ammonia afterwards, and starts the blender 116 Being pre-dissolved for ammonium chloride and liquid ammonia is carried out, so that chloride leach is formed ammonia and chloride salt ions in liquid ammonia, and this is maintained to stir Mix headroom of the continuous running of machine 116 into slot after reaction, disperse in reaction process to avoid powder it is uneven or because It reacts and solidifies agglomeration and cause to block, and magnesium silicide and catalyst are put into fixed rate by the magnesium silicide automatic feeder 112 51 enter the jacket type reactive tank 113, i.e. magnesium silicide and 51 powder of catalyst cooperates flow steady with the fixed rate of 0 ~ 150 kg/h Surely a little liquefied ammonia controlled fifty-fifty puts into the jacket type reactive tank 113 and is reacted with ammonium chloride, borrowed as carrying fluid This, can avoid magnesium silicide powder and cause to splash when contacting with liquefied ammonia in slot, and make that powder is attached in pipeline or cell wall is gradually led The obstruction of pipeline is caused, the process that silane generates belongs to exothermic reaction, therefore must continue to carry out thermal energy with -30 DEG C of refrigerants in reaction process Removal, to be maintained reaction temperature, more in reaction process, liquid ammonia also can by reaction generate thermal energy and vapour Change, and drift about the jacket type reactive tank 113 out with the silane of generation, lead to the reduction of reactivity or terminate the progress of reaction, is The amount for maintaining liquid ammonia in reaction process will be carried out the condensation of ammonia by the condenser 114 with -30 DEG C of refrigerants, make it again The jacket type reactive tank 113 is flowed back in liquefaction, and triggering reaction whereby generates silicomethane (SiH4) and hydrogen (H2) mix gas and via this 114 output of condenser, the silicon ethane of most of institute's output, therefore can be by the condensers because its physical characteristic is similar to the characteristic of ammonia 114 condensation and liquefy return in the jacket type reactive tank 113 again, be thus after silane reaction, must by participate in react Liquid ammonia and recycled as far as possible contained in silicon ethane therein, therefore convert the heating agent of the refrigerant to 90 DEG C in the condenser 114, Enable the liquid ammonia and the stable vaporization that heated up by boiling of silicon ethane in the jacket type reactive tank 113, whereby with 90 °C of heating agents Liquefied ammonia and silicon ethane (Si after assisted reaction2H6) carry out boiling and recycled via the condenser 114, wherein reaction raw materials make It is usually standard by magnesium silicide weight with ratio, and with magnesium silicide 1: ammonium chloride 3 ~ 6: 9 ~ 12 taken amount of liquid ammonia, and the reaction equation Are as follows:
Silicomethane reaction equation is following (main reaction):
Mg2Si(s) + 4NH4Cl(s) +8NH3(l) →SiH4(g) +2(MgCl2‧6NH3) (s)
Silicon ethane reaction equation is following (side reaction):
2Mg2Si(s)+8NH4Cl(s)+16NH3(l) →Si2H6(g)+4(MgCl2‧6NH3)(s)+ H2(g)
And the slag charge after reacting deposits in the slag charge dashpot 14 by the air driven pump 115 discharge, is discharged into the slag charge dashpot 14 slag charge makes the hydrogen-oxygen for being partially converted into indissoluble prior to water (or recycle-water 53) stirring is added in the jacket type reactive tank 113 Change magnesium solid-state powder and be dissolved in salt product therein, wherein the jacket type reactive tank 113 is rushed after slag charge emptying with nitrogen It blows, vacuumize and the heating of 90 DEG C of heating agents carries out cleaning and effective moisture removal in the slot of the jacket type reactive tank 113, to keep away Exempting from moisture influences the silane generated in next reaction process and thermonatrite environment oxidation reaction and forms silica, improves whereby Silane reaction rate, a gas-liquid separation slot 12 are connected to the condenser 114, which is sequentially connected with one second condenser 117 and a third condenser 118, and the gas-liquid separation slot 12 is connected with the third condenser 118, utilize each boiling point substance temperature Different physical characteristics carries out preliminary silane separation, then with 2 ~ 7 kg/cm2Level pressure sequentially import second condenser 117 It is condensed with -30 DEG C of condensation progress with the third condenser 118 with -75 DEG C, that is, can avoid silicon ethane and drift in gas phase again It is mixed with gaseous silicomethane and hydrogen, separation is carried out in the gas-liquid separation equipment and forms liquid-state silicon ethane and liquefied ammonia, with And gaseous silicomethane and hydrogen, a filter 119 is installed between the condenser 114 and second condenser 117, due to this Jacket type reactive tank 113, can companion in the silicomethane that reaction process generates mixes gas and boiling goes out after reaction ammonia and silicon ethane It is greater than 3 ~ 100 μm of powder on a small quantity through raw material carried by differential-pressure airflow or slag charge powder, utilizing the filter 119 to intercept Grain, by the upper end connection one of the gas-liquid separation slot 12 for storing the silicomethane temporary tank 21 of vaporization silicomethane, and the gas-liquid point From the connection of slot 12 one for storing the silicon ethane temporary tank 15 of liquefaction silicon ethane and liquefied ammonia, a silicon ethane Distallation systm 13 includes One desiliconization ethane tower 131, an ammonia purification column 132 and a silicon ethane purification column 133, the silicon ethane temporary tank 15 connect the desiliconization second Alkane tower 131, which connects the ammonia purification column 132, and 131 lower end of desiliconization ethane tower connects the silicon second One end of alkane purification column 133, and the other end of the silicon ethane purification column 133 is connected with a liquefaction silicon ethane buffer barrel 16, this is de- Silicon ethane tower 131 is with 18 ~ 24kg/cm of pressure2With 25 °C to 70 °C conditions of temperature by ammonia separation to the ammonia purification column 132, this point From liquid ammonia amount be 58 ~ 67wt%, while by silicon ethane separation to the silicon ethane purification column 133, and in the ammonia purification column 132 End connects the silicomethane temporary tank 21, which is back to the silicomethane with a small amount of silicomethane of temperature difference separation and keeps in Slot 21, and the silicon ethane is further purified with 30 °C to 100 °C of temperature in the silicon ethane purification column 133, and will purifying silicon ethane storage It is stored in the liquefaction silicon ethane buffer barrel 16, the selecting response rate of silicon ethane is enable to reach 5 ~ 25vol% whereby, the liquefaction silicon ethane Silicon ethane stored by buffer barrel 16 up to 4N8 (99.998%) purity, when silicon ethane fills demand, by vacuum and low temperature- 75 DEG C of condensations enable silicon ethane to be filled into an at least steel cylinder 17 by the liquefaction silicon ethane buffer barrel 16, also can be cold with identical vacuum Solidifying technology carry out a small amount of silicon ethane purifying and micro impure gas removal, and the ammonia purification column 132 and the silicon ethane purify The separated ammonia of tower 133 is stored in a liquefied ammonia dashpot 134, and the liquefied ammonia dashpot 134 connects the jacket type reactive tank 113, The ammonia of recycling is imported the jacket type reactive tank 113 by the liquefied ammonia dashpot 134 again to reuse, and then its life is effectively reduced Produce cost.
Another branch line of the utility model carries out the purifying operation of silicomethane, then please sees it as shown in Figure 2, and the silicomethane is temporary Slot 21 is connected with a silicomethane fractionating system 22, which includes a silicomethane recovery tower 221, a silicon first Alkane molecular sieve 222 and a silicomethane purification column 223,221 upper end of silicomethane recovery tower connect the silicomethane molecular sieve 222 and silicon 221 lower end of methane recovery tower connects the liquefied ammonia dashpot 134, and connects the silicomethane purification column by the silicomethane molecular sieve 222 223, the silicomethane recovery tower 221 is with 8 ~ 15 kg/cm of pressure2Most ammonia is fractionated with -60 °C ~ 40 DEG C of transformation temperature and is stored up It deposits to the liquefied ammonia dashpot 134, i.e., is the characteristic of relatively heavy substance using ammonia, by the silicomethane recovery tower 221 after being fractionated Tower bottom output and be delivered to the ammonia dashpot 134 and recycled, and the silicomethane gases isolated still contain about 2 ~ A small amount of ammonia ingredient of 10wt%, and the silicomethane gases fractionated out and a small amount of ammonia are again by the silicomethane molecular sieve 222 of the 3A ~ 5A The gas of Adsorption ammonia and other impurities, wherein the silicomethane molecular sieve 222 can be carried out heating to provide the pumping after switching The regeneration that adsorbent is removed in vacuo uses, then silicomethane is imported silicomethane purification column 223 and low with -160 °C to -50 DEG C Contained hydrogen is removed separation by temperature, and purifying silicomethane is allowed to be stored in a liquefaction silicomethane buffer barrel 23.The liquefaction silicomethane is slow The silicomethane stored by bucket 23 is rushed up to the purity of 6N (99.9999%), and the liquefaction silicomethane buffers 23 barrels and uses inside and outside bilayer Structure (shown in cooperation Fig. 3), stores liquefaction silicomethane by 23 internal layer of liquefaction silicomethane buffer barrel, and the liquefaction silicomethane buffers 23 outer layers of bucket are in vacuum shape and are arranged with the ring body coil pipe 232 of a circulation refrigerant, using the ring body coil pipe 232 circulation refrigerant up to- 50 DEG C of temperature control and voltage-controlled, and use refrigerant as the condensation of silicomethane when needing to use, and the liquefaction silicomethane buffer barrel 23 are connected with a vaporizer 231, and the vaporizer 231 is connected to a finished product pressuring machine 24, when silicomethane fills demand, allow silicon Methane imports the vaporizer 231 and is delivered to the finished product pressuring machine 24 with the control that -30 DEG C of refrigerants carry out regime flows, and by The finished product pressuring machine 24 is forced into 100 ~ 160 kg/cm2Pressure silicomethane is filled at least a steel cylinder 25 or at least a slot In vehicle 26, facilitate to carry out filling transport whereby.
Another branch line of the utility model carries out the recycling operation of slag charge, then please sees it as shown in Figure 4, the slag charge dashpot 14 It is serially connected with a centrifugal filter 31, an ammonia spirit dashpot 32, a magnesium hydroxide filter 33 and ammonium hydroxide buffering in order Bucket 34, and the centrifugal filter 31 and the magnesium hydroxide filter 33 are connected with a dry milling device 35 simultaneously, and dry with this Dry milling device 35 is connected with a high-pressure molding brick making system 351, and when operation is discharged into the slag charge of the slag charge dashpot 14 prior to this In jacket type reactive tank 113 plus water (or recycle-water 53) stirring, make the magnesium hydroxide solid-state powder for being partially converted into indissoluble and molten Pulpous state slag charge is flowed into the centrifugal filter in salt product therein, and under the uninterrupted stirring of the slag charge dashpot 14 31, slag charge can more effectively be carried out reacting the soluble salt of generation with water, enables the solid powder/particle of generation that can be uniformly distributed and keep away Exempt to precipitate, recycle the de- liquid that rotates of the centrifugal filter 31, i.e., the centrifugal filter 31 with the revolving speed of 300 ~ 1000 rpm into The de- liquid of row slag charge, and with the interception of the filter material of 200 ~ 400 mesh progress solid powder, so that the liquid part of slag charge is flow to the ammonium hydroxide Solution delays art slot 32, and the solid-state slag charge is drained in a manner of striking off to this when the centrifugal filter 31 forms a suitable thickness Dry milling device 35, and the drying milling device 35 with electric heating cooperation auger carry out solid-state slag charge heat drying and The disengaging of ammonia, and drain into the high-pressure molding brick making system 351 as the raw material of brickmaking, it also can be directly as the use of exhaust gas desulfurization Agent, and the ammonium hydroxide that recycling obtains is added in the ammonia spirit dashpot 32, and so that the magnesium chloride in solution is reacted generation and be converted into Ammonium chloride and magnesium hydroxide powder, then magnesium hydroxide powder chips with side-by-side is filtered with 1 ~ 30 μm of precision via the magnesium hydroxide filter 33 It lets out to the drying milling device 35, and the discharge regime is by powder using nitrogen by blowing off on the centrifugal filter 31, and with Powder is emitted into the drying milling device 35 by its gravity, is avoided solid-state powder from entering the ammonium hydroxide buffer barrel 34, is only deposited ammonium hydroxide Enter the ammonium hydroxide buffer barrel 34.The ammonium hydroxide buffer barrel 34 is connected with an ammonia separation recovery system 36, the ammonia separation recovery system 36 with One recovery ammonia tower 361 connects the ammonium hydroxide buffer barrel 34, and is connected with an ammonia rectifying column 362 by 361 upper end of recovery ammonia tower, and should Ammonia rectifying column 362 connects an ammonia Raw material pail 37 in tower top, and the ammonia rectifying column 362 is connected to the ammonium hydroxide buffer barrel 34 in tower bottom, And the recovery ammonia tower 361 is with 0 ~ 5 kg/cm2Pressure and 50 °C ~ 145 DEG C of temperature carry out ammonium chloride solution and ammonia spirit Separation, separated ammonia concn are that 10 ~ 30wt% belongs to relatively light materials, make ammonia spirit by the tower of the recovery ammonia tower 361 Top is emitted into the ammonia rectifying column 362, and carries out the purifying of ammonia and water with -30 °C ~ 130 DEG C of temperature in the ammonia rectifying column 362 Separation, purified ammonia can reach technical grade 98% ~ 99% purity level, and the ammonia rectifying column 362 in the purifying ammonia of tower top store up into The ammonia Raw material pail 37 is recycled, and the water that separates in tower bottom of the ammonia rectifying column 362 and micro ammonia are back to the ammonium hydroxide Buffer barrel 34, the another recovery ammonia tower 361 is connected to a multi-effect evaporation system 38 by tower bottom, and the recovery ammonia tower 361 is by tower bottom point The ammonium chloride solution separated out is delivered to the multi-effect evaporation system 38, by the multi-effect evaporation system 38 with 120 °C ~ 160 DEG C of steaming Vapour is heated, and ammonium chloride solution is made to vaporize contained moisture and be detached from ammonium chloride, and the moisture content of ammonium chloride can be lower than 1wt%, And the multi-effect evaporation system 38 is connected with a drying machine 381 and a recycle-water dashpot 39, and by the drying machine 381 recycling as The reaction raw materials of the jacket type reactive tank 113 use, and the steam recycles that provide the jacket type anti-with the recycle-water dashpot 39 Slag charge solvent of the slot 113 after reaction is answered to use, the ammonia Raw material pail 37, the drying machine 381 and the recycle-water buffer in summary The effect of slot 39 is connected to the jacket type reactive tank 113 and can be to reach recycling and reusing.
Tail (useless) gas of the utility model recycles operation, then please sees it as shown in Figure 5, and the utility model includes a tail gas Processing system 42, the exhaust treatment system 42 are connected to the silane reaction system 11, the silicon second with multiple exhaust emissions pipelines 41 Alkane Distallation systm 13, the silicomethane fractionating system 22, the slag charge dashpot 14, the ammonia separation recovery system 36 and the multiple-effect evaporation System 38, the exhaust treatment system 42 include a scrubbing tower 421, a tail gas fluid-tight buffer barrel 422, a high-temperature oxydation device 423 And a filter plant 424, and the tail gas fluid-tight buffer barrel 422 is connected to the tower top and the high-temperature oxydation device 423 of the scrubbing tower 421 Between one end, and the filter plant 424 is connected with the other end of the high-temperature oxydation device 423, and the scrubbing tower 421 is separately connected to this Ammonia spirit dashpot 32, tail (useless) gas branch to each of the exhaust treatment system 42 according to the composition containing ammonia and silane gas A stage, the scrubbing tower 421 discharge into the tail gas fluid-tight buffer barrel 422 with the adsorbing and removing that water carries out ammonia, then by the tail gas liquid Envelope buffer barrel 422, which is formed by ammonium hydroxide and imports the ammonia spirit dashpot 32, to be recycled, and adding as the conversion of ammonium chloride salt Add agent, and micro tail gas is then carried out the destruction of silane gas by the high-temperature oxydation device 423, it is made to be converted into the non-of silica Dangerous substances, then interception collection is carried out by the filter plant 424 of the exhaust treatment system 42, tail gas is effectively treated whereby makes it The pollution to environment is reduced with low cost.
Embodiment described above is only preferred embodiments for fully illustrating the utility model, the utility model Protection scope it is without being limited thereto.Those skilled in the art made equivalent substitute or change on the basis of the utility model It changes, both is within the protection scope of the present invention.The protection scope of the utility model is subject to claims.

Claims (8)

1. a kind of catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely, which is characterized in that include: one Silane reaction system, the silane reaction system include that a magnesium silicide inhales powder bucket, a magnesium silicide automatic feeder, a jacket type Reactive tank, a condenser and an air driven pump, and the magnesium silicide automatic feeder is connected to the magnesium silicide and inhales powder bucket and the collet Between formula reactive tank, and the jacket type reactive tank is installed with a blender, and the top of the jacket type reactive tank connects the condensation The bottom end of device and jacket type reactive tank connects one end of the air driven pump, and the other end of the air driven pump connects a slag charge dashpot;One Gas-liquid separation slot, the gas-liquid separation slot are connected to the condenser, and by the upper end of gas-liquid separation slot connection one for storing vapour The silicomethane temporary tank of SiClx methane, and gas-liquid separation slot connection one is temporary for storing the silicon ethane of liquefaction silicon ethane and liquefied ammonia Deposit slot;And a silicon ethane Distallation systm, which includes a desiliconization ethane tower, an ammonia purification column and a silicon Ethane purification column, the silicon ethane temporary tank connect the desiliconization ethane tower, which connects the ammonia purification column, and should Desiliconization ethane tower lower end connects one end of the silicon ethane purification column, and the other end of the silicon ethane purification column is connected with a liquefaction silicon second Alkane buffer barrel, and the ammonia purification column and the separated ammonia of the silicon ethane purification column are stored in a liquefied ammonia dashpot, and the liquefied ammonia is slow Jet-bedding connects the jacket type reactive tank, and the ammonia purification column upper end connects the silicomethane temporary tank.
2. catalyst according to claim 1 promotes the system that silane reaction generates and its process byproducts recycle entirely, special Sign is that the condenser is sequentially connected with one second condenser and a third condenser, and connects the gas with the third condenser Liquid separating tank.
3. catalyst according to claim 2 promotes the system that silane reaction generates and its process byproducts recycle entirely, special Sign is, is installed with a filter between the condenser and second condenser.
4. catalyst according to claim 1 promotes the system that silane reaction generates and its process byproducts recycle entirely, special Sign is that the silicomethane temporary tank is connected with a silicomethane fractionating system, which includes that a silicomethane returns It receives tower, a silicomethane molecular sieve and a silicomethane purification column, the silicomethane temporary tank and is connected to the silicomethane recovery tower, and the silicon Methane recovery tower upper end connects the silicomethane molecular sieve and silicomethane recovery tower lower end connects the liquefied ammonia dashpot, and by the silicon first Alkane molecular sieve connects the silicomethane purification column, and the silicomethane purification column connects a liquefaction silicomethane buffer barrel.
5. catalyst according to claim 4 promotes the system that silane reaction generates and its process byproducts recycle entirely, special Sign is, which uses interior outer double-layer structure, and the liquefaction silicomethane buffer barrel outer layer in vacuum shape simultaneously It is arranged with the ring body coil pipe of a circulation refrigerant, and the liquefaction silicomethane buffer barrel is connected with a vaporizer, and the vaporizer connects To a finished product pressuring machine.
6. catalyst according to claim 5 promotes the system that silane reaction generates and its process byproducts recycle entirely, special Sign is that the slag charge dashpot is serially connected with a centrifugal filter, an ammonia spirit dashpot, a magnesium hydroxide filter in order And an ammonium hydroxide buffer barrel, and the centrifugal filter and the magnesium hydroxide filter are connected with a dry milling device simultaneously, and with The drying milling device is connected with a high-pressure molding brick making system.
7. catalyst according to claim 6 promotes the system that silane reaction generates and its process byproducts recycle entirely, special Sign is that the ammonium hydroxide buffer barrel is connected with an ammonia separation recovery system, which should with recovery ammonia tower connection Ammonium hydroxide buffer barrel, and an ammonia rectifying column is connected with by the recovery ammonia tower upper end, and the ammonia rectifying column connects an ammonia raw material in tower top Bucket, and the ammonia rectifying column is connected to the ammonium hydroxide buffer barrel in tower bottom, the another recovery ammonia tower is connected to a multiple-effect evaporation system by tower bottom System, and the multi-effect evaporation system is connected with a drying machine and a recycle-water dashpot, and the ammonia Raw material pail, the drying machine and this time It receives water dashpot and is connected to the jacket type reactive tank.
8. catalyst according to claim 7 promotes the system that silane reaction generates and its process byproducts recycle entirely, special Sign is, further includes having an exhaust treatment system, and it is anti-that which with multiple exhaust emissions pipelines is connected to the silane It answers system, the silicon ethane Distallation systm, the silicomethane fractionating system, the slag charge dashpot, the ammonia separation recovery system and this is more Vapo(u)rization system is imitated, which includes a scrubbing tower, a tail gas fluid-tight buffer barrel, a high-temperature oxydation device and a filtering Equipment, and the tail gas fluid-tight buffer barrel is connected between the tower top of the scrubbing tower and the high-temperature oxydation device one end, and with the high temperature The other end of oxidator connects the filter plant, and the scrubbing tower is separately connected to the ammonia spirit dashpot.
CN201820599360.1U 2018-04-25 2018-04-25 Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely Active CN209128044U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201820599360.1U CN209128044U (en) 2018-04-25 2018-04-25 Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201820599360.1U CN209128044U (en) 2018-04-25 2018-04-25 Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely

Publications (1)

Publication Number Publication Date
CN209128044U true CN209128044U (en) 2019-07-19

Family

ID=67226876

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201820599360.1U Active CN209128044U (en) 2018-04-25 2018-04-25 Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely

Country Status (1)

Country Link
CN (1) CN209128044U (en)

Similar Documents

Publication Publication Date Title
RU2663032C2 (en) Phosphorus absorption by hydration and fluorine recovery for smoke exiting kiln in kiln process for production of phosphoric acid
CN104211031B (en) Equipment and process for recovery of fluorine from flue gas of hydration absorption of phosphorus in kiln-method phosphoric acid technology
CN102145912A (en) Process for preparing calcium chloride solution by utilizing ammonia soda filtration mother liquor
CN102120579B (en) Method and device for efficiently and continuously smelting and purifying polysilicon with electron beams
CN106435221A (en) Method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium
CN102372271A (en) Recovery method of waste chlorsilane in polysilicon produced through modified Simens Method
CN112624167B (en) Preparation method of pseudo-boehmite
CN101244970B (en) Apparatus and technique for producing ethylene with ethyl alcohol
CN103693649B (en) The removal of impurities of synthetic gas production technique and useless chlorosilane liquid produced recovery method
CN209128044U (en) Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely
CN112028023B (en) Method and device for purifying and pulverizing metal chloride
CN102309865B (en) Refining system for circulating 1, 3-propanediol in continuous production of poly(trimethylene terephthalate)
CN110395736A (en) Catalyst promotes the system that silane reaction generates and its process byproducts recycle entirely
CN114408929B (en) Separation and purification method and system for fluosilicic acid and silicon dioxide mixed slurry
CN106917108A (en) A kind of production technology of magnesium metal
CN206843079U (en) A kind of improved high purity silane production line
CN101817541A (en) Method and device for separating magnesium chloride hexammoniate during silane production by the magnesium silicide method
CN209259696U (en) A kind of continuous uninterrupted high-purity hydrogen phosphide process units
CN103673505A (en) Method for recycling ammonia gas exhausted in LED production
TWM566203U (en) System for production of silane with catalyst enhancement and total recycle of byproducts
TWI658001B (en) Catalyst for promoting silane reaction generation and full process byproduct recovery system
CN207970858U (en) Three aluminum hydride synthesis systems of solvent-recoverable
CN1420116A (en) Process and apparatus for synthesis of thiophene
CN109678158A (en) Exhaust gas treating method and system in polysilicon production process
CN108823419A (en) A kind of chlorination mentions the recovery and processing system and method for germanium and hydrochloric acid in germanium spent acid

Legal Events

Date Code Title Description
GR01 Patent grant
GR01 Patent grant