CN110395736B - System for catalyst promotes silane reaction and generates and technology accessory substance is retrieved entirely - Google Patents

System for catalyst promotes silane reaction and generates and technology accessory substance is retrieved entirely Download PDF

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Publication number
CN110395736B
CN110395736B CN201810379785.6A CN201810379785A CN110395736B CN 110395736 B CN110395736 B CN 110395736B CN 201810379785 A CN201810379785 A CN 201810379785A CN 110395736 B CN110395736 B CN 110395736B
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ammonia
tank
tower
silicomethane
silane
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CN110395736A (en
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谢嵩岳
李腾智
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Taiwan Speciality Chemicals Corp
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Taiwan Speciality Chemicals Corp
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/04—Hydrides of silicon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/04—Hydrides of silicon
    • C01B33/043—Monosilane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/04—Hydrides of silicon
    • C01B33/046—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/10—Separation of ammonia from ammonia liquors, e.g. gas liquors
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/06—Integration with other chemical processes
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Abstract

The invention provides a system for promoting the generation of a silane reaction by a catalyst and completely recovering a process by-product, wherein the system comprises the following components in percentage by weight: the invention separates silane mixed gas generated by reaction with a newly developed and designed separation and purification system and technology from solid raw materials participating in the reaction, then performs low-temperature gas-liquid separation on the silicomethane from the mixed gas according to the physical characteristics of the mixed gas, and uses the silicomethane fractionation system to recover ammonia raw materials in the silicomethane, purify the silicomethane and remove impurities of the silicomethane, and uses a silicoethane distillation system to fractionate and purify the gas-liquid separated silicoethane and ammonia raw materials, and combines with the developed unique catalyst application technology to improve the conversion rate of the silicoethane, implement a new feeding mode and developed equipment, and recover the ammonia to be used as the reaction raw materials again, thereby stabilizing the productivity and purification process of the silicomethane and the silicoethane.

Description

System for catalyst promotes silane reaction and generates and technology accessory substance is retrieved entirely
Technical Field
The present invention relates to a silane process system, and more particularly to a system for promoting the generation of silane and the recovery of the by-products of the process by using a catalyst.
Background
Nowadays, the silicon magnesium alloy method is a known industrial process for synthesizing raw materials of semiconductor special gases such as silicomethane and silicon ethane, and the silicon magnesium alloy method is known to be used for producing silane, the reaction selectivity of silicon ethane is too low, the cost is reduced along with the refinement of high-purity silicon methane production technology, and the problem of environmental influence caused by the storage of reaction slag and complicated treatment procedures with large energy consumption are solved, so that the process for producing silane by the silicon magnesium alloy method is difficult to meet economic benefits. Due to the disadvantages, the improved silicon-magnesium alloy method is gradually developed, and the selectivity, yield and purity of the silicon-ethane reaction production are improved, but the disposal problem of the reaction slag is still the obstacle of the silane production method, and the production process still has the derivation of a plurality of technical related problems, such as the oxidation reaction of silane to generate silicon dioxide powder particles or crystals due to the operating conditions and environment of the process, which leads to the reduction of the equipment efficiency and production efficiency and the increase of the frequency of cleaning and maintenance. Therefore, the invention aims to design and develop advanced production technology and equipment system, make up and improve the defects of the technology and process for producing silane by adopting the improved silicon-magnesium alloy method, and further develop the improved high-purity silane production method and system.
Disclosure of Invention
The invention aims to solve the defects in the prior art, provides a system for promoting the generation of silane reaction and the full recovery of process byproducts thereof by using a catalyst, improves the reaction rate of raw materials, reduces the influence of the blockage problem of a reaction system by solid powder, and promotes the productivity of silicon ethane by optimizing the silane reaction generation environment.
A silane reaction system comprises a magnesium silicide powder absorption barrel, a magnesium silicide automatic feeding device, a jacketed reaction tank, a condenser and a pneumatic pump, wherein the magnesium silicide powder absorption barrel stores magnesium silicide and a catalyst in an oxygen-free state, the mixing proportion of the catalyst is 15-30% of that of the magnesium silicide, the catalyst is a bimetal compound formed by 20-50wt% of silicon powder and 50-80wt% of metal powder, the magnesium silicide automatic feeding device is connected between the magnesium silicide powder absorption barrel and the jacketed reaction tank, the jacketed reaction tank is provided with a stirrer, the top end of the jacketed reaction tank is connected with the condenser, the bottom end of the jacketed reaction tank is connected with one end of the pneumatic pump, the other end of the pneumatic pump is connected with a slag buffer tank, an air-liquid separation tank is connected with the condenser, the upper end of the air-liquid separation tank is connected with a silicon methane tank for storing vaporized silicon methane, the liquid ammonia separation tank is connected with a temporary storage tank for storing liquefied silicon ethane and temporary storage tank for storing liquid ammonia purification, a silicon ethane purification tower is connected with a liquid ammonia purification tower, the liquid ammonia purification tower is connected with a temporary storage tank for liquid ammonia purification, and a purification tower for liquid ammonia purification of the ammonia purification and ammonia purification tower.
Wherein, the condenser is connected with a second condenser and a third condenser in sequence, and the third condenser is connected with the gas-liquid separation tank.
Wherein a filter is arranged between the condenser and the second condenser.
Wherein, the silicon ethane stored in the liquefied silicon ethane buffer barrel is condensed and filled into at least one steel cylinder at the vacuum low temperature of-75 ℃.
Wherein, this silicomethane groove of keeping in is connected with a silicomethane fractionating system, and this silicomethane fractionating system is including a silicomethane recovery tower, a silicomethane molecular sieve and a silicomethane purification tower, and this silicomethane groove of keeping in is connected in this silicomethane recovery tower, and this liquid ammonia dashpot is connected to this silicomethane molecular sieve of this silicomethane recovery tower upper end connection and this silicomethane recovery tower lower extreme to connect this silicomethane purification tower by this silicomethane molecular sieve, and a liquefaction silicomethane buffer tank is connected to this silicomethane purification tower.
The liquefied silicon methane buffer barrel adopts an inner-outer double-layer structure, liquefied silicon methane is stored in the inner layer of the liquefied silicon methane buffer barrel, the outer layer of the liquefied silicon methane buffer barrel is in a vacuum shape and is wound with a loop pipe for circulating a refrigerant, the liquefied silicon methane buffer barrel is connected with a vaporizer, the vaporizer is connected to a finished product pressurizing machine, and the finished product pressurizing machine is used for filling silicon methane into at least one steel cylinder or at least one tank car.
Wherein, the slag charge buffer slot is connected with a centrifugal filter, an ammonia water solution buffer slot, a magnesium hydroxide filter and an ammonia water buffer barrel in series in sequence, and the centrifugal filter and the magnesium hydroxide filter are connected with a drying and grinding device at the same time, and the drying and grinding device is connected with a high-pressure molding brick making system.
The ammonia water buffer barrel is connected with an ammonia separation and recovery system, the ammonia separation and recovery system is connected with the ammonia water buffer barrel through an ammonia recovery tower, the upper end of the ammonia recovery tower is connected with an ammonia rectifying tower, the top of the ammonia rectifying tower is connected with an ammonia raw material barrel, the bottom of the ammonia rectifying tower is connected with the ammonia water buffer barrel, the bottom of the ammonia recovery tower is connected with a multi-effect evaporation system, the multi-effect evaporation system is connected with a drier and a recovery water buffer tank, and the ammonia raw material barrel, the drier and the recovery water buffer tank are all connected to the jacketed reaction tank for recovery and reuse.
The system comprises a washing tower, a tail gas liquid-sealed buffer barrel, a high-temperature oxidizer and a filtering device, wherein the tail gas treatment system is connected to the silane reaction system, the silicon ethane distillation system, the silicon methane fractionation system, the slag buffer tank, the ammonia separation and recovery system and the multi-effect evaporation system through a plurality of tail gas discharge pipelines, the tail gas treatment system comprises the washing tower, a tail gas liquid-sealed buffer barrel, the high-temperature oxidizer and the filtering device, the tail gas liquid-sealed buffer barrel is connected between the top of the washing tower and one end of the high-temperature oxidizer, the other end of the high-temperature oxidizer is connected with the filtering device, and the washing tower is further connected to the ammonia water solution buffer tank.
The first main objective of the present invention is to improve the conversion rate of ethyl silicon by using an improved silicon-magnesium alloy method in a silane production manner, in combination with a developed unique catalyst application technology, and implement a new feeding manner and a developed device to improve the reaction rate of raw materials and reduce the influence of the blockage problem of the reaction system by solid powder, and effectively control and optimize the environment generated by the silane reaction by using an improved production operation technology to improve the production capacity of ethyl silicon.
The second main objective of the present invention is to separate the silane mixed gas generated by the reaction from the solid raw material involved in the reaction by means of the newly developed and designed separation and purification system and technology, then to separate the silicomethane from the mixed gas by means of low temperature gas-liquid separation according to its physical characteristics, and to use the silicomethane fractionation system to recover the ammonia raw material in the silicomethane and purify the silicomethane and remove its impurities, and then to store the silicomethane in a low temperature vacuum manner, and to fractionate and purify the gas-liquid separated silicoethane and ammonia raw materials by means of the silicoethane distillation system, and to recover the ammonia to reuse it as the reaction raw material, thereby stabilizing the production capacity and purification process of the silicomethane and silicoethane, and effectively reducing the production cost.
The third main objective of the present invention is to use the added water as a solvent after the reaction of the slag generated by the reaction is finished, so that part of the content of the slag can be converted into salt substances and dissolved in the ammonia water, and the subsequent separation and recovery treatment can be carried out by using slurry fluid. The liquid fluid is converted into a recoverable saline ammonia water solution by adding ammonia, and then the ammonium chloride salt solution, the ammonia and the water are separated, purified and recovered by using a distillation system. The ammonium chloride salt solution is subjected to moisture removal treatment and drying by using a high-efficiency evaporation system, and is recycled as a silane production reaction raw material. Thereby effectively reducing the influence of slag storage on the environment and the consumption of production cost.
The fourth main objective of the present invention is to introduce the tail gas (waste gas) generated by the process into a tail gas treatment system through a tail gas discharge pipeline, absorb and remove ammonia gas in the tail gas by means of ammonia adsorption removal technology, and recycle the ammonia gas to be used as salt solution additive solution, and perform oxidation reaction treatment on other silane waste gas by the tail gas treatment system to convert the silane waste gas into non-hazardous gas or slag for disposal, so as to reduce environmental pollution and harm.
Drawings
FIG. 1 is a structure and flow diagram of a process for producing ethyl silicon according to the present invention.
FIG. 2 is a structure and flow diagram of the silicomethane process of the present invention.
FIG. 3 is a schematic view of the structure of a liquefied silicomethane buffer tank according to the present invention.
FIG. 4 is a structure and flow diagram of the slag recovery process of the present invention.
FIG. 5 is a structural and flow diagram of the tail gas recovery process of the present invention.
In the figure:
silane reaction System- -11;
a magnesium silicide powder suction barrel-111;
magnesium silicide auto-feeder-112;
a jacketed reaction tank- - -113;
condenser-114;
a pneumatic pump-115;
mixers-116;
a second condenser- -117;
a third condenser- -118;
filter-119;
a gas-liquid separation tank-12;
a silicon ethane distillation system- - -13;
a desiliconized ethane column- -131;
ammonia purification column-132;
a silicane purification column-133;
liquid ammonia buffer tank-134;
slag buffer tank-14;
temporary storage tank-15 of silicon ethane;
liquefied silicon ethane buffer barrel-16;
a cylinder-17;
a temporary silicomethane storage tank- - -21;
a silane fractionation system-22;
a silicomethane recovery column-221;
silicomethane molecular sieves 222;
a silicomethane purification column-223;
liquefied silicon methane buffer barrel-23;
vaporizer-231;
a loop coil-232;
a finished product press-24;
a cylinder-25;
tank car-26;
centrifugal filter-31;
ammonia solution buffer tank- - -32;
magnesium hydroxide filter-33;
ammonia buffer tank-34;
a dry milling device-35;
high pressure forming brick making system-351;
ammonia separation recovery system-36;
an ammonia recovery column-361;
ammonia rectification column-362;
ammonia feed barrel-37;
multi-effect evaporation system-38;
a dryer 381;
a reclaimed water buffer tank-39;
an exhaust gas discharge line-41;
tail gas treatment system-42;
a scrub column-421;
a tail gas liquid seal buffer barrel-422;
a high temperature oxidizer-423;
filtering device-424;
magnesium silicide and catalyst- -51;
ammonium chloride-52;
recovering water-53.
Detailed Description
The present invention is further described with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Referring first to FIG. 1, a system for promoting the generation of silane and the recovery of the process by-products thereof with a catalyst comprises: a silane reaction system 11, a gas-liquid separation tank 12 and a silicon ethane distillation system 13, wherein the silane reaction system 11 comprises a magnesium silicide powder suction barrel 111, a magnesium silicide automatic feeding device 112, a jacketed reaction tank 113, a condenser 114 and a pneumatic pump 115, and the magnesium silicide powder suction barrel 111 stores magnesium silicide (Mg silicide) in an anaerobic state 2 Si) and a catalyst 51 which is in an oxygen-free state and is subjected to vacuum pumping and nitrogen replacement after being filled and sealed, wherein the mixing ratio of the catalyst is 15 to 30 percent of magnesium silicide, and the catalyst is 20 percentSilicon powder (Si) 50wt% to metal powder 80wt% to form a bimetal composite, wherein the metal powder can be metal elements of alkali metal group and alkaline earth metal group, or metal elements of transition metal such as iron (Fe), or alloys of elements in IIIA-VIA group, the magnesium silicide automatic feeding device 112 is connected between the magnesium silicide powder absorbing barrel 111 and the jacketed reaction tank 113, the jacketed reaction tank 113 is provided with a stirrer 116, the top end of the jacketed reaction tank 113 is connected with the condenser 114, the bottom end of the jacketed reaction tank 113 is connected with one end of the pneumatic pump 115, the other end of the pneumatic pump 115 is connected with a slag buffer tank 14, and the jacketed reaction tank 113 is fed with ammonium chloride 52 (NH 52) (NH) first 4 Cl) powder, sealed nitrogen replacement and vacuum deoxygenation are carried out, and pure ammonia (NH) is introduced 3 ) Then controlling the condensation of a refrigerant at-30 ℃ to form liquid ammonia, starting the stirrer 116 to pre-dissolve ammonium chloride and liquid ammonia to dissolve ammonium chloride in the liquid ammonia to form ammonia and chloride ions, and maintaining the continuous operation of the stirrer 116 until the stirrer finishes the reaction, so as to avoid the powder from being dispersed unevenly in the reaction process or from being solidified and agglomerated due to the reaction to cause retardation, and feeding magnesium silicide and a catalyst 51 into the jacketed reaction tank 113 at a constant rate by the automatic magnesium silicide feeding device 112, i.e. feeding the magnesium silicide and the catalyst 51 into the jacketed reaction tank 113 at a constant rate of 0 to 150 kg/h, and using a small amount of liquid ammonia with a stably controlled flow rate as a carrier fluid, feeding the liquid ammonia into the jacketed reaction tank 113 to react with ammonium chloride, thereby preventing the splashing caused by the contact of the magnesium silicide powder with the liquid ammonia in the tank, causing the powder to adhere to the pipeline or gradually causing the blockage of the pipe, the silane generation process is an exothermic reaction, and the heat energy removal is continuously performed at-30 ℃ in the reaction process, so as to maintain the reaction temperature of the reaction, and the ammonia generated in the process of the ammonia flows back to the liquid ammonia generated by the liquefied reaction, and the liquefied reaction of the ammonia generated ammonia flows back to the liquid ammonia through the jacketed reaction tank 113, thereby maintaining the liquefied reaction tank 113, and the liquefied ammonia generated by the ammonia in the condenser, so as to reduce the liquefied reaction, the liquefied reaction tank 113, the liquefied ammonia, and the liquefied ammonia in the liquefied reaction tank 113, thereby reducing the ammonia reaction process of the ammonia to reduce the ammonia in the ammonia reaction tank 113, and the ammonia generation process of the ammonia) With hydrogen (H) 2 ) The mixed gas is produced by the condenser 114, most of the produced silicon ethane is condensed by the condenser 114 and liquefied again and returned to the jacketed reaction tank 113 because the physical property of the produced silicon ethane is similar to that of ammonia, so that after the silane reaction is finished, the liquid ammonia and the silicon ethane contained in the liquid ammonia are recovered as much as possible, the refrigerant in the condenser 114 is converted to the heating medium of 90 ℃, the liquid ammonia and the silicon ethane in the jacketed reaction tank 113 can be stably steamed and heated to be vaporized, and the liquid ammonia and the silicon ethane (Si) after the reaction are assisted by the heating medium of 90 DEG C 2 H 6 ) And recovered through the condenser 114 by cooking, wherein the reaction raw material is used in a ratio of magnesium silicide 1: ammonium chloride 3 to 6: 9-12 of liquid ammonia, and the reaction formula is as follows:
the silicomethane reaction equation is as follows (main reaction):
Mg 2 Si (s) + 4NH 4 Cl (s) +8NH 3(l) →SiH 4(g) +2(MgCl 2 ‧6NH 3 ) (s)
the reaction equation for the silicon ethane is as follows (side reaction):
2Mg 2 Si (s) +8NH 4 Cl (s) +16NH 3(l) →Si 2 H 6(g) +4(MgCl 2 ‧6NH 3 ) (s) + H 2(g)
the reacted slag is discharged from the pneumatic pump 115 and stored in the slag buffer tank 14, the slag discharged into the slag buffer tank 14 is firstly added with water (or recycled water 53) in the jacketed reaction tank 113 and stirred to partially convert into insoluble magnesium hydroxide solid particles and salt products dissolved therein, wherein after the jacketed reaction tank 113 is emptied of the slag, the tank of the jacketed reaction tank 113 is cleaned and effectively dehydrated by nitrogen flushing, vacuum pumping and heating of 90 ℃ heating medium to avoid the influence of moisture on the oxidation reaction of silane generated in the next reaction process and the water-alkaline environment to form silicon dioxide, thereby improving the silane reaction rate, the gas-liquid separation tank 12 is connected to the condenser 114, and the condenser 114 is sequentially connected with a second condenser117 and a third condenser 118, and the third condenser 118 is connected to the gas-liquid separation tank 12, and the physical characteristics of different boiling point temperatures of the substances are utilized to carry out primary silane separation, and then 2 to 7 kg/cm 2 The constant pressure is sequentially led into the second condenser 117 to be condensed at-30 ℃ and then condensed at-75 ℃ with the third condenser 118, thus avoiding the silane from floating in gas phase and then mixing with gaseous silane and hydrogen, and the liquid silane, liquefied ammonia, and gaseous silane and hydrogen are formed by separation in the gas-liquid separation equipment, a filter 119 is arranged between the condenser 114 and the second condenser 117, because the silane mixed gas generated in the reaction process of the jacketed reaction tank 113 and the ammonia and silane boiled out after the reaction are accompanied by a small amount of raw material or slag powder carried by differential pressure airflow, the filter 119 is used to intercept powder particles larger than 3 to 100 mu m, a temporary storage tank 21 for storing vaporized silane is connected to the upper end of the gas-liquid separation tank 12, the gas-liquid separation tank 12 is connected to a temporary storage tank 15 for storing liquefied silane and liquid ammonia, a silicon ethane distillation system 13 comprises a desilication ethane tower 131, an ammonia purification tower 132 and a silicon ethane purification tower 133, the temporary storage tank 15 is connected to the desilication ethane tower 131, the upper end of the desilication ethane tower 131 is connected to the ammonia purification tower 132, the lower end of the desilication ethane tower 131 is connected to one end of the silicon ethane purification tower 133, the other end of the silicon ethane purification tower 133 is connected to a liquefied silane buffer tank 16, and the desilication ethane tower 131 has a pressure of 18 to 24kg/cm 2 Separating ammonia into the ammonia purification tower 132 under the condition of the temperature of 25-70 ℃, wherein the separated liquid ammonia amount is 58-67wt%, simultaneously separating the silicon ethane into the silicon ethane purification tower 133, the upper end of the ammonia purification tower 132 is connected with the temporary silicon methane storage tank 21, the ammonia purification tower 132 separates a small amount of silicon methane by the temperature difference and reflows to the temporary silicon methane storage tank 21, the silicon ethane purification tower 133 further purifies the silicon ethane at the temperature of 30-100 ℃, and the purified silicon ethane is stored in the liquefied silicon ethane buffer tank 16, so that the reaction selectivity of the silicon ethane can reach 5-25vol%, the silicon ethane stored in the liquefied silicon ethane buffer tank 16 can reach the purity of 4N8 (99.998%), and when the silicon ethane is required to be filled, the condensation is carried out at the vacuum low temperature of-75 ℃ under the condition of-75 DEG CThe liquefied ethyl silicate can be filled into at least one steel cylinder 17 from the liquefied ethyl silicate buffer barrel 16, small amount of purification of ethyl silicate and micro amount of impure gas removal can also be carried out by the same vacuum condensation technology, ammonia separated by the ammonia purification tower 132 and the ethyl silicate purification tower 133 is stored in a liquid ammonia buffer tank 134, the liquid ammonia buffer tank 134 is connected with the jacketed type reaction tank 113, and the recovered ammonia is introduced into the jacketed type reaction tank 113 for reuse through the liquid ammonia buffer tank 134, thereby effectively reducing the production cost.
Another branch line of the present invention performs a purification operation of the silicomethane, and as shown in fig. 2, the temporary storage tank 21 of the silicomethane is connected to a silicomethane fractionating system 22, the silicomethane fractionating system 22 includes a silicomethane recovering tower 221, a silicomethane molecular sieve 222 and a silicomethane purifying tower 223, the upper end of the silicomethane recovering tower 221 is connected to the silicomethane molecular sieve 222, the lower end of the silicomethane recovering tower 221 is connected to the liquid ammonia buffer tank 134, the silicomethane molecular sieve 222 is connected to the silicomethane purifying tower 223, the silicomethane recovering tower 221 is connected to the silicomethane purifying tower 223 at a pressure of 8 to 15 kg/cm 2 Most of the ammonia is fractionated and stored in the liquid ammonia buffer tank 134 at a variable temperature of-60 ℃ to 40 ℃, that is, the characteristic that the ammonia is a relatively heavy substance is utilized, the fractionated ammonia is produced from the bottom of the silane recovery tower 221 and is conveyed to the ammonia buffer tank 134 for recovery, the separated silane gas still contains a small amount of ammonia component with the weight percent of about 2 to 10wt%, the distilled silane gas and a small amount of ammonia are adsorbed by the silane molecular sieves 222 of 3A to 5A to remove ammonia and other impurity gases, wherein the silane molecular sieves 222 can be heated for regeneration of the adsorbed substances by vacuumization after switching, then the silane is introduced into a silane purification tower 223, hydrogen contained in the silane is removed and separated at a low temperature of-160 ℃ to-50 ℃, and the purified silane is stored in a liquefied silane buffer barrel 23. The silicomethane stored in the liquefied silicomethane buffer barrel 23 can reach the purity of 6N (99.9999%), the liquefied silicomethane buffer barrel 23 adopts an inner-outer double-layer structure (shown in a matched figure 3), the liquefied silicomethane is stored in the inner layer of the liquefied silicomethane buffer barrel 23, the outer layer of the liquefied silicomethane buffer barrel 23 is in a vacuum shape and is wound with a ring body coil 232 circulating a refrigerant, and the ring body coil 232 is utilized to circulate the refrigerantTemperature control and pressure control to-50 ℃, and using a refrigerant as condensation of the silicomethane when needed, wherein the liquefied silicomethane buffer tank 23 is connected with a vaporizer 231, the vaporizer 231 is connected to a finished product pressurizing machine 24, when the silicomethane is required to be filled, the silicomethane is guided into the vaporizer 231, is controlled by the refrigerant with the temperature of-30 ℃ to carry out stable flow and is conveyed to the finished product pressurizing machine 24, and is pressurized to 100 to 160 kg/cm by the finished product pressurizing machine 24 2 The pressure of (a) fills the silane into at least one cylinder 25 or at least one tank car 26, thereby facilitating the filling delivery.
The other branch of the present invention performs the slag recycling operation, and as shown in fig. 4, the slag buffering tank 14 is connected in series with a centrifugal filter 31, an aqueous ammonia solution buffering tank 32, a magnesium hydroxide filter 33 and an aqueous ammonia buffering tank 34 in sequence, and the centrifugal filter 31 and the magnesium hydroxide filter 33 are connected with a drying and grinding device 35 at the same time, and the drying and grinding device 35 is connected with a high pressure forming brick making system 351, during the operation, the slag discharged into the slag buffering tank 14 is stirred with water (or recycled water 53) in the jacket type reaction tank 113, so as to partially convert into insoluble magnesium hydroxide solid particles and salt products dissolved therein, and the slurry-like slag flows into the centrifugal filter 31 under the uninterrupted stirring of the slag buffering tank 14, so that the slag can more effectively react with water to form soluble salts, the generated solid particles can be uniformly distributed and prevented from precipitating, the rotary liquid removal of the centrifugal filter 31 is utilized, namely the centrifugal filter 31 removes liquid of slag materials at the rotating speed of 300 to 1000 rpm, the solid powder materials are intercepted by filter materials with 200 to 400 meshes, the liquid part of the slag materials flows to the ammonia water solution buffer tank 32, the solid slag materials are discharged to the drying and grinding device 35 in a scraping mode when the centrifugal filter 31 forms a proper thickness, the drying and grinding device 35 performs heating drying of the solid slag materials and ammonia removal by electric heating and spiral stirring, the solid slag materials are discharged to the high-pressure forming brick making system 351 and used as raw materials for brick making, the solid slag materials can also be directly used as agents for smoke discharge and desulfurization, the ammonia water obtained by recycling is added into the ammonia water solution buffer tank 32, and magnesium chloride in the solution can react to generate ammonium chloride and magnesium hydroxide particles, and the ammonium chloride and the magnesium hydroxide particles are converted into the raw materials for brick making through the ammonia water solutionMagnesium hydroxide powder particles are filtered by the magnesium hydroxide filter 33 with the precision of 1 to 30 μm and discharged to the dry milling device 35, and the discharge mode is that nitrogen is used to blow the particles off the centrifugal filter 31, and the particles are discharged to the dry milling device 35 by the gravity of the particles, so that solid particles are prevented from entering the ammonia water buffer bucket 34, and only ammonia water is stored in the ammonia water buffer bucket 34. The ammonia water buffer tank 34 is connected with an ammonia separation and recovery system 36, the ammonia separation and recovery system 36 is connected with the ammonia water buffer tank 34 through an ammonia recovery tower 361, the upper end of the ammonia recovery tower 361 is connected with an ammonia rectifying tower 362, the top of the ammonia rectifying tower 362 is connected with an ammonia raw material tank 37, the bottom of the ammonia rectifying tower 362 is connected with the ammonia water buffer tank 34, and the ammonia recovery tower 361 is connected with the ammonia raw material tank 34 at a ratio of 0-5 kg/cm 2 The concentration of the separated ammonia water is 10-30wt% which belongs to relatively light substances, the ammonia water solution is discharged to the ammonia rectifying tower 362 from the top of the ammonia recovery tower 361, the ammonia and water are purified and separated in the ammonia rectifying tower 362 at the temperature of-30 ℃ to 130 ℃, the purified ammonia can reach the industrial grade purity level of 98% -99%, the purified ammonia at the top of the ammonia rectifying tower 362 is stored in the ammonia raw material barrel 37 for recycling, the water and trace ammonia separated from the bottom of the ammonia rectifying tower 362 flow back to the ammonia water buffer barrel 34, the ammonia recovery tower 361 is connected to a multi-effect evaporation system 38 from the bottom of the tower, the ammonia chloride solution separated from the bottom of the ammonia recovery tower is conveyed to the multi-effect evaporation system 38, the ammonia solution is heated by steam at the temperature of 120 ℃ to 160 ℃ through the multi-effect evaporation system 38, the water contained in the ammonium chloride solution is separated from the ammonium chloride solution, the ammonium chloride solution is separated from the bottom of the ammonia recovery tower 361 and is conveyed to the multi-effect evaporation system 381, the drying reaction slag recovery tank 381, the drying reaction tank is used for recovering water, and the drying reaction water is provided by the jacket type evaporation system 381, and the drying reaction water recovery tank 39, the jacket type reaction tank 113 and the drying reaction tank 39, the reaction tank 113 and the jacket type reaction tank 39 is used for recovering water recovery system 39.
The present invention relates to a tail gas (waste) recovery operation, and more particularly, to a tail gas (waste) recovery operation, as shown in fig. 5, the present invention includes a tail gas treatment system 42, the tail gas treatment system 42 is connected to the silane reaction system 11, the ethyl silicate distillation system 13, the silicomethane fractionation system 22, the slag buffer tank 14, the ammonia separation recovery system 36 and the multi-effect evaporation system 38 through a plurality of tail gas discharge pipelines 41, the tail gas treatment system 42 includes a washing tower 421, a tail gas liquid seal buffer tank 422, a high temperature oxidizer 423 and a filtering device 424, the tail gas liquid seal buffer tank 422 is connected between the top of the washing tower 421 and one end of the high temperature oxidizer 423, the other end of the high temperature oxidizer 423 is connected to the filtering device, the washing tower 421 is further connected to the aqueous ammonia solution buffer tank 32, the tail gas (waste) is divided into various stages of the tail gas treatment system 42 according to the composition containing ammonia and silane gas, the washing tower 421 uses water to absorb and remove ammonia gas and discharge into the tail gas liquid seal buffer tank 422, and then the tail gas buffer tank 422 is collected as an ammonia solution for treating ammonia salt, thereby reducing the risk of the ammonia chloride ammonia, and the ammonia solution is collected by the ammonia solution 424, and the tail gas buffer tank 42.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.

Claims (9)

1. A system for promoting the generation of silane reaction by catalyst and fully recovering the by-products of the process is characterized by comprising: a silane reaction system, which comprises a magnesium silicide powder suction barrel, a magnesium silicide automatic feeding device, a jacketed reaction tank, a condenser and a pneumatic pump, wherein the magnesium silicide powder suction barrel stores magnesium silicide and a catalyst in an anaerobic state, the mixing proportion of the catalyst is 15-30% of the magnesium silicide, the catalyst is a bimetallic compound formed by 20-50wt% of silicon powder and 50-80wt% of metal powder, the magnesium silicide automatic feeding device is connected between the magnesium silicide powder suction barrel and the jacketed reaction tank, the jacketed reaction tank is provided with a stirrer, the top end of the jacketed reaction tank is connected with the condenser, the bottom end of the jacketed reaction tank is connected with one end of the pneumatic pump, and the other end of the pneumatic pump is connected with a slag material buffer tank; the gas-liquid separation tank is connected with the condenser, the upper end of the gas-liquid separation tank is connected with a temporary silicomethane storage tank for storing vaporized silicomethane, and the gas-liquid separation tank is connected with a temporary silicoethane storage tank for storing liquefied silicoethane and liquid ammonia; and a silicon ethane distillation system, this silicon ethane distillation system is including a desilication ethane tower, an ammonia purification tower and a silicon ethane purification tower, this silicon ethane scratch pad is connected this desilication ethane tower, this ammonia purification tower is connected to this desilication ethane tower upper end, and the one end of this silicon ethane purification tower is connected to this desilication ethane tower lower extreme, the other end of this silicon ethane purification tower is connected with a liquefaction silicon ethane buffer tank, and the ammonia that this ammonia purification tower and this silicon ethane purification tower separated stores in a liquid ammonia scratch pad, and this liquid ammonia scratch pad is connected this jacketed reaction tank and is let ammonia reflux reuse, and this silicon methane scratch pad is connected to this ammonia purification tower upper end.
2. The system as claimed in claim 1, wherein the condenser is sequentially connected to a second condenser and a third condenser, and the third condenser is connected to the gas-liquid separation tank.
3. The system as claimed in claim 2, wherein a filter is disposed between the condenser and the second condenser.
4. The system as claimed in claim 1, wherein the Silicones stored in the Silicones buffer tank are condensed and filled into at least one steel cylinder at a low temperature of-75 ℃ under vacuum.
5. The system as claimed in claim 1, wherein the temporary storage tank is connected to a silicomethane fractionating system, the system comprises a silicomethane recovering tower, a silicomethane molecular sieve and a silicomethane purifying tower, the temporary storage tank is connected to the silicomethane recovering tower, the upper end of the silicomethane recovering tower is connected to the silicomethane molecular sieve, the lower end of the silicomethane recovering tower is connected to the liquid ammonia buffer tank, the silicomethane molecular sieve is connected to the silicomethane purifying tower, and the silicomethane purifying tower is connected to a liquefied silicomethane buffer tank.
6. The system as claimed in claim 5, wherein the liquefied silane buffer tank has an inner and outer layer structure, the liquefied silane is stored in the inner layer of the tank, the outer layer of the tank is vacuum and wound with a coil pipe for circulating a refrigerant, the tank is connected to a vaporizer, the vaporizer is connected to a product pressurizing machine, and the liquefied silane is filled into at least one steel cylinder or at least one tank car by the product pressurizing machine.
7. The system as claimed in claim 5, wherein the slag buffer tank is serially connected with a centrifugal filter, an ammonia water buffer tank, a magnesium hydroxide filter and an ammonia water buffer tank, and the centrifugal filter and the magnesium hydroxide filter are connected with a drying and grinding device, and the drying and grinding device is connected with a high pressure molding brick making system.
8. The system of claim 7, wherein the ammonia buffering tank is connected to an ammonia separation and recovery system, the ammonia separation and recovery system is connected to the ammonia buffering tank via an ammonia recovery tower, the ammonia recovery tower is connected to an ammonia rectification tower at the top, the ammonia rectification tower is connected to the ammonia buffering tank at the bottom, the ammonia recovery tower is connected to a multi-effect evaporation system at the bottom, the multi-effect evaporation system is connected to a dryer and a recovery water buffering tank, and the ammonia buffering tank, the dryer and the recovery water buffering tank are connected to the jacketed reaction tank for recycling.
9. The system as claimed in claim 8, further comprising a tail gas treatment system, wherein the tail gas treatment system is connected to the silane reaction system, the silane distillation system, the silane fractionation system, the slag buffer tank, the ammonia separation and recovery system, and the multi-effect evaporation system through a plurality of tail gas discharge pipelines, the tail gas treatment system comprises a washing tower, a tail gas liquid-sealed buffer tank, a high temperature oxidizer, and a filtering device, the tail gas liquid-sealed buffer tank is connected between the top of the washing tower and one end of the high temperature oxidizer, the other end of the high temperature oxidizer is connected to the filtering device, and the washing tower is further connected to the ammonia solution buffer tank.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63248711A (en) * 1987-04-02 1988-10-17 Mitsui Toatsu Chem Inc Continuous production of silanes
CN101659414A (en) * 2009-09-17 2010-03-03 西安航天华威化工生物工程有限公司 Silicomethane low-temperature production and byproduct comprehensive recycling process
TW201412378A (en) * 2012-09-20 2014-04-01 Taiwan Special Chemicals Corp Purification method for silane

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63248711A (en) * 1987-04-02 1988-10-17 Mitsui Toatsu Chem Inc Continuous production of silanes
CN101659414A (en) * 2009-09-17 2010-03-03 西安航天华威化工生物工程有限公司 Silicomethane low-temperature production and byproduct comprehensive recycling process
TW201412378A (en) * 2012-09-20 2014-04-01 Taiwan Special Chemicals Corp Purification method for silane

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