CN208814668U - The system of the synthesis of silicon propane and Purification by filtration - Google Patents

Abstract

The utility model discloses a kind of synthesis of silicon propane and the systems of Purification by filtration, it includes: a silicon powder filtration treatment system, one silicon propane purification system and a silane conversion system, the desiliconization methane destilling tower of the silicon propane purification system, first destilling tower and after-fractionating tower are by silane molecule size and the difference of boiling point by silicon propane purifies and separates, the effect of reaching high-purity purifying silicon propane whereby, the micro/nano level silicon powder that the above reaction generates is regenerated with the filter group filtering of the silicon powder filtration treatment system with nitrogen backwash, and the filter group is added in sodium hydrate aqueous solution by medicine system, remaining micro/nano level silicon powder and sodium hydrate aqueous solution is set to react to form sodium silicate solution, row is emitted into deslagging bucket again, and then improve the safety of tapping process.

Description

The system of the synthesis of silicon propane and Purification by filtration

Technical field

The utility model relates to a kind of silane process system, refer in particular to it is a kind of can be promoted silane conversion reaction generation And the silicon propane of silicon powder safety filtering processing synthesizes and the system of Purification by filtration.

Background technique

Silicomethane (Silane) and silicon ethane (Disilane) belong to SEG (spy uses electron level gas), and major function is used Way deposits to be used as film.Wherein the main application industry of silicomethane includes LCD panel, solar battery, energy-saving glass and mixed gas Etc. industries, it includes that DRAM, Foundry, LED wafer and silicon are derivative that in addition silicon ethane, which is mainly used in the electronic industry of high-qualityization, The industries such as chemicals, existing market price silicomethane are ten dollars of per kilogram number, and silicon ethane is thousand dollar of per kilogram number, reason It is high for the production technology difficulty of silicon ethane product, and supply falls short of demand and expected future market demand will more increase in market, therefore Price differential is up to hundred times, and the excellent consistency due to silicon ethane and the characteristic compared with silicomethane low deposition temperature, and known silane turns Change reaction procedure and remained a little shortcoming, main cause is summarized as follows: can also have been generated in the silane conversion reaction processing procedure Silicon propane, and known way is all silicon propane is considered as to tail (useless) gas to be directly discharged to combustion tower to carry out burning processing, mainly It is that known technology is excessively high for the purifying cost of silicon propane, its purifying is made not meet economic cost, and by silicon propane together with other The silanes of higher order is discharged together, not only results in the reduction of production, also will increase the pollution to environment, this is this reality With novel the technical issues of being improved point, furthermore, reaction slag charge store caused by environment the problem of influencing and complicated and energy Big processing routine is consumed in source, if silane is because of the operating condition of processing procedure process and oxidation reaction generates silicon powder grain due to environment, will be led It causes the reduction of equipment effectiveness and production efficiency and tears clear maintenance frequency increase open, while also will increase and being generated in disassembly scale removal process The danger of burning, therefore known production of silane processing procedure is difficult to meet economic benefit.

In view of this, this creator is in the manufacturing development and design experiences of being engaged in Related product for many years, for above-mentioned mesh Mark designs in detail and after scrupulous assessment, obtains one eventually really with the utility model of practicability.

Utility model content

The technical problem to be solved by the utility model is to be directed to above-mentioned missing of the existing technology, a kind of silicon is provided The system of propane synthesis and Purification by filtration.

The utility model provides the system of a kind of synthesis of silicon propane and Purification by filtration, comprising: a silicon powder filtration treatment system It is connected with a deslagging bucket and a medicine system with a filter group, excessive fragmentation generates a large amount of micro- during silane conversion reaction Nanoscale silicon powder is directly filtered with the different pore size precision of the filter group, and is removed and be attached in such a way that nitrogen backwash is regenerated Micro/nano level silicon powder in filter group is simultaneously deposited in the deslagging bucket, and nitrogen backwash utilizes the dosing system after regenerating filter group The filter group is added in sodium hydrate aqueous solution by system, and remaining micro/nano level silicon powder and sodium hydrate aqueous solution is made to react to be formed Sodium silicate solution, then row be emitted into the deslagging bucket, and after discharge be added pure water cleaning be attached to it is residual in the filter group Remaining sodium ion avoids sodium ion from polluting silane conversion reaction silane generated；One silicon propane purification system includes sequentially concatenating A desiliconization methane destilling tower, one first destilling tower, an after-fractionating tower and a silicon propane temporary tank, the desiliconization methane distillation Tower, first destilling tower and the after-fractionating tower are by silane molecule size and the difference of boiling point by silicomethane, silicon ethane and silicon Propane purifies and separates make to purify silicon propane storage in the silicon propane temporary tank, and carry out silicon again by isolated silicomethane recycling Alkane conversion reaction；One silane conversion system includes a preheater, a converter, a dehydrogenation destilling tower, silicomethane supplement bucket And a compressor, silicomethane supplement bucket are connected to the preheater one end, and by silicomethane supplement bucket as silane conversion instead The raw material that silicomethane consumes during answering supplements source, and the other end of the preheater connects the converter, makes to be added by the preheater Heat is warming up to 400 °C ~ 500 °C of silicomethane in carrying out silane conversion reaction in the converter, and silicomethane is made to be partially converted into silicon The silanes of ethane, silicon propane and higher order, and the converter connects the filter group of the silicon powder filtration treatment system, makes to react The silicon powder being cracked to form is filtered out by filter group interception, and then will not be accumulated and be caused upstream device piping obstruction, the filtering The outlet of device group by the compressor connects the dehydrogenation destilling tower, and will not be condensed with the top of the dehydrogenation destilling tower and molecular weight most Small Hydrogen Separation removing, and dehydrogenation distillation tower bottom connects the desiliconization methane destilling tower of the silicon propane purification system, makes this The silicomethane of desiliconization methane destilling tower separation delivers into the preheater once again and carries out silane conversion reaction circulation, and the desiliconization first The follow-up process that the silicon propane and higher order silanes of alkane destilling tower separation then import the silicon propane purification system carries out fractionation purifying.

Wherein, which includes three filters sequentially concatenated, and three filters are sequentially equipped with 25 ~ 200 μ M, the filter core of 1 ~ 20 μm and 0.03 ~ 0.8 μm filtering partial size.Or three filters be set in sequence using 5 μm, 0.45 μm and The filter core of 0.1 μm of filtering partial size.

Wherein, three filters of different filtering partial sizes are equipped with array, and only enable one group simultaneously, and the filter is because of filter When wicking the attached excessive silicon powder of interception and the filter inlet/outlet being made to generate pressure gap, allowing hand over the filter and substitute makes With, and regeneration cleaning is carried out to the deactivated filter.

Wherein, which is conveyed in filling a to steel cylinder in a manner of condensate vacuum by silicon propane and carries out shipment.

Wherein, it is connected with a silicon ethane Distallation systm at the top of first destilling tower, and is purified by the silicon ethane Distallation systm Silicon ethane with separate silicomethane.

Wherein, the liquid nitrogen refrigerant that the dehydrogenation destilling tower of the silane conversion system and silicon propane purification system use creates institute Boiling point is lower does not condense hydrogen and silicomethane to distill separation for the pole low temperature environment needed, and the liquid nitrogen vaporization after heat exchange It is close to -160 DEG C of pole low temperature nitrogen for temperature, silicon propane can be condensed then at first destilling tower and after-fractionating tower, in Be re-fed into the shell-side of the silicon propane temporary tank after condensation silicon propane as cold insulation fluid, finally supply should the filter group as inverse It blows brokenly net regenerated nitrogen to use, efficiently uses the liquid nitrogen whereby and cooled down and rushed and blow broken only.

First main purpose of the utility model is, using silicomethane as the raw material of silicon propane conversion reaction, with the silicon The pressure heating heating that the preheater of alkane conversion system controls silicomethane, makes the carry out thermal cracking that silicomethane is stable and imports In converter, the hydrogen silicon molecule for promoting cracking to generate carries out the reaction synthesis of silicon propane, then with filter group by excessive fragmentation institute The solid silicon powder of formation, which filters, to be intercepted, and so that silane gas is entered fractionation purifier apparatus fractionation purifying, be can be effectively controlled silicon whereby The stability of alkane conversion reaction, and reduce or remit react derived from slag charge store and slag charge is to impact caused by environment.

Second main purpose of the utility model is, before Yu Jinhang nitrogen backwash regenerates filter group, by the filter It is vacuumized after group ontology isolation, then pours into nitrogen and carry out punching and blow and replace to be desorbed that filter intercepted by silane conversion reaction The silicon powder of cracking, and manufacture oxygen-free environment, make silicon powder react generation with sodium hydrate aqueous solution water-soluble under oxygen-free environment Sodium metasilicate colloid substance, therefore nitrogen backwash regenerate removal micro/nano level silicon powder after, can be added sodium hydrate aqueous solution into Row impregnates, and is just emitted into deslagging bucket after micro/nano level silicon powder is by big quantitative response, and it is clear to the filter group to add pure water Wash the residual sodium ion (Na of attachment⁺), avoid sodium ion (Na⁺) pollution silane conversion reaction silane generated, finally can just it pacify Complete tear open clearly, can effectively remove micro/nano level silicon powder whereby and maintain filter efficiency, and have both and be improved tapping process Safety the effect of, avoid silicon powder from being exposed in atmosphere and oxidizing fire.

The third main purpose of the utility model is that the silicon propane purification system includes that the desiliconization methane sequentially concatenated steams Evaporate tower, the first destilling tower, after-fractionating tower and silicon propane temporary tank, the desiliconization methane destilling tower, first destilling tower and this Two destilling towers, by the silicomethane, silicon ethane and silicon propane purifies and separates, make to purify by silane molecule size and the difference of boiling point Silicon propane storage is in the silicon propane temporary tank, it is ensured that the purity of silicon propane can reach international norm 4N or more, reach high-purity whereby The effect of degree purifying silicon propane.

The novel characteristics of other purposes, advantage and the utility model will from the following detailed description and related drawings more It is obvious.

Detailed description of the invention

Fig. 1 is the system structure flow chart of the silane conversion system in the utility model.

Fig. 2 is the system structure flow chart of the silicon powder filtration treatment system in the utility model.

Fig. 3 is the system structure flow chart of the silicon propane purification system in the utility model.

Symbol description in attached drawing:

10 silicon powder filtration treatment systems；11 filter groups；111 filters；12 deslagging buckets；13 medicine systems；20 Silicon propane purification system；21 desiliconization methane destilling towers；211 gas-liquid separation slots；22 first destilling towers；23 after-fractionating towers； 24 silicon propane temporary tanks；25 steel cylinders；30 silane conversion systems；31 preheaters；32 converters；33 dehydrogenation destilling towers；34 Silicomethane supplements bucket；35 compressors；40 silicon ethane Distallation systms.

Specific embodiment

To enable to have a better understanding and awareness to the purpose of this utility model, feature and effect, please match below Schema is closed to be described in detail as after:

As shown in Fig. 1 and Fig. 2, the system of a kind of silicon propane synthesis and Purification by filtration comprising have: a silicon powder filtration treatment System 10, a silicon propane purification system 20 and a silane conversion system 30, the silicon powder filtration treatment system 10 is with a filter group 11 are connected with a deslagging bucket 12 and a medicine system 13, a large amount of micro/nano levels that excessive fragmentation generates during silane conversion reaction Silicon powder (Si) is directly filtered with the different pore size precision of the filter group 11, and is removed and be attached in such a way that nitrogen backwash is regenerated Micro/nano level silicon powder in filter group 11 simultaneously deposits in the deslagging bucket 12, nitrogen backwash regenerate after filter group 11 using should plus The filter group 11 is added in sodium hydroxide (NaOH) aqueous solution by medicine system 13, makes remaining micro/nano level silicon powder and sodium hydroxide Reactant aqueous solution forms sodium metasilicate (Na₂SiO₃) solution, then go and be emitted into the deslagging bucket 12, and pure water is added after discharge (H₂O the remaining sodium ion (Na being attached in the filter group 11) is cleaned⁺), avoid sodium ion (Na⁺) pollution silane conversion reaction Silane generated.Its reaction equation is as follows:

Si+2NaOH+H₂O- > Na₂SiO₃+ 2H₂,

Wherein, which includes three filters 111 sequentially concatenated, and three filters 111 are sequentially set Having the filter core of 25 ~ 200 μm, 1 ~ 20 μm and 0.03 ~ 0.8 μm filtering partial sizes or three filters 111 that can also be set in sequence makes The filter core of partial size is filtered with 5 μm, 0.45 μm and 0.1 μm, three filters 111 of difference filtering partial size are equipped with array, and same When only enable one group, which makes 111 inlet/outlet of filter generate pressure gap because filter core intercepts excessive silicon powder When, it allows hand over the filter 111 and carries out substitution use, and regeneration cleaning carried out to the deactivated filter 111, then into one Step explanation, since the silicon powder contains micron order and nanoscale different-grain diameter, only regenerates the filter group 11 with nitrogen backwash The whole nanoscale silicon powder of deficiency removal, cause when dismantling the filter 111 often remaining silicon powder contacted with air and anti- It should cause oxidation that can generate the danger of burning, therefore the utility model overcomes above-mentioned missing with unique technology, Yu Jinhang nitrogen is inverse It blows before regenerating the filter 111, is vacuumized after 11 ontology of filter group must being completely cut off, and pour into nitrogen and rush and blow And it replaces the silicon powder cracked by silane conversion reaction that filter 111 is intercepted, and manufacture oxygen-free environment is desorbed, in anaerobic ring It reacts silicon powder with sodium hydrate aqueous solution and generates water-soluble sodium metasilicate (Na₂SiO₃) colloid substance, therefore in nitrogen After backwash regeneration removal micro/nano level silicon powder, sodium hydrate aqueous solution can be added and impregnated, it is a large amount of to micro/nano level silicon powder It is just emitted into deslagging bucket 12 after reaction, and adds the residual sodium ion (Na of pure water to the filter 111 cleaning attachment⁺), Finally just can safety tear open clear, can effectively remove micro/nano level silicon powder whereby and maintain 111 efficiency of filter, and with The effect of improving the safety of tapping process, avoids silicon powder from being exposed in atmosphere and oxidizing fire.

Again as shown in Fig. 1 and Fig. 3, the silicon propane purification system 20 include the desiliconization methane destilling tower 21 sequentially concatenated, One first destilling tower 22, an after-fractionating tower 23 and a silicon propane temporary tank 24, the desiliconization methane destilling tower 21, first distillation Tower 22 and the after-fractionating tower 23 are by silane molecule size and the difference of boiling point by silicomethane (SiH₄), silicon ethane (Si₂H₆) with Silicon propane (Si₃H₈) purifies and separates, make to purify silicon propane storage in the silicon propane temporary tank 24, the silicon propane temporary tank 24 is by silicon Propane is conveyed in a manner of condensate vacuum and carries out shipment in filling a to steel cylinder 25, and carries out silicon again by isolated silicomethane recycling Alkane conversion reaction.In addition it is connected with a silicon ethane Distallation systm 40 at the top of first destilling tower 22, and is distilled by the silicon ethane and is System 40 purifying silicon ethane with separate silicomethane.Further illustrate, the isolated silane liquid phase mixed liquor of the silane conversion system 30 Body enters the desiliconization methane destilling tower 21, which carries out heat exchange using 100 DEG C ~ 140 DEG C of heating agent, with So that the silicomethane in silane mixture liquid is completely vaporized, and controls 21 operating pressure of desiliconization methane destilling tower in 3 ~ 10kg/ cm²(g) under, make -90 DEG C ~ -50 DEG C of silicomethane boiling point, 20 DEG C ~ 70 DEG C of silicon ethane boiling point, then control cold medium flux and make the desiliconization The temperature of 21 top gaseous phase of methane destilling tower discharging is maintained at -80 DEG C ~ -40 DEG C, and carries out separation removal silicomethane, and by silicon first Alkane is transmitted back in the silane conversion system 30 carries out silane conversion reaction circulation again, and the effect of first destilling tower 22 is separation Silicon ethane and silicon propane, to ensure pan feeding steady sources, the 21 tower bottom liquid phase of desiliconization methane destilling tower discharging is not directly transported Into first destilling tower 22, but it is introduced into a gas-liquid separation slot 211, then via the flow control of the gas-liquid separation slot 211 System imports first destilling tower 22, in first destilling tower 22 with 0 ~ 5kg/cm of operating pressure²(g) with 0 DEG C ~ 120 DEG C of temperature, steam Evaporate and collect the silicon propane liquid that condenses out and enter the after-fractionating tower 23,23 content of after-fractionating tower be silicon propane and Higher order silanes such as silicon butane, but higher order silanes class content is minimum and still lacks market value at present, therefore is not purified And burnt as exhaust emissions Instruction-nearby, which vaporizes silicon propane using 100 DEG C ~ 140 DEG C of heating medium for heating, and with room temperature Cooling water carries out the condensation of silicon propane as refrigerant, and by the 23 overhead collection liquid-phase silicone propane of after-fractionating tower and discharges to silicon Propane temporary tank 24 obtains purifying effect up to the silicon propane of 4N electron level purity whereby.

As shown in Fig. 1, Fig. 2 and Fig. 3, which includes a preheater 31, a converter 32, a dehydrogenation Destilling tower 33, silicomethane supplement bucket 34 and a compressor 35, silicomethane supplement bucket 34 are connected to 31 one end of pre-heater, And source, the pre-heater are supplemented by the raw material that silicomethane supplement bucket 34 is consumed as silicomethane during silane conversion reaction 31 other end connects the converter 32, and the silicomethane for making the preheater 31 that will be heated to 400 ~ 500 °C is in the converter Silane conversion reaction is carried out in 32, silicomethane is made to be partially converted into the silanes of silicon ethane, silicon propane and higher order, and silane turns It is as follows to change reaction formula:

nSiH₄- > H_2(g)+ Si_(s)+ SiH_2(g)+ Si₂H_6(g)+ Si₃H_8(g)+ Si₄H_10(g)...,

And the converter 32 connects the filter group 11 of the silicon powder filtration treatment system 10, the silicon powder for being cracked to form reaction It is filtered out by the filter group 11 interception, and then will not accumulate and cause upstream device piping obstruction, in addition the filter group 11 goes out Mouth is forced into 5 ~ 15kg/cm by compressor 35²(g) conveying connects the dehydrogenation destilling tower 33, and with the top of the dehydrogenation destilling tower 33 Portion does not condense hydrogen (H for molecular weight is the smallest₂) separation removal, and 33 bottom of dehydrogenation destilling tower connects silicon propane purifying system The desiliconization methane destilling tower 21 of system 20, the silicomethane for keeping the desiliconization methane destilling tower 21 isolated deliver into the preheater 31 once again Reaction cycle is carried out, and the isolated silicon propane and higher order silanes of the desiliconization methane destilling tower 21 then imports the silicon propane purification system 20 follow-up process is purified.

As shown in Fig. 1, Fig. 2 and Fig. 3, dehydrogenation destilling tower 33 and the silicon propane purification system 20 of the silane conversion system 30 make Liquid nitrogen refrigerant create needed for pole low temperature environment to distill separation, boiling point is lower does not condense hydrogen and silicomethane, and it is hot Liquid nitrogen after exchanged is vaporizated into temperature still close to -160 DEG C of pole low temperature nitrogen, can be then at first destilling tower 22 and Two destilling towers 23 condense silicon propane, the shell-side of the silicon propane temporary tank 24 are re-fed into after Yu Lengning silicon propane as cold insulation fluid, Finally for should the filter group 11 use as the broken net regenerated nitrogen of backwash, efficiently use the liquid nitrogen whereby and cool down And punching is blown brokenly only.

The above, only a preferred embodiment of the utility model, it is real when the utility model cannot be limited with this The range applied；That is equivalent changes and modifications made according to the patent scope of the utility model generally should still belong to practical in this In the range of new patent is covered.

Claims (7)

1. the system of a kind of silicon propane synthesis and Purification by filtration, which is characterized in that include:

One silicon powder filtration treatment system, the silicon powder filtration treatment system are connected with a deslagging bucket and a dosing system with a filter group System, the micro/nano level silicon powder that excessive fragmentation generates during silane conversion reaction are direct with the different pore size precision of the filter group Filtering, and remove the micro/nano level silicon powder being attached in filter group in such a way that nitrogen backwash is regenerated and deposit in the deslagging bucket It is interior, the filter group is added in sodium hydrate aqueous solution using the medicine system after nitrogen backwash regeneration filter group, makes to remain Micro/nano level silicon powder and sodium hydrate aqueous solution react to form sodium silicate solution, then row is emitted into the deslagging bucket, and in row Pure water is added after putting and cleans the remaining sodium ion being attached in the filter group；

One silicon propane purification system, the silicon propane purification system include the desiliconization methane destilling tower sequentially concatenated, one first steaming Evaporate tower, an after-fractionating tower and a silicon propane temporary tank, the desiliconization methane destilling tower, first destilling tower and the after-fractionating tower By silane molecule size and the difference of boiling point by silicomethane, silicon ethane and silicon propane purifies and separates, make to purify silicon propane storage In the silicon propane temporary tank, and silane conversion reaction is carried out by isolated silicomethane recycling again；And

One silane conversion system, the silane conversion system include a preheater, a converter, a dehydrogenation destilling tower, a silicon first Alkane supplements bucket and a compressor, and silicomethane supplement bucket is connected to the preheater one end, and by silicomethane supplement bucket as silicon The raw material that silicomethane consumes during alkane conversion reaction supplements source, and the other end of the preheater connects the converter, makes by this Preheater is heated to 400 °C ~ 500 °C of silicomethane in carrying out silane conversion reaction in the converter, makes silicomethane part It is converted into the silanes of silicon ethane, silicon propane and high-order, and the converter connects the filter group of the silicon powder filtration treatment system, The silicon powder for being cracked to form reaction is filtered out by filter group interception, and filter group outlet connects this by the compressor and takes off Hydrogen destilling tower, and Hydrogen Separation removing will not be condensed with the top of the dehydrogenation destilling tower, and dehydrogenation distillation tower bottom connection should The desiliconization methane destilling tower of silicon propane purification system, it is pre- that the silicomethane for separating the desiliconization methane destilling tower delivers into this once again Hot device carries out silane conversion reaction circulation, and the silicon propane of desiliconization methane destilling tower separation and higher order silanes then import the silicon third The follow-up process of alkane purification system carries out fractionation purifying.

2. the system of silicon propane synthesis according to claim 1 and Purification by filtration, which is characterized in that wherein, the filter Group includes three filters sequentially concatenated, and three filters are sequentially equipped with 25 ~ 200 μm, 1 ~ 20 μm and 0.03 ~ 0.8 μm Filter the filter core of partial size.

3. the system of silicon propane synthesis according to claim 1 and Purification by filtration, which is characterized in that wherein, the filter Group includes three filters sequentially concatenated, and three filters are set in sequence using 5 μm, 0.45 μm and 0.1 μm filtering grains The filter core of diameter.

4. the system of silicon propane synthesis according to claim 2 or 3 and Purification by filtration, which is characterized in that wherein, different mistakes Three filters for filtering partial size are equipped with array, and only enable one group simultaneously, which makes due to filter core adsorbs and intercepts silicon powder When the filter inlet/outlet generates pressure gap, allows hand over the filter and carry out substitution use, and to the deactivated filtering Device carries out regeneration cleaning.

5. the system of silicon propane synthesis according to claim 1 and Purification by filtration, which is characterized in that wherein, the silicon propane Silicon propane is conveyed in filling a to steel cylinder in a manner of condensate vacuum and carries out shipment by temporary tank.

6. the system of silicon propane synthesis according to claim 1 and Purification by filtration, which is characterized in that wherein, first steaming Evaporate top of tower and be connected with a silicon ethane Distallation systm, and by silicon ethane Distallation systm purifying silicon ethane with separate silicomethane.

7. the system of silicon propane synthesis according to claim 1 and Purification by filtration, which is characterized in that wherein, which turns The dehydrogenation destilling tower of change system separates with the liquid nitrogen refrigerant distillation that silicon propane purification system uses and does not condense hydrogen and silicomethane, And the liquid nitrogen after heat exchange is vaporizated into the nitrogen that temperature is -160 DEG C, it can be then at first destilling tower and after-fractionating tower Silicon propane is condensed, the shell-side of the silicon propane temporary tank is re-fed into after Yu Lengning silicon propane as cold insulation fluid, finally for that should be somebody's turn to do Filter group is used as backwash broken net regenerated nitrogen, is efficiently used the liquid nitrogen whereby and is cooled down and rushed and blows brokenly only.