CN221156582U - Disilane synthesis system - Google Patents
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- CN221156582U CN221156582U CN202323067512.3U CN202323067512U CN221156582U CN 221156582 U CN221156582 U CN 221156582U CN 202323067512 U CN202323067512 U CN 202323067512U CN 221156582 U CN221156582 U CN 221156582U
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- silane
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- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 54
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 52
- 239000007789 gas Substances 0.000 claims abstract description 140
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 129
- 229910000077 silane Inorganic materials 0.000 claims abstract description 128
- 238000000926 separation method Methods 0.000 claims abstract description 77
- 239000002994 raw material Substances 0.000 claims abstract description 65
- 238000006243 chemical reaction Methods 0.000 claims abstract description 60
- 238000009833 condensation Methods 0.000 claims abstract description 35
- 230000005494 condensation Effects 0.000 claims abstract description 34
- 239000001257 hydrogen Substances 0.000 claims abstract description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 28
- 239000000047 product Substances 0.000 claims description 126
- 238000010992 reflux Methods 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000006227 byproduct Substances 0.000 claims description 7
- 150000002431 hydrogen Chemical class 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 10
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 2
- 238000000034 method Methods 0.000 description 19
- VEDJZFSRVVQBIL-UHFFFAOYSA-N trisilane Chemical compound [SiH3][SiH2][SiH3] VEDJZFSRVVQBIL-UHFFFAOYSA-N 0.000 description 13
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 description 11
- 229910021338 magnesium silicide Inorganic materials 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 8
- 238000009835 boiling Methods 0.000 description 8
- 238000007233 catalytic pyrolysis Methods 0.000 description 7
- -1 disilane Chemical class 0.000 description 6
- 238000001308 synthesis method Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 150000004756 silanes Chemical class 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- 239000012280 lithium aluminium hydride Substances 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 4
- 229910007264 Si2H6 Inorganic materials 0.000 description 3
- 238000003776 cleavage reaction Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000007017 scission Effects 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005686 electrostatic field Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910010082 LiAlH Inorganic materials 0.000 description 1
- 229910019752 Mg2Si Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The utility model discloses an disilane synthesis system, and belongs to the technical field of chemical synthesis. The system comprises: comprising the following steps: the disilane separation device comprises a disilane reaction module, a hydrogen separation module and a disilane separation module, wherein the disilane reaction module comprises a disilane synthesis reactor, a raw material gas-product gas heat exchanger, a raw material gas heater, a product gas cooler and a silane circulating compressor, the hydrogen separation module comprises a product gas condensation separator, and the disilane separation module comprises a silane separation tower and a disilane rectifying tower. The utility model adopts the tubular fixed bed reactor filled with the catalyst, the reaction equipment has small volume, high reaction efficiency, high yield of target products and simple product separation flow.
Description
Technical Field
The utility model belongs to the technical field of chemical synthesis, and particularly relates to an disilane synthesis system.
Background
Disilane is an important electron special gas, is mainly used in solar cells and semiconductor industry, and has the advantages of high deposition speed, low deposition temperature and the like compared with silane, and has good market prospect and high price.
The disilane has more synthesis methods, and the raw materials mainly comprise three kinds of magnesium silicide, halogenated disilane, silane and the like. The synthesis method using magnesium silicide and halogenated disilane as raw materials is limited by raw material and product separation, and is mostly used for small-batch production. The synthesis of silane as a raw material is attracting attention with the vigorous development of the silane industry and the continuous development of the downstream market of disilane.
Disilane is prepared from silane, and the key point is to break the silicon-hydrogen bond as much as possible and moderately generate the silicon-silicon bond. Methods for breaking silicon-hydrogen bonds include photolysis, glow discharge, atomic excitation, electrostatic field, pyrolysis, and the like. The photolysis, glow discharge, atomic excitation, electrostatic field and the like need special equipment with high difficulty; meanwhile, the capability of controlling the polymerization degree of the silicon-silicon bond is weak, the content price of a high-order product is high, and the product separation is complex. The pyrolysis can be performed by adopting chemical general equipment, so that the difficulty is low; the silicon-hydrogen bond can be broken and the polymerization degree of the silicon-silicon bond can be controlled by controlling the reaction temperature.
The method for preparing disilane by pyrolysis of silane is divided into non-catalytic pyrolysis and catalytic pyrolysis according to whether a catalyst is adopted. In either method, the key point is to select a reaction system with simple principle and reasonable structure, obtain disilane as much as possible at the lowest possible reaction temperature, and generate as little micropowder as possible. Compared with non-catalytic pyrolysis, the catalytic pyrolysis has the advantages of lower reaction temperature, higher disilane selectivity, lower micropowder yield and relatively reasonable.
The main current disilane synthesis method mainly comprises the following steps:
1) The synthesis of magnesium silicide and ammonium chloride mainly uses magnesium silicide and ammonium chloride to react and synthesize silane, disilane and other higher-order silanes, the main product being silane, but it also produces higher-order silanes, such as disilane, which account for about 3%. The reaction formula:
Mg2Si+4NH4Cl→SiH4+2MgCl2+4NH3
2Mg2Si+8NH4Cl→Si2H6+4MgCl2+8NH3+H2
2Mg3Si2+6NH4Cl→Si2H6+3MgCl2+6NH3
2) The magnesium silicide acidolysis method adopts the chemical reaction of magnesium silicide and inorganic acid to prepare silane, in the experiment, dilute hydrochloric acid is firstly injected into a vacuum reactor, then powdered magnesium silicide is added, and at the moment, the reaction can be immediately carried out in the vacuum reactor to generate mixed gas of various silanes. The reaction is characterized in that higher silanes such as disilane, trisilane and the like are generated in a relatively large amount, wherein the mixed gas generated by the reaction comprises the following components: 40% silane, 30% disilane, 15% trisilane, 10% monosilane and 5% higher order silane, the reaction equation is:
2Mg2Si+8HCl→Si2H6+4MgCl2+H2
The reaction temperature of the reaction is 40-50 ℃, and in actual production, heating is not needed, because the heat released by the reaction can maintain the reaction temperature required by the reaction system when the reaction is carried out at room temperature. Finally, impurities such as silane, H 2、H2 O, HCl and the like are removed by using a low-temperature rectification method, and disilane with higher purity can be obtained.
3) The halodisilane reduction process prepares disilane by reducing hexachlorodisilane (Si 2Cl6) with lithium aluminum hydride (LiAlH 4). The reaction formula:
3LiAlH4+2Si2C16→2Si2H6+3LiCl+3AlCl3
An ethereal solution of lithium aluminum hydride was slowly added to an ethereal solution of hexachlorodisilane under vacuum at 0 ℃ with 15% excess of lithium aluminum hydride. The conversion rate of hexachlorodisilane reaches 87%, and the majority of the product is disilane, and only a small amount of the product is monosilane.
The method reduces halogenated disilane in a solvent to obtain disilane, and the disilane can be reacted under normal pressure and under pressurized conditions, and inert gas is blown into the solvent during the reaction, so that the disilane is separated from the solvent.
4) A silane plasma conversion process is provided by passing silane through a plasma generator. A condenser is connected in series behind the plasma generator, and the whole device forms a closed circulation system. The disilane produced is condensed in a condenser, and unreacted silane is purified by a distillation column and recycled.
5) The non-catalytic pyrolysis method of silane is that the silane is pyrolyzed at a high temperature of 350-500 ℃ to generate disilane, trisilane, higher-order silane and hydrogen, and the higher the reaction temperature is, the easier the silicon-hydrogen bond is broken, and the easier the silicon-silicon bond is formed. At the same time, the higher silanes such as disilane and trisilane are further higher. The excessive progress of the higher-order process results in a fine powder, which reduces the selectivity of disilane and causes clogging by solid silicon deposited on the inner walls of the reactor and the subsequent equipment and lines. The addition of hydrogen and the increase of the reaction pressure can inhibit the generation of micro powder to a certain extent. The main reaction in the method is as follows:
The existing disilane synthesis technology has the defects that:
1) The product of the magnesium silicide ammonium chloride synthesis method takes silane as a main material and disilane as an auxiliary material, and also accompanies H 2、NH3 and other byproducts, so that the product separation difficulty is high;
2) The magnesium silicide acidolysis method is carried out under negative pressure, so that flammable and explosive gases such as disilane, hydrogen and the like are generated, and if a leakage point exists in the reactor, oxygen is easily brought in, and the danger is high. The raw materials are strong in acidity, and have other special requirements on the materials of the reactor and subsequent equipment, pipelines and instruments;
3) The halodisilane reduction method uses hexachlorodisilane with high price as a raw material, and has low economic rationality. The manufacturing difficulty of the reducing agent lithium aluminum hydride is high. The disilane is blown out by inert gas, the obtained crude product contains inert gas and solvent, and the product separation process is complex.
4) The silane plasma conversion method has relatively mild conditions, but the equipment for generating the plasma is more complex, the content of the high-order silane in the product is higher, and the product separation process is more complex;
5) The non-catalytic pyrolysis method of the silane has high reaction temperature, more generated micro powder and easy blockage of equipment and pipelines. Meanwhile, disilane is generated and hydrogen is generated, the reaction is inhibited from going to the disilane generating direction by the existence of the hydrogen in a reaction system, the silane conversion rate, disilane selectivity and disilane yield are limited, and meanwhile, the separation difficulty of the hydrogen and the silane is high.
Therefore, how to develop an disilane synthesis system with small reaction equipment volume, high reaction efficiency, high target product yield and simple product separation flow is a problem to be solved by those skilled in the art.
Disclosure of utility model
In view of this, the present utility model provides an disilane synthesis system.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
An disilane synthesis system, comprising: the disilane separation device comprises a disilane reaction module, a hydrogen separation module and a disilane separation module, wherein the disilane reaction module comprises a disilane synthesis reactor, a raw material gas-product gas heat exchanger, a raw material gas heater, a product gas cooler and a silane circulating compressor, the hydrogen separation module comprises a product gas condensation separator, and the disilane separation module comprises a silane separation tower and a disilane rectifying tower;
The raw material gas-product gas heat exchanger is provided with a raw material gas inlet, a raw material gas outlet of the raw material gas-product gas heat exchanger is communicated with a raw material gas inlet of a raw material gas heater, a raw material gas outlet of the raw material gas heater is communicated with a fresh silane inlet at the top of a disilane synthesis reactor, a mixed silane outlet at the bottom of the disilane synthesis reactor is communicated with a product gas inlet of the raw material gas-product gas heat exchanger, a product gas outlet of the raw material gas-product gas heat exchanger is communicated with a product gas inlet of a product gas cooler, a product gas outlet of the product gas cooler is communicated with a product gas inlet of a product gas condensation separator, a silane outlet of the product gas condensation separator is communicated with a mixed silane inlet of a silane separation tower, a hydrogen outlet is arranged at the top of the product gas condensation separator, a tower kettle of the silane separation tower is communicated with a mixed silane inlet of the disilane rectification tower, a disilane outlet is arranged at the tower top of the disilane rectification tower, and a byproduct outlet is arranged at the tower of the disilane rectification tower;
The top of the silane separation tower is communicated with a circulating silane inlet of a silane circulating compressor, and a circulating silane outlet of the silane circulating compressor is communicated with a feed gas inlet of a feed gas-product gas heat exchanger;
the disilane synthesis reactor is a tubular fixed bed reactor;
the communication modes are all communicated through pipelines.
Further, the product gas condensation separator is divided into a separation part and a condensation part, the separation part is of a cavity structure, the condensation part is of a tube shell structure, a condensation part tube side is used for feeding a gas-phase product and a liquid-phase product, a condensation part tube side is used for feeding condensate, the tube side is provided with a condensate inlet and a condensate outlet, and the separation part is connected with a silane liquid level control system.
The beneficial effect of adopting the further technical scheme is that: the product gas condensation separator integrates two functions of condensation and separation, condenses and collects high-boiling components in the product gas in one device, achieves the purpose of separating hydrogen and the high-boiling components, and avoids a complex pipeline system and a control system.
The device further comprises a reboiler I, a reboiler II, a condenser I, a condenser II, a reflux liquid tank I, a reflux liquid tank II and a reflux ratio control system, wherein the top of the silane separation tower, the condenser I, the reflux liquid tank I and the upper section of the silane separation tower are sequentially connected, the top of the disilane rectifying tower, the condenser II, the reflux liquid tank II and the upper section of the disilane rectifying tower are sequentially connected, the bottom of the silane separation tower is connected with the reboiler I, the bottom of the disilane rectifying tower is connected with the reboiler II, and the condenser I and the condenser II are respectively connected with the reflux ratio control system.
The beneficial effect of adopting the further technical scheme is that: the silane separation tower separates silane from disilane, silane and other light components are obtained at the tower top and returned to the reaction module for recycling, disilane and other heavy components are obtained at the tower bottom and sent to the disilane rectifying tower. Disilane and heavy components are separated by the disilane rectifying tower, disilane is obtained at the tower top, and trisilane and other high-boiling-point substances are obtained at the tower bottom.
Further, the device also comprises a compressor control system, an inlet buffer tank and an outlet buffer tank, wherein the silane circulating compressor is connected with the compressor control system, the top of the silane separating tower, the inlet buffer tank and a circulating silane inlet of the silane circulating compressor are sequentially communicated, and a circulating silane outlet and an outlet buffer tank of the silane circulating compressor are sequentially communicated with a raw material gas inlet of the raw material gas-product gas heat exchanger.
The beneficial effect of adopting the further technical scheme is that: and the silane in the product gas is recycled through pressurization of the compressor, so that the conversion rate of the silane in the raw material gas is improved.
Further, the system also comprises a temperature control system, and the hydrogen outlets of the disilane synthesis reactor, the raw material gas-product gas heat exchanger, the product gas cooler and the product gas condensation separator are respectively connected with the temperature control system.
The beneficial effect of adopting the further technical scheme is that: by the action of the temperature control system, the stability of indexes such as the temperature of the reactor, the temperature of the product gas of the product cooler, the purity of the hydrogen of the product gas condensation separator and the like is ensured.
Further, the condensing portion shell side is connected with a temperature control system.
Further, heat transfer oil heat transfer or water vapor heat transfer is adopted in the heat transfer of the disilane synthesis reactor shell side, and water vapor heat transfer is preferred.
The beneficial effect of adopting the further technical scheme is that: the heat exchange medium transfers the heat generated by the reaction out of the reaction system, so as to avoid the temperature runaway of the catalyst bed.
Further, the above silane recycle compressor employs a diaphragm compressor.
The beneficial effect of adopting the further technical scheme is that: the whole selected compressor has compact and reasonable structure, high compression efficiency, low maintenance rate, good performance of an oil pump system and good cooling condition of the compressor, and high purity gas is prevented from being polluted.
Further, the raw material gas-product gas heat exchanger adopts a shell-and-tube type, the raw material gas passes through a shell side, and the product gas passes through a tube side.
The beneficial effect of adopting the further technical scheme is that: the product gas passes through the tube pass, and the scaling of high-boiling components in the product gas in the heat exchanger is avoided.
The utility model has the beneficial effects that: the tubular fixed bed reactor has the advantages of simple equipment structure, easy control of reaction temperature and the like, and the utility model adopts a condensation and separation integrated mode to realize the separation of hydrogen. The utility model adopts the tubular fixed bed reactor filled with the catalyst, the tube side can be filled with the catalyst to promote the silane pyrolysis reaction to be carried out at a lower temperature and generate the target product disilane, the reaction equipment is small in volume, the reaction efficiency is high, the yield of the target product is high, and the product separation flow is simple.
The tube type fixed bed reactor is universal chemical equipment, the manufacturing process is simple, and the cost is low; the reactor is simple to maintain; the reactor temperature is easy to control.
Compared with an electrocatalytic synthesis system: electrocatalytic synthesis systems have complex reactions, a large number of byproducts, and relatively complex subsequent separations. The fixed bed reaction system has simple reaction, high disilane selectivity and low byproduct content under the action of the catalyst, and the subsequent separation process flow is simple;
The electrocatalytic synthesis system needs to use a relatively complex ionization system, has a complex equipment structure and is large in maintenance workload. The fixed bed reaction system has simple equipment structure and simple maintenance;
Electrocatalytic synthesis systems are relatively noisy and operate in a relatively harsh environment. The fixed bed reaction system has low noise and excellent operation environment.
Compared with the methods such as a magnesium silicide ammonium chloride synthesis method, a magnesium silicide acidolysis method and the like, the product is relatively simple and is suitable for industrial production;
Compared with the halogenated disilane reduction method, the method has the advantages of simple sources of reaction raw materials, relatively low raw material price and higher economic rationality;
Compared with the non-catalytic pyrolysis method of silane, the reaction temperature is lower, the yield of micropowder is lower, and the selectivity and yield of disilane are higher.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present utility model, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the primary structure of the disilane synthesis system of the present utility model;
FIG. 2 is a schematic diagram showing the specific structure of the disilane synthesis system of the present utility model;
In the figure: the device comprises a 101-disilane reaction module, a 102-hydrogen separation module, a 103-disilane separation module, a 1-disilane synthesis reactor, a 2-raw material gas-product gas heat exchanger, a 3-raw material gas heater, a 4-product gas cooler, a 5-silane recycle compressor, a 6-product gas condensation separator, a 7-silane separation tower, an 8-disilane rectifying tower, a 9-separation part, a 10-condensation part, a 11-reboiler I, a 12-condenser I, a 13-reflux tank I, a 14-reboiler II, a 15-condenser II, a 16-reflux tank II, a 17-inlet buffer tank and an 18-outlet buffer tank.
Detailed Description
The following description of the technical solutions in the embodiments of the present utility model will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
As shown in fig. 1-2, the disilane synthesis system includes: the disilane reaction module 101, the hydrogen separation module 102 and the disilane separation module 103, wherein the disilane reaction module 101 comprises a disilane synthesis reactor 1, a raw material gas-product gas heat exchanger 2, a raw material gas heater 3, a product gas cooler 4 and a silane recycle compressor 5, the hydrogen separation module 102 comprises a product gas condensation separator 6, and the disilane separation module 103 comprises a silane separation tower 7 and a disilane rectification tower 8;
the raw material gas-product gas heat exchanger 2 is provided with a raw material gas inlet, a raw material gas outlet of the raw material gas-product gas heat exchanger 2 is communicated with a raw material gas inlet of the raw material gas heater 3, a raw material gas outlet of the raw material gas heater 3 is communicated with a fresh silane inlet at the top of the disilane synthesis reactor 1, a mixed silane outlet at the bottom of the disilane synthesis reactor 1 is communicated with a product gas inlet of the raw material gas-product gas heat exchanger 2, a product gas outlet of the raw material gas-product gas heat exchanger 2 is communicated with a product gas inlet of the product gas cooler 4, a product gas outlet of the product gas cooler 4 is communicated with a product gas inlet of the product gas condensation separator 6, a silane outlet of the product gas condensation separator 6 is communicated with a mixed silane inlet of the silane separation tower 7, a tower kettle of the silane separation tower 7 is communicated with a mixed silane inlet of the disilane rectification tower 8, a disilane outlet is arranged at the top of the disilane rectification tower 8, and a byproduct outlet is arranged at the tower kettle of the disilane rectification tower 8;
The top of the silane separation tower 7 is communicated with a circulating silane inlet of the silane circulating compressor 5, and a circulating silane outlet of the silane circulating compressor 5 is communicated with a raw material gas inlet of the raw material gas-product gas heat exchanger 2;
The disilane synthesis reactor 1 is a tubular fixed bed reactor;
The communication modes are all communicated through pipelines.
In one embodiment, the product gas condensation separator 6 is divided into a separation part 9 and a condensation part 10, the separation part 9 is of a cavity structure, the condensation part 10 is of a shell-and-tube structure, the condensation part 10 is of a tube side for removing gas-phase products and liquid-phase products, the condensation part 10 is of a shell side for removing condensate, a condensate inlet and a condensate outlet are arranged on the shell side, and the separation part 9 is connected with a silane liquid level control system.
In one embodiment, the device further comprises a reboiler I11, a reboiler II 14, a condenser I12, a condenser II 15, a reflux liquid tank I13, a reflux liquid tank II 16 and a reflux ratio control system, wherein the top of the silane separation tower 7, the condenser I12, the reflux liquid tank I13 and the upper section of the silane separation tower 7 are sequentially connected, the top of the disilane rectification tower 8, the condenser II 15, the reflux liquid tank II 16 and the upper section of the disilane rectification tower 8 are sequentially connected, the bottom of the silane separation tower 7 is connected with the reboiler I11, the bottom of the disilane rectification tower 8 is connected with the reboiler II 14, and the condenser I12 and the condenser II 15 are respectively connected with the reflux ratio control system.
In one embodiment, the device further comprises a compressor control system, an inlet buffer tank 17 and an outlet buffer tank 18, wherein the silane circulating compressor 5 is connected with the compressor control system, the top of the silane separating tower 7 and the inlet buffer tank 17 are sequentially communicated with a circulating silane inlet of the silane circulating compressor 5, and a circulating silane outlet of the silane circulating compressor 5 and the outlet buffer tank 18 are sequentially communicated with a raw material gas inlet of the raw material gas-product gas heat exchanger 2.
In one embodiment, a temperature control system is further included, and hydrogen outlets of disilane synthesis reactor 1, feed gas-product gas heat exchanger 2, product gas cooler 4, and product gas condensate separator 6 are respectively connected to the temperature control system.
In one embodiment, the condensing portion 10 shell side is connected to a temperature control system.
In one embodiment, disilane synthesis reactor 1 shell side heat exchange uses conduction oil heat exchange or water vapor heat exchange.
In one embodiment, disilane synthesis reactor 1 shell side heat exchange uses water vapor heat exchange.
In one embodiment, the silane recycle compressor 5 employs a diaphragm compressor.
In one embodiment, the feed gas-product gas heat exchanger 2 employs a shell and tube shell type, the feed gas going through the shell side and the product gas going through the tube side.
Example 1
The disilane synthesis method comprises the following steps:
(1) Fresh silane enters a shell side heat exchange and temperature rise of a raw material gas-product gas heat exchanger 2, then the raw material gas is heated and raised by a raw material gas heater 3, an active alumina catalyst loaded with 3wt% of palladium is arranged on the tube side of an disilane synthesis reactor 1, a heat exchange medium is arranged on the shell side, raw material gas enters the top of the tube side of the disilane synthesis reactor 1, unreacted silane and product gas composed of disilane, trisilane, high-boiling substances and hydrogen generated by reaction are discharged from the bottom of the tube side and enter the tube side heat exchange and temperature reduction of the raw material gas-product gas heat exchanger 2, and then the temperature reduction of the product gas is carried out by a product gas cooler 4; the disilane synthesis reactor 1 had a tube side operating pressure of 0.30MPa, an operating temperature of 250 ℃, a shell side operating pressure of 2.70MPa, an operating temperature of 230℃and a shell side pressure difference of 2.40MPa.
(2) The product gas obtained after cooling from the product gas cooler 4 enters a separation part 9 of a product gas condensation separator 6, the light components of the product gas rise into a tube side of a condensation part 10, heavy component trisilane and high-boiling substances are condensed under the action of condensate and fall into the separation part 9, the light components of the product gas are condensed and fall into the separation part 9 under the action of shell side condensate, the silane and disilane are condensed and fall into the separation part 9, the hydrogen rises and exits the product gas condensation separator 6, and a low-temperature liquid-phase silane mixture consisting of the silane, disilane, trisilane and reboiling substances enters a silane separation tower 7;
(3) The top of the silane separation tower 7 obtains silane, the silane is pressurized by the silane circulating compressor 5 and then mixed with fresh silane, and then the mixture is subjected to heat exchange by the raw material gas-product gas heat exchanger 2, and the mixture is heated by the raw material gas heater 3 and then returned to the disilane synthesis reactor 1; and (3) obtaining a mixture of disilane, trisilane and high-boiling-point substances at the tower bottom of the silane separation tower 7, and feeding the mixture into the disilane rectifying tower 8, obtaining a main product disilane at the tower top of the disilane rectifying tower 8, and obtaining byproduct trisilane and high-boiling-point substances at the tower bottom of the disilane rectifying tower 8.
The silane conversion rate was 2.20%, the product was mainly disilane, and a small amount of trisilane and high boiling substances were contained, and no silane cleavage products such as silicon powder were found, and the results are shown in Table 1.
Example 2
The catalyst in example 1 was changed to activated alumina not supporting metal, the tube side operating pressure of disilane synthesis reactor 1 was 0.45MPa, the operating temperature was 300 ℃, the shell side operating pressure was 6.40MPa, the operating temperature was 280 ℃, the shell side pressure difference was 5.95MPa, and the rest was the same as in example 1.
The silane conversion rate was 1.12%, the product was mainly disilane, and a small amount of trisilane and high boiling substances were contained, and no silane cleavage products such as silicon powder were found, and the results are shown in Table 1.
Example 3
The catalyst in example 1 was changed to an activated carbon catalyst supporting 20wt% of nickel, the tube side operating pressure of the disilane synthesis reactor 1 was 0.40MPa, the operating temperature was 200 ℃, the shell side operating pressure was 0.90MPa, the operating temperature was 180 ℃, the shell side pressure difference was 0.50MPa, and the rest was the same as in example 1.
The silane conversion was 3.05%, the product was mainly disilane, and a significant amount of trisilane and high boiling substances were contained, and no silane cleavage products such as silicon powder were found, and the results are shown in Table 1.
TABLE 1
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present utility model. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the utility model. Thus, the present utility model is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. An disilane synthesis system, comprising: the disilane separation device comprises a disilane reaction module, a hydrogen separation module and a disilane separation module, wherein the disilane reaction module comprises a disilane synthesis reactor, a raw material gas-product gas heat exchanger, a raw material gas heater, a product gas cooler and a silane circulating compressor, the hydrogen separation module comprises a product gas condensation separator, and the disilane separation module comprises a silane separation tower and a disilane rectifying tower;
The raw material gas-product gas heat exchanger is provided with a raw material gas inlet, a raw material gas outlet of the raw material gas-product gas heat exchanger is communicated with a raw material gas inlet of a raw material gas heater, a raw material gas outlet of the raw material gas heater is communicated with a fresh silane inlet at the top of a disilane synthesis reactor, a mixed silane outlet at the bottom of the disilane synthesis reactor is communicated with a product gas inlet of the raw material gas-product gas heat exchanger, a product gas outlet of the raw material gas-product gas heat exchanger is communicated with a product gas inlet of a product gas cooler, a product gas outlet of the product gas cooler is communicated with a product gas inlet of a product gas condensation separator, a silane outlet of the product gas condensation separator is communicated with a mixed silane inlet of a silane separation tower, a tower kettle of the silane separation tower is communicated with a mixed silane inlet of the disilane rectification tower, a disilane outlet is arranged at the top of the disilane rectification tower, and a byproduct outlet is arranged at the tower kettle of the disilane rectification tower;
The top of the silane separation tower is communicated with a circulating silane inlet of a silane circulating compressor, and a circulating silane outlet of the silane circulating compressor is communicated with a feed gas inlet of a feed gas-product gas heat exchanger;
the disilane synthesis reactor is a tubular fixed bed reactor;
The communication modes are all communicated through pipelines.
2. The disilane synthesis system of claim 1, wherein the product gas condensate separator is divided into a separation portion and a condensation portion, the separation portion is of a cavity structure, the condensation portion is of a shell-and-tube structure, the condensation portion tube side is used for removing a gas-phase product and a liquid-phase product, the condensation portion tube side is used for removing condensate, the shell side is provided with a condensate inlet and a condensate outlet, and the separation portion is connected with a silane level control system.
3. The disilane synthesis system according to claim 1, further comprising a reboiler one, a reboiler two, a condenser one, a condenser two, a reflux tank one, a reflux tank two and a reflux ratio control system, wherein the top of the silane separation column, the condenser one, the reflux tank one and the upper section of the silane separation column are sequentially connected, the top of the disilane rectification column, the condenser two, the reflux tank two and the upper section of the disilane rectification column are sequentially connected, the bottom of the silane separation column is connected with the reboiler one, the bottom of the disilane rectification column is connected with the reboiler two, and the condenser one and the condenser two are sequentially connected with the reflux ratio control system.
4. The disilane synthesis system of claim 1, further comprising a compressor control system, an inlet buffer tank and an outlet buffer tank, wherein the silane recycle compressor is connected to the compressor control system, the top of the silane separation column, the inlet buffer tank are sequentially connected to the recycle silane inlet of the silane recycle compressor, and the recycle silane outlet and the outlet buffer tank of the silane recycle compressor are sequentially connected to the feed gas inlet of the feed gas-product gas heat exchanger.
5. The disilane synthesis system of claim 1, further comprising a temperature control system, wherein the hydrogen outlets of the disilane synthesis reactor, the feed gas-product gas heat exchanger, the product gas cooler, and the product gas condensate separator are each coupled to the temperature control system.
6. The disilane synthesis system of claim 1, wherein the disilane synthesis reactor shell side heat exchange uses conduction oil heat exchange or water vapor heat exchange.
7. The disilane synthesis system of claim 1, wherein the silane recycle compressor is a diaphragm compressor.
8. The disilane synthesis system of claim 1, wherein the feed gas-product gas heat exchanger is shell-and-tube type, the feed gas going through a shell side, and the product gas going through a tube side.
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